Edible and biodegradable coating materials and methods
A biodegradable and edible food coating composition using seaweed extract, vegetable or algal oil, and plant extract addresses the need for environmentally friendly packaging by extending the shelf-life of perishable products through barrier and antimicrobial properties.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2025-09-15
- Publication Date
- 2026-03-19
AI Technical Summary
There is a need for economical and environmentally friendly biodegradable and edible food coatings that offer multiple functionalities, as existing packaging materials like films and synthetic polymers do not adequately address this requirement.
A composition comprising seaweed extract, vegetable or algal oil, and plant extract, such as spice or essential oil, is developed, which can be used to coat perishable food products, providing a barrier against moisture and gases, and can be applied using electrostatic spraying or ultrasound-assisted methods.
The composition extends the shelf-life of perishable commodities by retarding ripening and spoilage, offering specific barrier, bioactive, and antimicrobial properties, while being biodegradable and edible.
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Figure US2025046366_19032026_PF_FP_ABST
Abstract
Description
Attorney Docket No.:2024-027-01EDIBLE AND BIODEGRADABLE COATING MATERIALS AND METHODSRELATED APPLICATION INFORMATION
[0001] This application claims priority to U.S. Application No. 63 / 694,934 filed on September 16, 2024, the contents of which are herein incorporated by reference.FIELD OF THE DISCLOSURE
[0002] The subject disclosure relates to food packaging materials, more specifically, biodegradable and edible food coatings.BACKGROUND
[0003] The use of packaging is important for protecting perishable food products. The most commonly used materials are films, wax coatings, and synthetic polymer packaging with a physical barrier effect to the transfer of moisture and gases. However, there is still need of economical and environment friendly materials and methods for food packaging materials, especially for biodegradable and edible food coatings that offer multiple functionalities in one product.SUMMARY
[0004] In some embodiments, disclosed herein is a composition comprising: (1) a seaweed extract comprising sodium alginate; (2) at least one vegetable oil, at least one algal oil, or a combination thereof; and (3) at least one plant extract, wherein the plant extract is a spice extract or an essential oil.
[0005] In some aspects, the seaweed extract is derived from a brown seaweed. In other aspects, the seaweed extract is derived from Saccharina latissima.
[0006] In still other aspects, the at least one vegetable oil in the composition is wheat bran oil, rice bran oil, coconut oil, soy oil, canola oil, avocado oil, olive oil, sunflower flower, peanut oil, or any combination thereof.
[0007] In still further aspects, the at least one algal oil in the composition is a Schizochytrium oil, a Crypthecodinium cohnii oil, a Nannochloropsis oil, a Chlorella oil, a Botryococcus braunii oil, a Dunaliella tertiolecta oil, a Pleurochrysis carterae oil, or any combination thereof.Attorney Docket No.:2024-027-01
[0008] In still further aspects, the at least one plant extract in the composition is a spice extract. In further aspects, the at least one spice extract is a vanilla extract, a cinnamon extract, a clove extract, a coriander extract, a cumin extract, a garlic extract, a ginger extract, a mustard extract, a nutmeg extract, a turmeric extract, a liquid spice oleoresins, or any combination thereof.
[0009] In still further aspects, the at least one plant extract is an essential oil. In further aspects, the at least one essential oil is derived from bay leaf, holy basil, cilantro, lemongrass, marjoram, mint, oregano, parsley, peppermint, rosemary, savory, spearmint, thyme, amaranth, bergamot, cannabis, eucalyptus, grapefruit, lemons, lime, mandarin, neem, orange, pandan, rose, wintergreen, or any combination thereof.
[0010] In still further aspects of the above composition, the sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract are each present in the composition in a ratio of 100:10:1 to 200:10:1. In further aspects of the above composition, the sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract are each present in the composition or formulation in a ratio of 100:20:2 to 200: 10: 1. In yet still further aspects of the above composition, the sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract are each present in the composition or formulation in a ratio of 100:20:2.
[0011] In yet further aspects of the above composition, the composition further comprises at least one emulsifier. In yet further aspects, the at least one emulsifier is at least one lecithin, at least one quillaja saponin, at least one yucca saponin, at least one ginseng saponin, or any combination thereof. In still further aspects, the sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract, and at least one emulsifier are each present in the composition in a ratio of 100: 10: 1 : 1 to 200:10: 1:1. In yet still further aspects, the sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract, and at least one emulsifier are each present in the composition in a ratio of 100:20:2:2 to 200:10:1:1. In yet further aspects, the sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract, and at least one emulsifier are each present in the composition or formulation in a ratio of 100:20:2:2.
[0012] In yet further aspects of the above composition, the composition further comprises a solvent. In some aspects, the solvent is water.Attorney Docket No.:2024-027-01
[0013] In yet further aspects of the above composition, the composition is in the form of an aqueous dispersion.
[0014] In another embodiment, disclosed herein is a method of coating biological material. The method comprises coating a biological material with an effective amount of the composition disclosed above to coat the biological material. In some aspects, the biological material is a plant, part of plant, a fruit, a vegetable, seed of a fruit, seed of a vegetable, a fungi, or any combination thereof.
[0015] In yet another embodiment, disclosed herein is a method of coating a fiber-based material. The method comprises coating the fiber-based material with an effective amount of the composition disclosed above to coat the fiber-based material. In some aspects, the fiber-based material is a paper, paperboard, cardboard, molded fiber products, fiber board, tissue products, or any combination thereof. In yet further aspects, the fiber-based material is in the form of a bottle or a container. In still further aspects, the bottle or container contains at least one liquid or beverage.
[0016] In still yet another embodiment, disclosed herein is a method of slowing the ripening of a perishable food product. The method comprises the step of coating a perishable food product with an effective amount of the composition of the above composition to coat the perishable food product. In some aspects, the perishable food product is a fruit, a vegetable, a seed of a fruit, a seed of a vegetable, a fungi, or any combination thereof.
[0017] In still yet another embodiment, disclosed herein is a method for preparing a seaweed extract, the method comprising:
[0018] a) mixing brown seaweed with at least one food-grade acid to create a mixture, wherein the mixture has a pH of 2-4, and further wherein the treating of the brown seaweed with the at least one food-grade acid produces a by-product fraction and a fraction enriched with alginic acid;
[0019] b) separating the by-product fraction from the fraction enriched with alginic acid;
[0020] c) mixing the fraction enriched with alginic acid with at least one base to form a mixture, wherein the mixture has a pH of 8-12, and further wherein the treating of the fraction enriched with alginic acid with at least one base produces a by-product fraction and a sodium alginate product; and
[0021] d) separating the sodium alginate product from the by-product fraction of step c); andAttorney Docket No.:2024-027-0I
[0022] e) recovering the sodium alginate product from step d).
[0023] In some aspects of the above method, the food-grade acid is selected from the group consisting of: citric acid, acetic acid, carbonic acid, lactic acid, tartaric acid, ascorbic acid, phosphoric acid, fumaric acid, succinic acid, and hydrogen peroxide, or any combinations thereof.
[0024] In yet other aspects of the above method, the base is a carbonate, a bicarbonate, a hydroxide, an oxide, or any combination thereof. In yet further aspects, the base is calcium carbonate, potassium carbonate, sodium carbonate, ammonium carbonate, calcium bicarbonate, potassium bicarbonate, sodium bicarbonate, ammonium bicarbonate, calcium hydroxide, potassium hydroxide, sodium hydroxide, magnesium hydroxide, calcium oxide, potassium oxide, sodium oxide, or any combination thereof.
[0025] In still other aspects of the above method, the separating in step b) is performed using filtration.
[0026] In yet still other aspects of the above method, the separating in step d) is performed using centrifugation.
[0027] In yet still other aspects of the above method, the mixture in step a) is subjected to ultrasound.
[0028] In yet still other aspects of the above method, the mixing of step a) occurs for about 1 to about 24 hours at a temperature of about 20°C to about 80°C.
[0029] In still yet other aspects of the above method, the mixing of step c) occurs for about 5 minutes to about 4 hours at a temperature of about 20°C to about 80°C.
[0030] In still yet other aspects of the above method, the brown seaweed is Saccharina latissima.
[0031] In yet another embodiment, also disclosed herein is a Saccharina latissima extract produced by the above-described method.
[0032] These and other aspects of the present disclosure are described in more detail below.BRIEF DESCRIPTION OF THE DRAWINGS
[0033] The accompanying drawings are included to provide a further understanding of the methods and compositions of the disclosure, and are incorporated in and constitute a part of thisAttorney Docket No.:2024-027-01 specification. The drawings illustrate one or more embodiment(s) of the disclosure, and together with the description serve to explain the principles and operation of the disclosure.
[0034] Figure 1 shows conventional sodium alginate extraction (Figure 1 A) and the simplified two-stage green extraction process of the present disclosure (Figure IB).
[0035] Figure 2 shows a process flow diagram and mass balance of a process to derive different sugar kelp fractions including the sodium alginate rich fraction.
[0036] Figure 3 shows possible routes for acid extraction using relatively green chemistry to derive sodium alginate rich fraction of varying viscosities.
[0037] Figure 4 shows a schematic of composition of the composite liquid formulation when dispersed in water or other solvents (Figure 4A) and in the form of a dried coating on a substrate such as fruit or vegetable surface) (Figure 4B).
[0038] Figure 5 shows the particle size distribution of native emulsions (5% alginate, 1% coconut oil, 0.1% emulsifier, and 0.1% carvacrol) prior to spray drying and emulsions obtained by redispersing the spray dried powders in water. Formulations with different emulsifiers- Figure 5A: Soy lecithin; Figure 5B: Quillaja saponaria extract- QSE (source of saponin emulsifiers); Figure 5C: No Emulsifier; Figure 5D: Mixture of Lecithin and QSE in the ratio of 1 : 1. In each subfigure, the first three lines represent the native aqueous emulsions, and the next three lines represent the emulsions formed by redispersing (redisp) the spray dried powders in water. The addition of emulsifier helps control the PSD.
[0039] Figure 6 shows the particle size distribution of a powder obtained by spray-drying the liquid emulsion. Three lines represent replicate readings. Spray dried particles are aggregates of the components dispersed in the liquid emulsions.
[0040] Figure 7 shows the effect of lipid (Figure 7A) and emulsifier (Figure 7B) on the water vapor transmission rate (WVTR) of films cast from 5% sodium alginate-based emulsions.
[0041] Figure 8 shows emulsifiers added at 0.1% by weight of the emulsion with 5% low viscosity sodium alginate, 1% vegetable oil, 0.1% carvacrol. Emulsifiers employed- Tween 80, Soy lecithin, and plant extracts containing saponin emulsifiers- PG Extract: Panax ginseng, QS: Quillaja saponaria, and YS: Yucca schidigera. Bars represent average and standard deviation of n=6 replicates. Emulsifiers reduce surface tension, that has benefits for fluid transport, spray drying, and wetting of substrate after spraying applications.Attorney Docket No.:2024-027-01
[0042] Figure 9 shows the total solid yield of spray dried powders was significantly affected by the emulsifier. Inclusion of emulsifier helped increase the yield p<0.00 ) and a lipophilic emulsifier (Soy lecithin) had numerically highest yield versus emulsion with Quillaja saponaria extract, and no emulsifier (none).
[0043] Figure 10A shows the schematic of the setup- 1 - Flow control pump; 2- syringe to feed the formulation; 3- tubing; 4- dispensing needle; 5- high voltage source, shown in subfigure C; 6 and 7- grounding; 8- collector metal plate; 9- Taylor-cone formed by the liquid during electro spraying. Figure 10B shows the actual set up showing the dispenser needle and the collector covered with aluminum foil to catch the dripping liquid. Figure 10C shows a high voltage source.
[0044] Figure 11 shows the average weight of liquid solution picked up by ping pong balls immediately after two coating methods- electro spraying and dipping. The balls were submerged in a beaker containing the same formulation and immediately removed so that contact time was approximately 2-3 s, prior to weighing (n = 4).
[0045] Figure 12 shows drying kinetics of ping pong balls coated with the alginate-based formulation. Figure 12A (electrospray coating) and Figure 12B (dip coated) represent the raw data of 4 replicates in terms of the average moisture ratio, and drying rate equation in the form of y=A*exp(k*t) where A is a constant (100) and k is the drying rate. Absolute value of k=0.067 for ES and 0.015 for dip coating drying kinetics. Figure 12C represents the fitted equations- drying kinetics from Figure 12A and Figure 12B, and Figure 12D represents the moisture content on dry basis- weight of ping pong balls, which is aligned with the data presented in Figure 9.
[0046] Figure 13 shows weight loss of berries held under accelerated shelf-life test conditions undergoing different dip coating treatments (Figure 13A) and relative weight loss index normalized to the uncoated control (value normalized to 1) such that the index value higher than 1 indicates reduction in weight loss rate (Figure 13B). For example- Final formulation showed 1.46 times slower weight loss rate compared to the uncoated control. The different treatments also help delineate the barrier function of coconut oil / vegetable oil- the primary barrier to water vapor transmission.
[0047] Figure 14 shows the loss in initial weight after storage for 1 day at ambient temperature (23 °C) and relatively humidity (-45%) of strawberries (Figure 14 A) and weight loss rate index normalized to uncoated control group, set to 1 (Figure 14B) receiving theAttorney Docket No.:2024-027-01 following treatments: Control- no coating; LV: Low viscosity sodium alginate emulsion; MV: medium viscosity sodium alginate emulsion; ES: electrostatic spray coating; DIP: Dip coating.
[0048] Figure 15 shows the effect of variation in coconut oil to essential oil ratio within the 1.1% by weight addition to the sodium alginate formulation on appearance and weight loss of berries. Optimal ratio was between 10:1 and 7:3 CO:EO wt / wt. A very obvious loss of red color and greying, as well as loss of natural peel integrity (index value < control) was observed in the extreme condition of 2:8 where too high concentration of essential oil likely injured the fruit.
[0049] Figure 16 shows a decrease in weight loss (Figure 16A) and fungal incidence (Figure 16B) observed due to coating formulation applied via dip and electrostatic spray (called spray in the figures) on strawberries, later stored under commercial conditions for real-time shelf-life testing. One experimental unit was a composite sample of ten berries in a plastic “clamshell” box and n=4 clamshells per treatment.
[0050] Figure 17 shows a representative FTIR transmittance spectra of SI, S2, and P2 fractionated from sugar kelp with the simplified green biorefinery, compared to conventional sodium alginate as described in Example 3.
[0051] Figure 18 shows molecular weight distribution profiles of the highest viscosity sample (S2 T5: 20 % amplitude, 32.5 minutes, pH 2) and the lowest viscosity sample (S2_T2: 100 % amplitude, 5 minutes, pH 4), compared to commercially purchased sodium alginate as described in Example 3.DETAILED DESCRIPTION
[0052] Before the disclosed processes and materials are described, it is to be understood that the aspects described herein are not limited to specific embodiments, or examples, and as such can, of course, vary. It is also to be understood that the terminology used herein is for the purpose of describing particular aspects only and, unless specifically defined herein, is not intended to be limiting.
[0053] Disclosed invention includes edible coating formulations utilizing seaweeds and plant extracts that can extend the shelf-life of perishable commodities and associated processes to extract biopolymers from seaweeds such as sugar kelp, to manufacture liquid emulsion and dispersion formulations, to manufacture shelf-stable microencapsulate powders, and applicationAttorney Docket No.:2024-027-01 methods to deliver these formulations cost and energy-effectively using precisely controlled coating technologies.
[0054] The biopolymers of interest are derived from biological materials such as seaweeds using a green biorefinery approach that eliminates the need for harsh or strong acids (e.g., hydrochloric acid) or alkali reagents (e.g., sodium hydroxide), along with other remaining fractions. These biopolymers are utilized for making the formulations disclosed herein. The formulations include seaweed biopolymer extracts, plant lipids / fats, and edible surface-active agents of plant origins. The ingredients are blended, homogenized for uniform dispersion and emulsification, and spray dried to microencapsulate the various materials within the polymer matrices. Spray drying is used as it produces shelf-stable dry powder form of multiphase formulations. The powders can be reconstituted to liquid emulsions by end-users without the need of high -power shearing blenders or homogenizers unlike the native emulsion upstream of spray-drying. The reconstituted emulsions can be applied by precisely controlled electrostatic spraying or ultrasound assisted electrostatic spraying methods on various food products (e.g., fruits, vegetables, eggs, cheese, etc.) and non-food biological fresh produce commodities (e.g., flowers, grass, seeds, saplings, etc.) to retard senescence and spoilage arising from various causes (e.g., microbiological, enzymatic, and respiratory and physical abuse). The disclosed formulations provide specific barrier, bioactive, and antimicrobial properties. The formulations and application systems can also be applied onto fruits, vegetables, and other natural products in the field pre-harvest or in post-harvest (for example, fruit / vegetable waxing lines in packhouses). The invention can also be used on non-food materials such as leaves, grasses, and shrubs.
[0055] I. A process for deriving seaweed extracts of interest
[0056] In one aspect, a process is disclosed for deriving or preparing a sodium alginate-rich seaweed extract from biological materials, such as brown seaweeds. Examples of brown seaweeds that can be used in the processes described herein are sugar kelp (Saccharina latissima), Ascophyllum nodosum, Sargassum, Laminaria, Lessonia, Ecklonia, Macrocystis, Durvillea, other genera of brown seaweeds, or any combination thereof. In some aspects, the brown seaweed is sugar kelp (Saccharina latissima).
[0057] The first step in the process involves providing or supplying brown seaweed (e.g., biomass) for use in the process. As mentioned previously, examples of brown seaweeds that can be used in the processes described herein are sugar kelp (Saccharina latissima), AscophyllumAttorney Docket No.:2024-027-01 nodosum, Sargassum, Laminaria, Lessonia, Ecklonia, Macrocystis, Durvillea, other genera of brown seaweeds, or any combination thereof. In some aspects, the seaweed is sugar kelp (Saccharina latissima').
[0058] In some aspects, the seaweed to be provided, supplied, or used is harvested from a shoreline. In some aspects, the seaweed to be supplied or used is the product of seaweed farming.
[0059] In some aspects, the seaweed used in the process is provided fresh, meaning it was recently harvested and is “wet”. In other aspects, the seaweed used in the method may have been dried (e.g., such as by using low-temperature drying), refrigerated, frozen, fermented, or any combination thereof. In some aspects, the seaweed used in the process is dried. In other aspects, the seaweed used in the process is frozen. In still further aspects, the seaweed used in the process is fermented.
[0060] In some aspects, the seaweed can be fermented using lactic acid bacteria (LAB) fermentation, a technique well-known in the art. Lactic acid bacteria (LAB)-induced fermentation is used to stabilize harvested kelp due to its low energy requirements and minimal need for advanced equipment. LAB fermentation techniques under anaerobic conditions (also referred to as “ensiling”) are preservation methods commonly applied to food and forage in agriculture. Successful fermentation lowers the pH (typically below 4.3) to inhibit the growth of pathogenic microorganisms (e.g., clostridia and molds). Low pH may be achieved directly by the addition of an organic acid or indirectly by inoculating the biomass with a starter culture (SC) of LAB, which converts fermentable sugars into lactic acid.
[0061] In some embodiments, the process includes acid extraction or acid treatment, phase separation, alkali extraction, followed by phase separation to derive the sodium alginate-rich extract as shown in Figures 1 and 2.
[0062] In some embodiments, prior to the acid extraction or acid treatment, the seaweed can be milled, chopped, and / or diced using routine techniques in the art (e.g., using a meat or grain grinder). In some aspects, the seaweed is milled. In other aspects, the seaweed is chopped. In still other aspects, the seaweed is diced.
[0063] In an embodiment, the acid extraction or acid treatment is conducted by mixing the seaweed with at least one food-grade acid to form a mixture. Any food-grade acid that facilitates the breakdown of calcium-alginate linkages in the cell matrix of the seaweed to promote alginateAttorney Docket No.:2024-027-01 release can be used. Examples of food-grade acids that can be used include, for example, citric acid, acetic acid, carbonic acid, lactic acid, tartaric acid, ascorbic acid, phosphoric acid, fumaric acid, succinic acid, hydrogen peroxide, or any combination thereof. In some aspects, the acid is citric acid, acetic acid, hydrogen peroxide, and / or carbonic acid. In further aspects, the acid is citric acid. For example, in some aspects, carbonic acid is generated in situ by pumping pressurized carbon dioxide gas into the aqueous slurry of seaweed.
[0064] The amount of food-grade acid to be added should be from about 5% to about 200% (w / w) based on the dry weight of the seaweed used at the beginning of the process. If wet seaweed is used at the beginning of the process, since wet seaweeds are about 90% water, that amount of food-grade acid would be in the same range as described above, but divided by a factor of 10, namely, a range of about 0.5% to about 20% (w / w).
[0065] During the acid extraction or acid treatment, the pH of the mixture should be adjusted to be between a pH 2-4. In some aspects, the pH of the mixture is 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, or 4.0.
[0066] In some embodiments, ultrasound is used during acid extraction or acid treatment. In other words, the mixture is subjected to ultrasound. In some aspects the mixture is subjected to ultrasound for a period of about 30 minutes to about two hours. In other aspects, the mixture is subjected to ultrasound for about one hour. Ultrasound-assisted extraction (UAE) can be used to enhance the extraction efficiency of the food-grade acid. Ultrasound works on the principle of acoustic cavitation, where the rapid formation, growth, and collapse of microscopic bubbles in the solvent generate localized high temperatures, pressures, and shear forces. These mechanical effects disrupt the algal cell walls, facilitating penetration of the food-grade acid and improving the release of intracellular components. By disrupting the cell walls and accelerating mass transfer, UAE complements the food-grade acids, enabling a more sustainable process to achieve a comparable yield as strong acids (See, Figure 1 A).
[0067] In some embodiments, the mixture is allowed to mix for about 1 to about 24 hours at a temperature of about 20°C to about 80°C. In some aspects, the mixture is allowed to mix for about 1 to about 24 hours under ambient conditions (e.g., about 20°C to about 25°C). In some aspects, the mixture is allowed to mix for about 2 to about 24 hours under ambient conditions. InAttorney Docket No.:2024-027-01 still further aspects, the mixture is allowed to mix for about 2 to about 16 hours under ambient conditions.
[0068] The acid extraction or acid treatment produces a resulting mixture that contains: (1) a byproduct (e.g., supernatant) fraction containing a mixture of fucoidan, laminarian, and various solubles (e.g., cellulose, ash, small amounts of alginate / alginic acid (less than 6% w / v), and water); and (2) an alginate / alginic acid-rich (or alginate / alginic acid enriched) fraction or stream. The alginate / alginic acid-rich fraction or stream contains alginate / alginic acid, cellulose, ash, small amounts of fucoidan and laminarian (10% or less combined), water, and other solubles. The alginate / alginic acid-rich fraction or stream is separated from the byproduct using routine techniques known in the art, such as filtration.
[0069] The alginate / alginic acid-rich fraction or stream is subject to alkali extraction or alkali treatment. Specifically, the alkali extraction is performed by mixing at least one base with the alginate / alginic acid-rich fraction or stream to form a mixture. The at least one base can be a carbonate (such as calcium carbonate, potassium carbonate, sodium carbonate, ammonium carbonate, or any combination thereof), a bicarbonate (such as calcium bicarbonate, potassium bicarbonate, sodium bicarbonate, ammonium bicarbonate, or any combination thereof), hydroxides (such as calcium hydroxide (i.e., lime), potassium hydroxide, sodium hydroxide, magnesium hydroxide, or any combination thereof), oxides (such as calcium oxide, potassium oxide, sodium oxide, or any combination thereof), or any combination thereof.
[0070] The amount of at least one base that can be added is from about 25% to about 100% (w / w), based on the dry weight of the seaweed used at the beginning of the process. If wet seaweed is used at the beginning of the process, since wet seaweeds are about 90% water, that amount of base would be in the same range as described above, but divided by a factor of 10, namely, a range of about 2.5% to about 10% (w / w).
[0071] During alkali extraction or alkali treatment, the pH of the mixture should be adjusted to a range of 8-12. In some aspects, the pH of the mixture is 8.0, 8.1, 8.2, 8.3, 8.4, 8.5, 8.6, 8.7,Attorney Docket No.:2024-027-018.8, 8.9, 9.0, 9.1, 9.2, 9.3, 9.4, 9.5, 9.6, 9.7, 9.8, 9.9, 10.0, 10.1, 10.2, 10.3, 10.4, 10.5, 10.6, 10.7,10.8, 10.9, 11.0, 11.1, 11.2, 11.3, 11.4, 11.5, 11.6, 11.7, 11.8, 11.9, or 12.0.
[0072] In some aspects, the mixture is stirred at a temperature between about 20°C to about 80°C for about 5 minutes to about 4 hours. In other aspects, the mixture is stirred at a temperature between about 25 °C to about 60°C for about 2 to about 3 hours.
[0073] The alkali extraction or treatment produces a resulting mixture that contains: (1) a byproduct (e.g., supernatant) fraction containing a mixture of fucoidan, laminarian, and various solubles (e.g., cellulose, ash, small amounts of sodium alginate (less than 6% w / v), base, and water); and (2) a crude alginate-rich product or fraction. The crude alginate-rich product or fraction contains sodium alginate, cellulose, ash, small amounts of fucoidan and laminarian (1% or less combined), water, base, and other solubles.
[0074] The byproduct (e.g., supernatant) fraction and crude sodium alginate-rich product or fraction can be separated using routine techniques known in the art. For example, the resulting mixture (e.g., the byproduct fraction and the crude sodium alginate-rich product or fraction) can be separated using a strainer and / or centrifugation. In some aspects, the resulting mixture is separated using membrane separation. In some aspects, the resulting mixture is separated using centrifugation. In further aspects, the resulting mixture is separated using a combination of membrane separation and centrifugation.
[0075] Once the crude sodium alginate-rich product or fraction is separated from the byproduct (e.g., supernatant), the resulting product can be recovered. This recovered product is a sodium alginate extract (also referred to interchangeably herein as a “seaweed extract”). The main component of the sodium alginate extract or seaweed extract is sodium alginate. In certain embodiments, the seaweed extract includes impurities such as minerals, cellulose, fucoidan, laminarin, sugars, oligonucleotides, lipids, or any combination thereof, which are present in aAttorney Docket No.:2024-027-01 seaweed. When the seaweed used is wet Saccharina latissima, the sodium alginate extract produced from the above process contains:
[0076] a. sodium alginate in an amount of from about 0.1% to about 6.0% (weight / weight (w / w));
[0077] b. laminarin in an amount of from about 0.1% to about 6.5 % (w / w);
[0078] c. fucoidan in an amount of from about 0.1 % to about 2.0% (w / w);
[0079] d. cellulose in an amount of from about 0.1% to about 2.0% (w / w);
[0080] e. sugars, oligonucleotides, and / or lipids, collectively in an amount of 0.1 % to about 6.0% (w / w); and
[0081] f. minerals (e.g., ash) in amount of from about 2% to about 4% (w / w).
[0082] In some aspects, the sodium alginate is present in the extract in an amount of from about 0.1% to about 5.5% (w / w), about 0.1% to about 5.0% (w / w), about 0.1% to about 4.5% (w / w), about 0.1% to about 4.0% (w / w), about 0.1% to about 3.5% (w / w), about 0.1% to about 3.0% (w / w), about 0.1% to about 2.5% (w / w); about 0.1% to about 2.0% (w / w), about 0.1% to about 1.5% (w / w), about 0.1% to about 1.0% (w / w), about 0.1% to 0.75% (w / w), about 0.5% to about 5.5% (w / w), about 0.5% to about 5.0% (w / w), about 0.5% to about 4.5% (w / w), about 0.5% to about 4.0% (w / w), about 0.5% to about 3.5% (w / w), about 0.5% to about 3.0% (w / w), about 0.5% to about 2.5% (w / w); about 0.5% to about 2.0% (w / w), about 0.5% to about 1.5% (w / w), about 0.5% to about 1.0% (w / w), about 0.5% to 0.75% (w / w), about 1.0% to about 5.5% (w / w), about 1.0% to about 5.0% (w / w), about 1.0% to about 4.5% (w / w), about 1.0% to about 4.0% (w / w), about 1.0% to about 3.5% (w / w), about 1.0% to about 3.0% (w / w), about 1.0% to about 2.5% (w / w); about 1.0% to about 2.0% (w / w), or about 1.0% to about 1.5% (w / w).
[0083] The resulting sodium alginate extract produced from the above process can be mixed with one or more additional ingredients to produce a sodium alginate composition or seaweed extract formulation. For example, the sodium alginate extract described herein can be mixed with: (1) at least one vegetable oil, at least one algal oil, or combinations thereof; (2) at least one plant extract, such as a spice extract, and / or an essential oil; (3) one or more emulsifiers; (4) one or more solvents; or (5) any combinations of (l)-(4). Additionally, the sodium alginate extract composition or formulation can be subjected to further processing techniques such as homogenization, emulsification, or a combination of homogenization and emulsification, usingAttorney Docket No.:2024-027-0I routine techniques known in the art. Homogenization and / or emulsification can be used to create an aqueous dispersion of the sodium alginate extract composition or formulation.
[0084] In some aspects, the sodium alginate composition or formulation is a liquid, such as an aqueous dispersion. In some aspects, the sodium alginate composition or formulation is dried into a powder. For example, the sodium alginate composition or formulation can be dried into a powder using spray-drying techniques known in the art. If dried, the sodium alginate composition or formulation can be reconstituted into a liquid (e.g., aqueous dispersion) prior to use using routine techniques known in the art. In some aspects, the sodium alginate composition or formulation is a solid.
[0085] Unlike conventional sodium alginate extraction processes known in the art (See, Figure 1 A), the process described herein employs a green biorefinery approach that eliminates the dependence on harsh alkali (NaOH) and harsh acids (HC1), extensive purification steps and high energy inputs. The process described herein exhibits enhanced extraction efficiency and yield over the conventional sodium alginate extraction processes known in the art while also reducing operational complexity, waste generation, and the reliance on hazardous substances. The process of the present disclosure provides a sustainable and scalable alternative for sodium alginate production that aligns with the growing demand for greener technologies in marine biomass valorization.
[0086] IL A composition for use in food packaging materials
[0087] In another embodiment, disclosed is a composition (or formulation) comprising: (1) a biological material extract such as a seaweed extract; (2) at least one vegetable oil, an algal oil, or a combination thereof; and (3) at least one plant extract, such as a spice extract or an essential oil. In some embodiments, disclosed is a composition (or formulation) comprising: (1) a biological material extract such as a seaweed extract; (2) at least one vegetable oil; and (3) at least one plant extract, such as a spice extract or an essential oil. In some embodiments, disclosed is a composition (or formulation) comprising: (1) a biological material extract such as a seaweed extract; (2) at least one vegetable oil, an algal oil, or a combination thereof; (3) at least one plant extract, such as a spice extract or an essential oil; and (4) at least one emulsifier. In some embodiments, disclosed is a composition (or formulation) comprising: (1) a biological material extract such as a seaweed extract; (2) at least one vegetable oil; (3) at least one plant extract, such as a spice extract or an essential oil; and (4) at least one emulsifier.Attorney Docket No.:2024-027-01
[0088] In some aspects, the composition or formulation contains sodium alginate, at least one vegetable oil, and / or at least one algal oil, and at least one plant extract (e.g., a spice extract or an essential oil) in a ratio in a range of: 100:10:1 to 200:10:1 (sodium alginate vegetable oil and / or algal oikplant extract), in a ratio in a range of: 100:20:2 to 200:10:1, or in a ratio of: 100:50:5 to 200: 10: 1. In some aspects, the ratio of sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract (e.g., a spice extract or an essential oil) is: 100:20:2. In some aspects, the composition or formulation contains sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one spice extract in a ratio in a range of: 100: 10: 1 to 200:10:1 (sodium alginate:vegetable oil and / or algal oil: spice extract), in aratio in a range of: 100:20:2 to 200:10:1, or in a ratio of: 100:50:5 to 200:10:1. In some aspects, the ratio of sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one spice extract is: 100:20:2.
[0089] In some aspects, the composition or formulation contains sodium alginate, at least one vegetable oil, and at least one plant extract (e.g., a spice extract or an essential oil) in a ratio in a range of: 100:10:1 to 200:10:1 (sodium alginate:vegetable oikplant extract), in aratio in a range of: 100:20:2 to 200: 10:1, or in a ratio of: 100:50:5 to 200:10:1. In some aspects, the ratio of sodium alginate, at least one vegetable oil, and at least one plant extract (e.g., a spice extract or an essential oil) is: 100:20:2. In some aspects, the composition or formulation contains sodium alginate, at least one vegetable oil, and at least one spice extract in a ratio in a range of: 100: 10: 1 to 200: 10:1 (sodium alginate:vegetable oikspice extract), in a ratio in a range of: 100:20:2 to 200:10:1, or in a ratio of: 100:50:5 to 200:10:1. In some aspects, the ratio of sodium alginate, at least one vegetable oil, and at least one spice extract is: 100:20:2.
[0090] In some aspects, when the composition or formulation is in the form of a liquid, it contains: sodium alginate in an amount of about 0.1 % to about 10% (w / w), vegetable oil, an algal oil, or a combination thereof in an amount of about 0.02% to about 2%, (w / w) and at least one plant extract in an amount of about 0.02% to about 2% (w / w). It should be noted that the concentration of sodium alginate used in the compositions or formulations described herein can vary from about 0.1% to about 10% (w / w) depending on the molecular weight of the sodium alginate. Specifically, it was found that sodium alginate: (a) having a molecular weight of about 32 to about 200 kiloDalton (kDa) exhibits a low viscosity in the compositions or formulationsAttorney Docket No.:2024-027-01 described herein; (b) having a molecular weight greater than about 200 to about 600 kDa exhibits a medium viscosity in the compositions or formulations described herein; and (c) having a molecular weight greater than about 600 kDa exhibits a high viscosity in the compositions or formulations described herein. When the compositions or formulations of the present disclosure are in the form of a liquid (e.g., aqueous dispersion), sodium alginate having a molecular weight of about 32 to about 200 kDa and a low viscosity are present in said compositions in a concentration of about 2% to about 10% (w / w). When the compositions or formulations of the present disclosure are in the form of a liquid, sodium alginate having a molecular weight of greater than about 200 to about 600 kDa and a medium viscosity are present in said compositions in a concentration of about 0.1% to about 3% (w / w). When the compositions or formulations of the present disclosure are in the form of a liquid, sodium alginate having a low molecular weight of greater than about 600 kDa and a high viscosity are present in said compositions in a concentration of about 0.1% to about 1% (w / w).
[0091] In some embodiments, the composition or formulation is in the form of a liquid, such as a multiphase liquid (e.g., an aqueous dispersion). In some embodiments, the composition or formulation is in the form of a powder (e.g., the aqueous dispersion can be dried using routine techniques known in the art (e.g., spray drying, drum drying, fluidized bed drying, or tray drying among others) to create a powder, flakes, or pellets, and the solids formulation reconstituted in one or more solvents before use.). In some embodiments, the composition or formulation is in the form of a solid.
[0092] When the composition or formulation is in the form of a solid (which is achieved by drying), it contains about 70% to about 80% (w / w) of sodium alginate, about 10% to about 30% (w / w) of at least one vegetable oil and / or at least one algal oil; and about 1% to about 10% (w / w) of at least one plant extract. Additionally, if the composition or formulation contains at least one emulsifier, the emulsifier is present in an amount of about 1% to about 10% (w / w).
[0093] In an embodiment, the biological material extract includes a seaweed extract. In an embodiment, the seaweed extract includes sodium alginate, cellulose, pectin, laminarin, or a combination thereof. In an embodiment, the seaweed extract is an extract of biological materials such as sugar kelp (Saccharina latissima).
[0094] In an embodiment, the seaweed extract is an extract derived from wet sugar kelp (Saccharina latissima). In some aspects, the seaweed extract is a sodium alginate extract derivedAttorney Docket No.:2024-027-01 from wet sugar kelp that contains sodium alginate in an amount of from about 0.1% to about 6.0% (weight / weight (w / w)). In some aspects, the sodium alginate is present in the extract in an amount of from about 0.1% to about 5.5% (w / w), about 0.1% to about 5.0% (w / w), about 0.1% to about 4.5% (w / w), about 0.1% to about 4.0% (w / w), about 0.1% to about 3.5% (w / w), about 0.1% to about 3.0% (w / w), about 0.1% to about 2.5% (w / w); about 0.1% to about 2.0% (w / w), about 0.1% to about 1.5% (w / w), about 0.1% to about 1.0% (w / w), about 0.1% to 0.75% (w / w), about 0.5% to about 5.5% (w / w), about 0.5% to about 5.0% (w / w), about 0.5% to about 4.5% (w / w), about 0.5% to about 4.0% (w / w), about 0.5% to about 3.5% (w / w), about 0.5% to about 3.0% (w / w), about 0.5% to about 2.5% (w / w); about 0.5% to about 2.0% (w / w), about 0.5% to about 1.5% (w / w), about 0.5% to about 1.0% (w / w), about 0.5% to 0.75% (w / w), about 1.0% to about 5.5% (w / w), about 1.0% to about 5.0% (w / w), about 1.0% to about 4.5% (w / w), about 1.0% to about 4.0% (w / w), about 1.0% to about 3.5% (w / w), about 1.0% to about 3.0% (w / w),
[0095] In addition, the seaweed extract (derived from wet brown kelp, such as sugar kelp) can also contain one or more of the following ingredients:
[0096] a. laminarin in an amount of from about 0.1 to about 6.5% (w / w);
[0097] b. fucoidan in an amount of from about 0.1 to about 2.0% (w / w);
[0098] c. cellulose in an amount of from about 0.1 to about 2.0% (w / w);
[0099] d. sugars, oligonucleotides, and / or lipids, collectively in an amount of 0.1 to about 6.0% (w / w); and / or
[0100] e. minerals (e.g., ash) in amount of from about 2 to about 4% (w / w).
[0101] In still further aspects, the seaweed extract can be a sodium alginate extract derived from wet sugar kelp produced by the process described in Section I, which contains:
[0102] a. sodium alginate in an amount of from about 0.1 to about 6.0% (weight / weight (w / w));
[0103] b. laminarin in an amount of from about 0.1 to about 6.5% (w / w);
[0104] c. fucoidan in an amount of from about 0.1 to about 2.0% (w / w);
[0105] d. cellulose in an amount of from about 0.1 to about 2.0% (w / w);
[0106] e. sugars, oligonucleotides, and / or lipids, collectively in an amount of 0.1 to about 6.0% (w / w); andAttorney Docket No.:2024-027-01
[0107] f. minerals (e.g., ash) in amount of from about 2 to about 4% (w / w).
[0108] In some embodiments, the composition or formulation is in the form of an aqueous dispersion. In some aspects, the concentration of the seaweed extract is about 0.1% to about 10% w / w, about 0.1% to about 9% (w / w), about 0.1% to about 8% (w / w), about 0.1% to about 7% (w / w), about 0.1% to about 6% (w / w), about 0.1% to about 5% (w / w), about 0.1% to about 4% (w / w), about 0.1% to about 3% (w / w), about 0.1% to about 2% (w / w), about 0.1% to about 1% (w / w), about 0.1% to about 0.5% (w / w), about 0.5 to about 9% (w / w), about 0.5 to about 8% (w / w), about 0.5 to about 7% (w / w), about 0.5 to about 6% (w / w), about 0.5 to about 5% (w / w), about 0.5 to about 4% (w / w), about 0.5 to about 3% (w / w), about 0.5 to about 2% (w / w), or about 0.5 to about 1% (w / w) in an aqueous dispersion. In an embodiment, the concentration of the seaweed extract is about 0.5 to about 6% (w / w) in an aqueous dispersion.
[0109] In certain aspects, the seaweed extract acts as a barrier for gas exchange after film or coating formation, when applied as a coating (See, Figure 4). In certain aspects, the seaweed extract acts as a matrix / bulking agent (See, Figure 4). In certain embodiments, the seaweed extract acts as a wet and dry scaffold for the other ingredients, such as at least one vegetable oil, at least one algal oil, and / or at least one plant extract. (See, Figure 4).
[0110] As used herein, “vegetable oil” refers to an edible oil derived from plant sources, typically seeds, fruits, nuts, or cereal grains, and comprises primarily of monoglycerides (monoacylglycerol), diglycerides (diacylglycerol), and triglycerides (triacylglycerols), with minor components such as phospholipids, sterols, and antioxidants. Vegetable oils are often liquid at room temperature (except some oils like coconut and palm), and their fatty acid profiles vary depending on botanical origin. Examples of vegetable oils are wheat bran, rice bran, coconut, com, soy, canola, avocado, olive, sunflower, safflower, sesame, mustard, peanut, walnut, flaxseed, cashew nut, or any combination thereof. In some aspects, the concentration of the vegetable oil used in the composition is about 0.01% to about 5% (w / w), about 0.01% to about 4% (w / w), about 0.01% to about 3% (w / w), about 0.01% to about 2% (w / w), about 0.01% to about 1% (w / w), about 0.01% to about 0.5% (w / w), about 0.1% to about 5% (w / w), about 0.1% to about 4% (w / w), about 0.1% to about 3% (w / w), about 0.1% to about 2% (w / w), about 0.1% to 1% (w / w), or about 0.1% to 0.5% (w / w) in an aqueous dispersion. In an embodiment, the concentration of the vegetable oil is about 0.1% to 2% (w / w) in an aqueous dispersion. In certain embodiments, the vegetable oil acts as a barrier for gas and moisture exchange (FigureAttorney Docket No.:2024-027-014). In certain embodiments, the vegetable oil acts as a matrix for essential oil and emulsifiers (Figure 4). In certain embodiments, the vegetable oil acts as a controlled release agent for essential oils (Figure 4). In certain embodiments, the vegetable oil acts as an antimicrobial and / or plasticizer (Figure 4).[oni] As used herein, the term “algal oil” refers to a lipid-rich extract obtained from certain species of algae, such as microalgae, and is characterized by a high content of long-chain polyunsaturated fatty acids, such as omega-3 s such as docosahexaenoic acid (DHA) and eicosapentaenoic acid (EP A). Algal oils are produced by cultivating microalgae under controlled conditions, harvesting the biomass, and extracting the oil, which is then refined for use as a nutritional supplement, ingredient in functional foods, infant formula, as a sustainable marinesource alternative for vegetarians and vegans, or other applications. Examples of algal oils include, Schizochytrium oil, Crypthecodinium cohnii oil, Nannochloropsis oil, Chlorella oil, Botryococcus braunii oil, Dunaliella tertiolecta oil, Pleurochrysis carterae oil, or any combination thereof.
[0112] In some aspects, the concentration of the algal oil used in the composition is about 0.01% to about 5% (w / w), about 0.01% to about 4% (w / w), about 0.01% to about 3% (w / w), about 0.01% to about 2% (w / w), about 0.01% to about 1% (w / w), about 0.01% to about 0.5% (w / w), about 0.1% to about 5% (w / w), about 0.1% to about 4% (w / w), about 0.1% to about 3% (w / w), about 0.1% to about 2% (w / w), about 0.1% to 1% (w / w), or about 0.1% to 0.5% (w / w) in an aqueous dispersion. In an embodiment, the concentration of the algal oil is about 0.1% to 2% (w / w) in an aqueous dispersion.
[0113] In an embodiment, the composition or formulation contains at least one plant extract. A “plant extract” as used herein refers to a concentrated preparation or product obtained by using solvents to selectively remove desired active substances or compounds from plant material (such as leaves, stems, bark, fruits, roots, flowers, seeds, or any combination thereof). Plant extracts can be found in various forms, including tinctures, glycerites, decoctions, infusions, distillates and liquids. Examples of plant extracts are essential oils, spice extracts, cold-pressed oils, resins, or solvent extracts such as lecithins and saponins.
[0114] In one aspect, the plant extract is a spice extract. Spices are typically derived from seeds, bark, roots, fruits, or flowers of plants and trees. Spice extracts are concentrated flavors, colors, or actives from spices which can be in the form of tinctures, glycerites, decoctions,Attorney Docket No.:2024-027-01 infusions, and liquids. They are typically made by extracting spice material (such as, for example, vanilla, cinnamon, clove, coriander, cumin, garlic, ginger, mustard, nutmeg, turmeric) with food-safe solvents like alcohol, oil, or water, and then filtering and concentrating the desired compounds. Examples of spice extracts include vanilla, cinnamon, clove, coriander, cumin , garlic , ginger , mustard , nutmeg , turmeric, mint, spearmint, anise, bay leaf, cardamom, pepper, allspice, mace, fennel, fenugreek, carom, nigella, oregano, thyme, sage, basil, curry leaf, lemongrass, galangal, sumac, wormseed, bishop’s weed, caraway, sesame, vetiver, poppy, mullein, and lavender, liquid spice oleoresins, or any combination thereof.
[0115] In some aspects, the concentration of spice extract used in the composition or formulation is in an amount of about 0.01% to about 3% (w / w), about 0.01% to about 2% (w / w), about 0.05% to about 2% (w / w), about 0.01% to about 1% (w / w), about 0.01% to about 0.5% (w / w), about 0.1% to about 3% (w / w), about 0.1% to about 2% (w / w), about 0.1% to about 1% (w / w), about 0.1% to about 0.5% (w / w), or about 0.1% to 0.4% (w / w) in an aqueous dispersion. In an embodiment, the concentration of the spice extract in the composition or formulation is about 0.05% to 2% (w / w) or about 0.1% to about 0.4% (w / w) in an aqueous dispersion.
[0116] In another aspect, the plant extract is an essential oil. Essential oils derived from plants are concentrated, volatile, aromatic liquids extracted from various plant parts, such as leaves, flowers, seeds, bark, roots, stems, fruits, or any combination thereof, using methods like steam distillation, cold pressing, or solvent extraction. These oils contain the characteristic fragrance and flavor of the source plant, comprising numerous small, volatile compounds such as terpenes, phenols, and aldehydes. Examples of essential oils that can be used are essential oils derived from Bay leaf, basil, caraway, cilantro, cinnamon, cardamom, carom, coriander, curry leaf, fennel, fenugreek, galangal, garcinia, lemongrass, mace, matjoram, mint, mullein, nutmeg, oregano, parsley, peppermint, rosemary, sage, sumac, savory, sumac, sesame, spearmint, thyme, amaranth, bergamot, cannabis, eucalyptus, grapefruit, lavender, lemon, lemongrass, lime, mandarin, neem, orange, pandan, rose, Wintergreen, or any combination thereof. In still further aspects, the essential oil can also contain one or more of trans-cinnamaldehyde, cinnamyl acetate, cinnamyl alcohol, linalool, E-2-decanal, limonene, linalyl acetate, a-pinene, 0-binene, methyl chavicol, 1,8 cineole, ocimene, borneol, eugenol, eugenyl acetate, caryophyllene, cuminaldehyde, o-cumenol, myrcene, a-terpineol, sabinene, phellandrene, a-humelene, cannabichromenic acid, eucalyptol, gingerol, zingiberene, allicin, alliin, and ajoene, diallylAttorney Docket No.:2024-027-01 disulfide, diallyl sulfide, and diallyl trisulfide, ally isothiocyanate, limonene, b-pinene, gammaterpinene and a-terpinene, phytol, squalene, pentadecanal, myrcene, citronellal, geranial, camphene, n-octanol, menthol, menthone, 1,8-cineole, erucic acid, a-linolenic acid, carvacrol, thymol, terpinen-4-ol, trans-caryophyllene, myristicin, apiol, azadirachtin, capsaicin, hexyl isovalerate, alpha-cubebene, (E,E)-alpha-famesene, citronellol, geraniol, nerol, menthofuran, 1,8-p-methadiene, 1,4-p-methadiene, thujone, camphor, p-cymene, gamma-terpinene, p-chavicol, dihydrocarvone, trans-craveol, b-bourbonene, verbenone, bornyl acetate, rans-anethole, isoanethole, b-sesquiphellandrene, a-turmerone, b-turmerone, P-bisabolene, curcumin, methyl salicyclate, withanolides, ginsenosides, or any combinations thereof. In an embodiment, the essential oil is derived from clove, anise, thyme, sage, cinnamon, citrus rind, pepper, turmeric, or any combination thereof.
[0117] In some aspects, the concentration of essential oil used in the composition or formulation is in an amount of about 0.01% to about 3% (w / w), about 0.01% to about 2% (w / w), about 0.05% to about 2% (w / w), about 0.01% to about 1% (w / w), about 0.01% to about 0.5% (w / w), about 0.1% to about 3% (w / w), about 0.1% to about 2% (w / w), about 0.1% to about 1% (w / w), about 0.1% to about 0.5% (w / w), or about 0.1% to 0.4% (w / w) in an aqueous dispersion. In an embodiment, the concentration of the spice extract in the composition or formulation is about 0.05% to about 2% (w / w) or about 0.1% to about 0.4% (w / w) in an aqueous dispersion.
[0118] The plant extract (e.g., the at least one spice extract, the at least one essential oil, or a combination thereof) performs various functions depending on the source and its properties. In some embodiments, the plant extract acts as an antimicrobial. In some embodiments, the plant extract acts or functions as an antioxidant. In certain embodiments, the plant extract acts or functions as an antimicrobial (microbicidal or microbistatic towards, for example, bacteria, yeasts, molds, parasites, and viruses). In some embodiments, the plant extract acts or functions as a plant defense elicitor (for example, an essential oil derived from oregano, garlic, peppermint, grapefruit, orange, or any combination thereof can be used as a plant defense elicitor).
[0119] In some embodiments, the composition or formulation further includes at least one emulsifier. In some aspects, the composition or formulation contains sodium alginate, at least one vegetable oil, and / or at least one algal oil, at least one plant extract (e.g., a spice extract or an essential oil) and at least one emulsifier in a ratio in a range of: 100: 10: 1 : 1 to 200: 10:1:1 (sodium alginate:vegetable oil and / or algal oikplant extract:emulsifier), in a ratio in a range of:Attorney Docket No.:2024-027-01100:20:2:2 to 200:10:1:1, or in a ratio of: 100:50:5:5 to 200:10:1:1. In some aspects, the ratio of sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract (e.g., a spice extract or an essential oil), and at least one emulsifier is: 100:20:2:2. In some aspects, the composition or formulation contains sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one spice extract, and at least one emulsifier in a ratio in a range of: 100: 10: 1 : 1 to 200: 10:1:1 (sodium alginate:vegetable oil and / or algal oikspice extract: emulsifier), in a ratio in a range of: 100:20:2:2 to 200:10:1:1, or in a ratio in a range of: 100:50:5:5 to 200: 10: 1:1 In some aspects, the ratio of sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one spice extract, and at least one emulsifier is: 100:20:2:2.
[0120] In some embodiments, the composition or formulation further includes at least one emulsifier. In some aspects, the composition or formulation contains sodium alginate, at least one vegetable oil, at least one plant extract (e.g., a spice extract or an essential oil) and at least one emulsifier in a ratio in a range of: 100: 10: 1 : 1 to 200: 10:1:1 (sodium alginate:vegetable oikplant extract:emulsifier), in a ratio in arange of: 100:20:2:2 to 200:10:1:1, or in a ratio of: 100:50:5:5 to 200: 10: 1:1. In some aspects, the ratio of sodium alginate, at least one vegetable oil, at least one plant extract (e.g., a spice extract or an essential oil), and at least one emulsifier is: 100:20:2:2. In some aspects, the composition or formulation contains sodium alginate, at least one vegetable oil, at least one spice extract, and at least one emulsifier in a ratio in a range of: 100:10:1:1 to 200:10:1:1 (sodium alginate:vegetable oikspice extractemulsifier), in aratio in a range of: 100:20:2:2 to 200:10:1 :1, or in a ratio in a range of: 100:50:5:5 to 200:10:1 :1 In some aspects, the ratio of sodium alginate, at least one vegetable oil, at least one spice extract, and at least one emulsifier is: 100:20:2:2.
[0121] In some embodiments, the emulsifier can be derived or sourced from at least one algal oil, at least one plant extract (e.g., a spice extract and / or an essential oil), or a combination tthereof, or any suitable biocompatible emulsifier. In certain embodiments, the plant extract acts as the emulsifier. In some embodiments, the emulsifier is a suitable biocompatible and biodegradable material other than the plant extract.
[0122] In some embodiments, the plant extract can act or serve as an emulsifier / surface active agent / wetting agent and is derived from a variety of plant sources such as seeds, bark, stem, fruit, vegetable, or any combination thereof. Any suitable emulsifier with hydrophilic lipophilic balance values (HLB) between about 0 to 20 can be used for this invention. ForAttorney Docket No.:2024-027-01 example, the emulsifier with HLB values between about 0 to 19, about 0 to 18, about 0 to 17, about 0 to 16, about 0 to 15, about 0 to 14, about 0 to 13, about 0 to 12, about 0 to 11, about 0 to 10, about 0 to 9, about 0 to 8, about 0 to 7, about 0 to 6, about 0 to 5, about 0 to 4, about 0 to 2, about 0 to 1, about 1 to 10, about 1 to 15, about 10 to 20, about 10 to 18, about 12 to 20, about 12 to 18, or about 8 to 12 can be used for this invention. In an embodiment, the emulsifier is any suitable food grade surface active agent. In an embodiment, the emulsifier is derived from a variety of suitable plant sources. In certain embodiments, the emulsifier is derived from lecithins from various sources (HLB values ranging from about 0-8), modified vegetable oils, saponins (ranging from HLB values about 12-20) from yucca, ginseng, quillaja, chestnut, chickpea, aescins, or any combination thereof. In an embodiment, the concentration of emulsifier is about 0.01% to about 1% (w / w), about 0.01% to about 0.9%, about 0.01% to about 0.8% (w / w), about 0.01% to about 0.7% (w / w), about 0.01% to about 0.6% (w / w), about 0.01% to about 0.5% (w / w), about 0.01% to about 0.4% (w / w), about 0.01% to about 0.3% (w / w), about 0.01% to about 0.2% (w / w), about 0.01% to about 0.1% (w / w), about 0.01% to about 0.5% (w / w), about 0.01 to about 0.1% (w / w), about 0.1 to about 1% (w / w), about 0.1 to about 0.9% (w / w), about 0.1 to about 0.8% (w / w), about 0.1 to about 0.7% (w / w), about 0.1 to about 0.6% (w / w), about 0.1 to about 0.5% (w / w), about 0.1 to about 0.4% (w / w), about 0.1 to about 0.3% (w / w), or about 0.1 to about 0.2% (w / w) in an aqueous dispersion. In an embodiment, the concentration of the seaweed extract is about 0.1 to 1% (w / w) in an aqueous dispersion. In certain embodiments, the emulsifies improve emulsion formation and stability. In certain embodiments, the emulsifier improves dispersion of solid fats in the alginate matrix. In certain embodiments, the emulsifier acts as a plasticizer. In some aspects, the emulsifier is at least one lecithin, at least one quillaja saponin, at least one yucca saponin, at least one ginseng saponin, or any combinations thereof.
[0123] In some embodiments, the plant extracts (e.g., spice extract and / or essential oil) include emulsifiers such as saponins that may be derived from plant sources such as ginseng, legumes such as kidney bean, chickpea, alfalfa, sunflower seeds, asparagus, horse chestnut, tea plant, Quillaja tree, spinach, quinoa, beet root, Yucca schidigera, yam, eggplant, fenugreek, garlic, spinach, oats, liqorice, lentil, nutmeg, sunflower, tea, winter squash, peas, red gram, horse gram, peanuts, thyme, sarsaparilla, lucerne, mung beans, or a combination thereof.Attorney Docket No.:2024-027-01
[0124] In some embodiments, the saponins include barringtogenol, priverogenin, protoaescigenin, protoprimulagenin, bayogenin, glycyrrhetinic acid, hederagenin, oleanolic acid, polygalic acid, quillajic acid, gypsogic acid, medicagenic acid, presenegin, ginsenosides, or a combination thereof.
[0125] In some embodiments, the plant extracts (e.g., spice extract and / or essential oil) include emulsifiers such as lecithins derived from soybean, rapeseed, cottonseed, sunflower, wheat, or a combination thereof.
[0126] In some embodiments, the lecithins include phosphatidylcholine, phosphatidylethanolamine, phosphatidylinositol, phosphatidic acid, phosphaditylserine, phosphaditylglycerol, or a combination thereof.
[0127] In some embodiments, the composition further includes at least one solvent. In some embodiments, the solvent is at least one organic solvent, water, or a combination thereof. Any suitable solvent can be used for this invention. Examples of organic solvents include alcohols and esters, for example, ethanol, ethyl acetate, propanol, isopropyl alcohol, or a combination thereof. In an embodiment, the solvent is water. When the solvent is water, water is present in an amount of about 90% (w / w) to about 95% (w / w). In certain embodiments, the solvent also acts as a dispersing agent for other ingredients. In certain embodiments, the solvent also acts as a plasticizer.
[0128] In some aspects, the composition or formulation comprises at least about 1.0 to 6.0% (w / w) of sodium alginate, at least about 0.2%-l .5% (w / w) of at least one vegetable oil, at least about 0.04% to about 0.5% (w / w) of at least one plant extract, at least about 0.01% to about 0.5% (w / w) of at least one emulsifier, and the balance at least one solvent, such as water.
[0129] In some embodiments, the composition or formulation can be used as a coating on a plant, plant part, food, or food product. In some aspects, the composition or formulation can be used as a coating on a perishable food product, such as one or more fruits, seeds of fruits, vegetables, seeds of vegetables, fungi, or any combination thereof. In some aspects, the composition or formulation can be used as a coating for any plant, a part of a plant, fruit, vegetable and / or fungi (e.g., mushrooms) that is sensitive to ethylene (C2H4) which leads to changes such as de-greening, tissue softening, an increase in sugar and soluble solids, and a reduction in acidity, all of which are indicative of ripening. It was surprisingly discovered that the composition or formulations of the present disclosure can slow or delay ripening-relatedAttorney Docket No.:2024-027-01 changes when compared to fruits and / or vegetables that are not coated with the composition or formulation described herein. For example, coating a fruit, a vegetable, a fungi, or any combination thereof with the composition or formulation described herein: (1) limits the diffusion of ethylene from inside the fruit, vegetable and / or fungi to the outside, effectively retaining or modulating ethylene concentration around the fruit, vegetable and / or fungi; (2) helps to control oxygen and ethylene flow, thereby reducing respiration rates and delaying the enzymatic and genetic activation triggered by ethylene, thereby slowing the ripening process; and / or (3) helps preserve quality, firmness, and freshness (e.g., shelf-life) of fruits, vegetables, and / or fungi during storage, shipping, and retail handling, decreasing spoilage and waste. In certain embodiments, the composition or formulation is used for a coating on various surfaces, such as, for example on a plant and / or on one or more fruits, seeds of fruits, vegetables, seeds of vegetables, fungi (e.g., mushrooms), or any combinations thereof.
[0130] In one embodiment, at least 50%, at least 55%, at least 60%, at least 65%, at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, at least 95%, at least 98%, at least 99%, or at least 100% of the surface area of a plant, plant part, food, or food product is coated with the composition or formulation described herein.
[0131] In yet another embodiment, the thickness of the coating formed on a plant, plant part, a food, or food product after deposition of the liquid composition or formulation range between about 1 nanometer (nm) to about 0.5 millimeter (mm) For example, about 1 nm to about 0.45 mm, about 1 nm to about 0.4 mm, about 1 nm to about 0.35 mm, about 1 nm to about 0.3 mm, about 1 nm to about 0.25 mm, about 1 nm to about 0.2 mm, about 1 nm to about 0.15 mm, about 1 nm to about 0.1 mm, or about 1 nm to about 0.05 mm.
[0132] The primary ingredient of the composition or formulation, namely, the seaweed extract (e.g., sodium alginate), can be derived from oceans without encroaching on any land resources (agriculture, animal feed, forestry, etc.). In certain embodiments, the composition / formulation or the coatings developed by using the composition provides specific functions such as barrier properties in terms of moisture or gas transmission rates (ethylene, CO2, and O2), which is critical to extend shelf-life different gas dependent climacteric fresh food products or produce (e.g., Bananas, tomatoes, apples, pears, mangoes, avocados, peaches, plums, apricots, melons) and non-climacteric fresh food products or produce, for example, climacteric fruits are known to be sensitive to ethylene at ppm levels and ripen rapidly in its presence.Attorney Docket No.:2024-027-01
[0133] In certain embodiments, the compositions or formulations described herein are multiphase liquids (for example, a combination of dispersion and emulsion (e.g, an aqueous dispersion)) that can be bulk manufactured to form shelf-stable dry powders by employing spray drying. In an embodiment, the dry product can be easily reconstituted in water or another solvent to provide properties similar to the native dispersion without the need for sophisticated blenders. Having shelf-stable dry forms will drastically reduce the cost of transport and logistics (e.g., storage, pumping, etc.). In certain embodiments, the liquid formulations can be prepared from the powder on on-demand basis wherever necessary. In certain embodiments, the compositions are water-based, and they do not rely on inflammable organic solvents. In certain embodiments, the compositions are applied utilizing electro spraying or ultrasound-assisted electro spraying that increases the mass transfer efficiency and reduces the wastage of coating material that would be otherwise over-sprayed, thus reducing the biological and chemical oxygen demand (BOD and COD) of the effluent streams.
[0134] In an embodiment, the composition forms a thin coating that is invisible and flavorless on plants (e.g., grasses, vegetable plants, flowering plants, shrubs (e.g., fruit bushes) and / or combinations thereof), parts of plants (e.g., leaves, flowers, fruits, seeds obtained from fruits, vegetables, seeds obtained from vegetables, fungi, or any combinations thereof. There is no requirement for the coating to be washed off (e.g., the fruit and / or vegetable washed or cleaned prior to consumption by a human). In other words, the fruit, vegetable, seeds obtained from fruits and / or vegetables, and / or fungi are capable of being consumed as is. The composition can be fine-tuned to deliver various bioactive agents such as antioxidant (e.g., plant polyphenols, vitamin C, etc.), antimicrobial (e.g., organic acids, aldehydes, fatty acids etc.), and pesticidal agents (plant oils, resins, etc.) in the matrix. The composition can be fine-tuned to provide sheen / gloss / other functionalities depending on the target products (e.g., for cherries or roses). The composition is applied prior to harvest of fresh produce to improve the yields by decreasing the ill-effects of various physical, chemical, and biological factors, or can be applied post-harvest. In certain embodiments, the composition can alter the sprouting of seeds, tubers, and other biologically active materials by either simulating or delaying the onset of sprouting.
[0135] III. A process for precision coating
[0136] In another embodiment, a process for precision coating is disclosed using the composition or formulation described in Section II. In an embodiment, the process employsAttorney Docket No.:2024-027-01 coating one or more biological materials using electro spraying, an ultrasound-assisted electro spraying, or a combination thereof. To coat a biological material using electro spraying, ultrasound-assisted electro spraying, or a combination thereof, the composition or formulation must be provided in the form of a liquid, such as a multi-phase liquid (e.g., an aqueous dispersion). In some embodiments, the composition or formulation described in Section II may be in the form of a powder or solid. In some embodiments, when the composition of Section II is in the form of a powder (e.g., a spray-dried powder), the process involves redispersing the powder (e.g., spray-dried powder) in a suitable solvent or vehicle. Examples of suitable solvents or vehicles include organic solvents such as alcohols and esters, such as ethanol, ethyl acetate, propanol, isopropyl alcohol, as well as water or combinations thereof. In some aspects, the solvent or vehicle is water. Similarly, if the composition or formulation described in Section II is in the form of a solid, the process involves transforming the solid into a liquid in a suitable solvent or vehicle. A liquid form could be prepared by dispersing the solid formulation in water using agitation, such as by, stirring with a paddle mixer or more rigorous agitation in the form of high shear mixers such as throttling valves and rotary homogenizers to create a liquid.
[0137] Once the composition or formulation described in Section II is provided or supplied in liquid form (e.g., as an aqueous dispersion), electro spraying, ultrasound-assisted electro spraying, or a combination thereof can be used to precisely coat the composition or formulation onto one or more biological materials. In other words, precision coating can be used to coat one or more biological materials with the liquid composition or formulation. As used herein, the phrase “precision coating” refers to the controlled application of a coating material, such as the composition or formulation described in Section II, in the form of a liquid (e.g., as an aqueous dispersion), onto one or more biological materials with high accuracy to achieve exact and repeatable thickness, coverage, and functional properties. In some aspects, the biological materials include plants (e.g., grasses, vegetable plants, flowering plants, shrubs (e.g., fruit bushes) and / or combinations thereof), parts of plants (e.g., leaves and / or flowers), and food products, such as, fruits, seeds obtained from fruits, vegetables, seeds obtained from vegetables, fungi, or any combinations thereof. In some aspects, the food products are fresh, meaning they are perishable.
[0138] In some aspects, at least 50%, at least 55%, at least 60%, at least 65%, at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, at least 95%, at least 98%, at least 99%, or atAttorney Docket No.:2024-027-0I least 100% of the surface area of the biological materials is coated with the composition or formulation described herein.
[0139] In another embodiment, the composition or formulation of Section II can be used to coat the fiber-based materials. As used herein, the term “fiber-based materials” refers to materials that consist mainly of fibers (e.g., greater than 50% are fibers, greater than 60% are fibers, greater than 70% are fibers, greater than 75% are fibers, greater than 80% are fibers, greater than 85% are fibers, greater than 90% are fibers, greater than 95% are fibers, greater than 98% are fibers, greater than 99% are fibers) either natural (from plants, animals, or minerals) or synthetic (manufactured from chemicals), that are processed and combined to form sheets, boards, or molded items. These materials are characterized by their high length-to-width ratio of the constituent fibers, as well as properties like renewability, biodegradability, and strength. Examples include paper, paperboard, cardboard, molded fiber products (e.g., paper cups, plates, bags, etc.), fiberboard, tissue products, or any combinations thereof. For example, in one aspect, the compositions or formulations described in Section II can be used to coat the inner layer of a paper bottle. In some aspects, the compositions or formulations described in Section II can be used to coat one or more sides of a fiber-based material, or the entire fiber-based material.
[0140] In some aspects, the compositions or formulations described in Section II can be used to coat one or more sides of gusseted pouches used for sauces and gravies. In some further aspects, the compositions or formulations described in Section II can be used to coat one or more sides of bottles or containers (e.g., bioplastic, or fiber-based materials) used for liquids or beverages such as, for example, sports drinks (e.g., Gatorade, Liquid I.V.), soft drinks, water, tea, meal supplements, protein drinks, fruit drinks, dairy and non-dairy alternatives (e.g., soy, almond, cashew, oat, or plant based milk alternatives).
[0141] Compared to coating with alternative, simpler options like dipping or using compressed air-activated spray nozzles, electro-spraying provides multiple benefits such as higher mass transfer efficiency, lesser drip and wastage of solution, a thin, uniform layer, and quicker drying, among others.
[0142] In an embodiment, an electro sprayer prototype design consists of a high voltage source connected to a syringe needle, fed with a liquid from a syringe using a screw pump, as shown in Figure 10. This assembly enables electrospray coating of biological materials placed on the grounded platform underneath the needle tip under the given process parameter ranges:Attorney Docket No.:2024-027-01Flow rate (about 0.1 to 30 mL / h), voltage (about 0.1-15 kV), distance between the needle tip and collector (about 1 to 15 cm).
[0143] Due to introduction of charge as means of aerosolizing, electro spraying leads to finer liquid droplets with net non-zero charge (+ or - depending on polarity applied at source) which attracts the particles to a neutral (grounded) substrate to be coated. This results in lesser liquid being picked up and more uniformly coated across the surface compared to a dip coating as shown in Figure 11. In this experiment, ping pong balls were used as test substrates since they have negligible piece to piece variation in terms of surface area, roughness, material composition, and risk of inherent mass loss from respiration- all of which apply to fresh fruits or vegetables.
[0144] The drying kinetics that plot moisture ratio (Weight ratio of the liquid on the basis of initial weight as 100%) versus time are one way to monitor drying. The kinetics show that electrospray coated ping pong balls dried almost 4 times faster (rate constants for ES: 0.067, for Dip: 0.015) than the dip coated ones. This could be attributed to less liquid being picked up initially as well as more uniform and thin distribution of liquid on the same surface area, applicable between the two treatments (Figure 12).
[0145] In an embodiment, the precision coating is performed using an electro spraying. In an embodiment, the electro spraying process parameters are as follows: voltage (about 0.1 kV to 100 kV) of the electro spraying equipment, and conductivity (about 0.1 pS / cm to 50 mS / cm), concentration (about 0.1 % to 10% (w / w) dissolved solids), surface tension (about 1 mN / m to 100 mN / m ), and viscosity (about 0.001 mPa.s to 10,000 mPa.s) of the solutions being electro sprayed.
[0146] Some electrostatic spraying processes have practical risks of - a) Arcing - which is dielectric barrier discharge of electricity through the air from the nozzle to the grounded collector, to the food item being coated, or the nearest grounded surface of the equipment assembly- whichever is the path of least resistance. This leads to current surges that can cause damage to the high voltage source and to whatever material is on the receiving end of the discharge- similar to a lightning strike. b) Ozone generation - The dielectric barrier discharge creates plasma in situ (ionized gas molecules and atoms) that leads to the generation of ozone andAttorney Docket No.:2024-027-01 potentially other byproducts harmful to human health. The generation of ozone is sensible (since human olfactory threshold is < 0.1 ppm) and occurs at certain conditions of high voltage, low feed flow rate, high surface tension, high viscosity, high concentration, etc.) and presents human health and safety risks in the absence of engineering controls to mitigate the risks.
[0147] Arcing is basically the electric energy getting leaked out of the system into the surrounding air which reduces the energy efficiency and increases the risks enlisted above.
[0148] Nebulization with compressed air or other fluids will negatively affect the electro spraying at the cost of energy efficiency since air and other aerosolizing media behave like dielectrics and absorb energy, leaving less for droplet formation and droplet charging.
[0149] The said risks could be reduced or completely eliminated by aiding the nebulization of solutions with said properties (high viscosity, high surface tension, high dissolved solids concentration, or inflammable components) either upstream of electrostatic spraying (ESS) or at the point of ESS using an ultrasonic nebulizer with process parameters ranging as follows: Power (0 kW to about 10 kW), input voltage (0 V to about 250 V), input power frequency (0 to about 60 Hz), ultrasonic frequency of output (about 20 kHz to 40 KHz), working temperature (0 °C to about 100 °C), and droplet size of nebulized fluid (about 0.1 pm to 100 pm).
[0150] In certain embodiments, the process for precision coating includes ultrasound-assisted ESS.
[0151] Using the disclosed precision coating methods can drastically reduce the energy input of drying (hot air-drying tunnels) or altogether eliminate the unit operation, which is a major energy hotspot for the fresh produce industry, leading to cost savings.
[0152] IV. A method for improving the shelflife and marketability of biological materials
[0153] In another embodiment, a method is disclosed for improving the shelf life and marketability of biological materials. In an embodiment, the biological materials include plants (e.g., grasses, vegetable plants, flowering plants, shrubs (e.g., fruit bushes) and / or combinations thereof), parts of plants (e.g., leaves and / or flowers), and food products, such as, fruits, seeds obtained from fruits, vegetables, seeds obtained from vegetables, fungi, or any combinations thereof. In some aspects, the food products are fresh, meaning they are perishable.
[0154] The method involves treating biological materials with an effective amount or sufficient amount of the composition or formulation of Section II to coat at least 50%, at leastAttorney Docket No.:2024-027-0155%, at least 60%, at least 65%, at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, at least 95%, at least 98%, at least 99%, or at least 100% of the surface of the biological material.
[0155] In another aspect, a method is disclosed for slowing the ripening of perishable food products. Examples of perishable food products include Suits, seeds of fruits, vegetables, seeds of vegetables, fimgi, or any combination thereof. Such perishable food products are coated with an effective amount or sufficient amount of the composition or formulation of Section II to coat at least 50%, at least 55%, at least 60%, at least 65%, at least 70%, at least 75%, at least 80%, at least 85%, at least 90%, at least 95%, at least 98%, at least 99%, or at least 100% of the surface of the perishable food product.
[0156] Experiments were conducted in accelerated shelf-life conditions over 24 hours (Temperature elevated and humidity decreased compared to commercial conditions) to show that an emulsion formulation prepared using commercial sodium alginate (as a proxy for alginate rich seaweed extract fraction) was comparable in terms of barrier performance (retarding mass loss due to inherent respiration) to the disclosed composition or formulation prepared using seaweed extract as described in Sections I and II. (Figure 13). This formulation contained about 1.8% (w / w) seaweed extract, about 0.2% (w / w) coconut oil, about 0.02% (w / w) oregano essential oil, and about 0.02% (w / w) soy lecithin dissolved and dispersed in water. Formulations with commercial alginate included about 1% (w / w) medium viscosity sodium alginate or about 5% (w / w) low viscosity alginate with the relative ratio of alginate to all other non-water ingredients remaining the same.
[0157] Emulsion formulations created with commercial sodium alginates (low viscosity: LVSA and medium viscosity: MVSA) as proxies for formulations with seaweed extract showed comparable barrier performance between formulations (variation in viscosity dependent on variation in molecular weight distribution) and between dip and electrospray (ES) coating. (Figure 14).
[0158] In another accelerated shelf-life experiment with strawberries, the ratio of coconut oil (vegetable oil) to carvacrol (essential oil) (CO:EO) was varied. This was done to test the effect on barrier property to weight loss and visual color. Beyond CO:EO :: 7:3, obvious change in visual color (greying) and loss of barrier properties was observed as assessed from the weight loss index value returning closer to 1. (Figure 15).Attorney Docket No.:2024-027-01
[0159] Shelf-life studies were observed to monitor weight loss and fungal incidence (from natural microbiota present on berries) under typical commercial supply chain conditions: 15 days with refrigeration temperature (< 4°C) and high humidity (>90%) for berries coated with the commercial sodium alginate containing emulsion. This was applied via dip coated or electrostatic spray coating. Both the coating methods showed clear benefits in terms of reducing weight loss and fungal incidence at the end of shelf-life. The reduction in fungal incidence due to ES coating lower than dip coating signifying that the antifungal performance could further be improved with better ES coating. (Figure 16). Without wishing to be bound by a theory, it is believed that the compositions or formulations described herein, prepared by the methods described herein in Section I, can be employed to control the rate of sprouting (either delayed or stimulated sprouting) in a dose-dependent manner.
[0160] This compositions or formulations of the present disclosure extend the shelf-life of perishable or fresh food products (e.g., produce and other foods, such as, fruits, vegetables, seeds of fruits and / or vegetables and / or fungi), and other perishable biological materials to reduce food loss: “shrink” in the supply chain- about 20-50% ib average and can be up to 100%. The shelflife extending aspect of the invention can reduce the shrink down to about 10% or lower based on lab studies simulating the commercial supply chains.
[0161] The compositions or formulations described herein provide more time for distribution and sale of various food products or produce (e.g., fruits, vegetables, seeds of fruits and / or vegetables, and / or fungi) to various agents in the supply chain and improve their revenue. This can result in increase in the radius of distribution for highly perishable produce - for or example, greenhouse grown organic strawberries could be distributed and sold in a 100 mile radius with extended shelf-life as opposed to the current situation with 10 mile radius (new markets); and trans-Atlantic flower shipments that witness -50% loss in their journey from South America to North-west Europe could bring down the loss to less than 10% (lesser loss).
[0162] The disclosed compositions or formulations are edible and free of allergens. All the ingredients used have received GRAS (Generally Recognized as Safe) approval from the FDA. The composition or formulation can be compliant with USDA Organic Standards (therefore suitable for use on organic fruits and vegetables).Attorney Docket No.:2024-027-01
[0163] The precision coating methods (quick drying coating) disclosed herein can drastically reduce the energy input of hot air drying or altogether eliminate the unit operation, providing major energy, cost, and sustainability benefits to end users.
[0164] The present disclosure is illustrated and further described in more detail with reference to the following non-limiting examples.EXAMPLES
[0165] Example 1
[0166] Process for preparing compositions / formulations: Liquid dispersion / emulsion and solid powder
[0167] The compositions / formulations are formed by dispersing the seaweed extract in water using heat, high shear or a combination of the two until the alginate is completely hydrated.Depending on the nature (Hydrophilic Lipophilic Balance or HLB value) of the emulsifier, it is separately dissolved either in the aqueous seaweed extract dispersion (hydrophilic emulsifier) or in the oil phase comprising a mixture of vegetable oil and spice extracts (hydrophobic emulsifier). Emulsifiers with HLB values < 6 are dissolved in the lipid phase, those with HLB between ~ 6 to 10 are dissolved in either the lipid or water phase, whereas those with HLB values > 10 are dissolved in the aqueous phase.1. The aqueous and lipid phase is combined per the compositions described herein.2. The two immiscible phases are emulsified with a high shear homogenizer with RPM varying between 100 to 20,000. The process may be sped up by pre-heating the two phases separately or together due to which viscosity and surface tension drop aiding emulsification.3. The mixture (dispersion of alginate and emulsion of solid and liquid fats) is kept above the melting point of the vegetable oil to ensure maximum fluidity (for example, 28 °C for coconut oil).4. The emulsion is then spray dried to achieve a low moisture free flowing powder, comprising spherical particles and randomly shaped flakes using the following process parameters: a. Inlet feed rate ~ 5 - 500 mL / h (preferably for lab scale spray dryer about 3-9 mL / h) b. Inlet temperature ~ 90 - 200 °C (preferably about 100-140 °C)Attorney Docket No.:2024-027-01 c. Inlet air speed ~ 80-3000 mL / min (preferably about 1400 - 2000 mL / h) d. Aspirator aid speed - 5 - 50 m3 / h (preferably about 20-30 m3 / h) e. Outlet temperature being about ambient - 90°C (preferably ambient to 27°C) The dried formulation can be reconstituted in water using relatively very low energy input compared to the manufacturing process (for example, gentle stirring using - 300 rpm on a magnetic stir bar, or a household kitchen blender) to provide an emulsion with material properties similar to the native emulsion (used as the feed for spray drying). However, temperature range of about l-100°Cand RPM range of about 30 - 20,000 may be utilized to reconstitute the powder in water or other solvents to get the liquid formulation. This would provide a straightforward method for end users (for example, farmers or fruit packers) to prepare the formulation / emulsion in fields without needing any sophisticated knowledge or technology. Particle size distribution data provided in the following content shows similarity in the two emulsions (native: original emulsion and emulsion redispersed from spray dried powder) in terms of median particle size and distribution. (Figure 5) The PSD of spray dried powder shows that dispersed materials in the emulsion form aggregates after drying (Figure 6). The barrier properties of the films (and coatings) formed from casting the liquid emulsion can be controlled based on the composition of the emulsion. Longer fatty acids and bigger acyl glycerol molecules are better barriers to water vapor transmission compared to shorter chained fatty acids and small essential oil lipid molecules (measured by water vapor transmission rate WVTR). (Figure 7) Contact angle of emulsions therefore surface tension and wettability can be modified with the selection of emulsifier as shown in Figure 8. Reducing surface tension has benefits for fluid transport (pumping), wetting, and with unit operations that are part of this invention (spray drying, electro spraying, ultrasound assisted electro spraying).Attorney Docket No.:2024-027-01
[0168] The emulsifier in the native emulsion could help improve the total solids yield of spray drying (as it functionally ensures more homogenous oil and fat phase distribution) and choice of emulsifier could help control the yield. (Figure 9)
[0169] Example 2
[0170] Process for making various seaweed extract fractions from sugar kelpSaccharina latissima) using the green biorefinery approach and their compositions1. Drying / milling: a. Freshly harvested sugar kelp {Saccharina latissima') from Connecticut coast was stored at 4-10 °C until further processing. b. Three to five pounds of fresh sugar kelp was taken out and washed in cross stack container with DI water for 3 cycles. During each wash, fresh sugar kelp was gently kneaded for 5 minutes without breaking the tissue. c. The washed kelp was aligned on the dehydrator racks, with thickness of 1 -2 inches. d. Turn on dehydrator to allow forced air to gently dry the loaded sugar kelp at 40°C (least conservative T range: 20°C to 70°C; optimal range 30-50°C), for approximately 48 h. e. Once the fresh sugar kelp strips moisture content reached 5-18% (optimally 5- 8%) the brittle dried sugar kelp sheets were transferred to a mill. f. The milled content was passed through a sieve shaker with 80-mesh sieve. g. The product coming out from the 80-mesh sieve was stored in a Ziploc bag with a desiccant pouch. The content retained on the 80-mesh sieve were reground for one or more cycles to make them small enough to pass through this sieve. The ground material was collected and stored as described.2. Extraction- 1: a. Dried sugar kelp powder was mixed with DI water at 1 :(14-50) w / w ratio. One of the different types of extraction strategies was applied: i. Citric acid was added at 1 : 1 w / w ratio with respect to sugar kelp powder, or ii. Carbonic acid was added by applying 1 bar to 25 bar (optimally 3-10 bar) of pressure of compressed CO2, orAttorney Docket No.:2024-027-01 iii. Acetic acid was added to achieve 0.05M-1M (optimally 0.1M-0.3M) final concentration in the mixture, resulting pH should be 2.8 -3.0, or iv. H2O2 was added at (0.1 -15): 1 w / w (optimally 0.5-1.5:1 w / w) with respect to sugar kelp powder, or v. Ultrasound was applied at 10-100% amplitude, 700W, for 5-60 min. b. Resulting mixture was allowed to incubate / react for Ih to 7 d at 4°C - 180°C (optimal range 20°C-130°C), depending on different types of extraction strategies applied. The different methods can be used to fine tune the viscosity desired for the sodium alginate rich fraction. aration- 1 : a. Mixture achieved from extraction- 1 was transferred to a 200-mesh strainer to let soluble aqueous phase (SI) to separate from the insoluble particles (Pl) under the force of gravity b. SI was the laminarin rich fraction that could be used for making nutritional supplements, therapeutics, tissue engineering, etc.4. Extraction-2: a. Insoluble particles (Pl) achieved was then mixed with DI water at (7-36): 1 w / w ratio with respect to initial sugar kelp powder, depending on different types of acid / oxidant added. b. Na2COs was added at 0.5 : 1 w / w ratio with respect to initial sugar kelp powder. c. The mixture was allowed to mix well under vigorous stir at 40°C for 3h d. Resulting mixture have a viscosity ranging from 2 mPa s to 40,000 mPa-saration -2: a. Viscosity of mixture, if higher than 1000 mPa-s, was adjusted to be 10-1000 mPa s by dilution with DI water or by modifications of the acid extraction unit operation that resulted in lower viscosity sodium alginate rich fraction. b. The mixture was then centrifuged at 4,000 rpm for 10 min at temperatures not greater than 30°C to separate the soluble aqueous phase (sodium alginate rich fraction) and insoluble particles (cellulose rich fraction P2). c. Sodium alginate rich fraction achieved sodium alginate concentration ranging between 0.5 to 10% was then used in making formulations for food preservation.Attorney Docket No.:2024-027-01
[0171] The cellulose rich (P2) fraction with majority of cellulose with traces of other biomaterials in the dry matter was dried and stored. This fraction can be used as a cellulose source for a variety of uses such as fermentation, packaging, material bulking, substrate for mushroom and other fungal growth, etc.
[0172] EXAMPLE 3
[0173] Sugar kelp Saccharina latissima) was farmed and harvested in April 2023 from Fishers Island Sound, Connecticut, USA. The collected biomass was triple washed in tap water and air dried using a food grade commercial dehydrator (Commercial Dehydrators America, TX, USA) at 35°C until weight was constant. The dried sugar kelp was milled into powder using a high-speed grain grinder (Yaetek HC-500, Shanghai, China). Powder particles that passed through 80-mesh sieves were collected and stored in ZipLoc™ bags with desiccant (Humidity Sponge™, Control Company, TX, USA) until future use. The mixture of CO2 in water was generated using a household sparkling water maker (SodaStream, NY, USA) following the manufacturer’s manual. A pH meter (Orion Star™ A211, Thermo Scientific, MA, USA) was used to monitor the pH. Citric acid, sodium carbonate (NaiCOs), and sodium alginate (>80 % pure) were purchased from Sigma- Aldrich Corp (St. Louis, MO, USA). Ethanol (200 proof) was purchased from Greenfield global (Brookfield, CT, USA). Pullulan standard kit was purchased from Agilent Technologies (PSS-PULKIT, Polymer Standards Service, MA, USA).
[0174] Moisture and ash contents of sugar kelp powder and different fractions out of the simplified green biorefinery were tested following a protocol modified from AOAC method 925.09 and AOAC method 942.05 (A. International, Official Methods of Analysis of AOAC International, AOAC International). Briefly, approximately 2 g of each sample was weighed in a crucible and recorded as W0. The samples were then heated in a muffle furnace (Thermo Scientific™ Thermolyne™, Waltham, MA, USA) at 105°C until no further weight loss was observed. The samples were allowed to cool in the muffle furnace to below 60°C and weighed. The weight was recorded as Wl. The furnace temperature was subsequently raised to 600°C, and the samples were heated for another 2 hours. The samples were allowed to cool in the Muffle oven to below 60°C and weighed. The weight was recorded as W2.
[0175] The moisture and ash content were calculated as follows:
[0176] Moisture content = (W0-W1 ) / W0 * 100Attorney Docket No.:2024-027-01
[0177] Ash content = W2 / W0 * 100
[0178] The simplified green biorefinery is carried out following the flow diagram in Figure 1. Ten grams (10 g) of dried sugar kelp powder was mixed with 600 mL of extraction liquid to achieve 1.6% solid content. The mixture was then allowed to mix for 20 ± 4 h under ambient conditions. Ultrasound was applied via a probe sonicator (Fisherbrand™Model 705 Sonic Dismembrator, Thermo Fisher, USA) with an ! / 2inch probe under constant magnetic stirring. Extraction liquids and ultrasound conditions are listed in Table 1.Attorney Docket No.:2024-027-01with freshly prepared carbonic acid using a household sparkling water maker (SodaStream, NY, USA), and pH 2 was achieved with 2% citric acid. The resulting mixture was separated using a 200-mesh strainer. The soluble fraction collected was concentrated using a rotary evaporator under reduced pressure to remove excess water and freeze-dried to achieve supernatant 1 (SI). Precipitate 1 (Pl) was collected and mixed with deionized (DI) water until the total volume reached 500 mL. Two and a half grams (2.5 g) of Na CC was added to adjust the pH to above 10 and stirred at 40°C for 3 hours. Extracted mixture was separated by centrifugation at 8000 rpm for 20 minutes. Supernatant 2 (S2) and precipitate 2 (P2) were collected. A hydrochloric acid (HCl)-based extraction was carried out to serve as a benchmark comparison. An extraction modified from conventional method was carried out as follows: Ten grams (10 g) of dried sugar kelp powder was mixed with 600 mL of 0.1 M HC1 to achieve 1.6 % solid content. The mixture was then allowed to mix for 20 ± 4 hours under ambient conditions. Resulting mixture was separated using a 200-mesh strainer. With the precipitate collected and mixed with DI water until the total volume reached 500 mL. Two and a half grams (2.5 g) of NazCCh was added to adjust the pH to above 10 and stirred at 40°C for 3 hours. Extracted mixture was separated by centrifugation at 8000 rpm for 20 minutes. Supernatant 2 (S2) and precipitate 2 (P2) were collected.
[0180] The crude yield of all fractions was calculated as the weight percentage of dried powder from SI, S2, and P2 relative to the total weight of dried seaweed powder initially used. SI and S2 fractions were freeze-dried, while P2 was heat dried using a convection dehydrator at 50 °C until weight was constant.
[0181] The purity of sodium alginate in S2 was determined using a modified ethanol precipitation process, adapted from conventional alginate purification methods known in the art. Basically, a known amount of the mixture of S2 and P2 was added to five times its volume of ethanol, added dropwise under continuous stirring to precipitate the alginate. The precipitate was collected, dried, and rehydrated in DI water to restore the volume to the initial level. The resulting suspension was centrifuged at 8000 rpm for 10 minutes to separate the supernatant.Attorney Docket No.:2024-027-01
[0182] The supernatant was then subjected to another round of ethanol precipitation under the same conditions. After decanting the supernatant, the final precipitate was dried in a fume hood until a constant weight was achieved. This dried product was considered purified sodium alginate. The purity of S2 was expressed as the weight ratio of the purified alginate to the weight of S2 obtained from the same amount of mixture before purification.
[0183] Fourier-Transform Infrared Spectroscopy (FTIR) measurements were taken on each of the fractions obtained from the simplified green bio-refinery, as well as conventional sodium alginate purchased from Sigma Aldrich (Saint Louis, MA, USA). FTIR spectra were recorded using a Fisher Scientific Nicolet Is5 Spectrometer equipped with an all-diamond crystal attenuated total reflectance (ATR) accessory (iD7 ATR, Thermo Fischer Scientific Inc., Waltham, MA, USA) in the wavelength region of 500-4000 cm1and analyzed using OMNIC software version 8.0. All measurements were carried out in single-beam reflectance mode, and blank background calibration was carried out between switching samples. Each measurement represented average spectrum of a total of 64 scans. Spectra were collected and converted into transmittance between 400 and 1800 cm1.
[0184] Separated and lyophilized samples were dissolved in Milli-Q water at 1 mg / mL. Samples were allowed to be fully hydrated at 4°C for overnight and let possible particles, dusts, and impurities to form sediments on the bottom at ambient condition for 24 hours and then injected without filtration. Separation by high-performance size exclusion chromatography (SEC) was conducted using a size exclusion chromatography / gel permeation chromatography (SEC / GPC) with Waters GPC-1 (1515 HPLC Pump and Waters 717Plus Autoinjector) liquid chromatography system coupled with a Waters 2414 refractive index detector and a Phenomenex PolySep-SEC P-5000 column. Ultrapure water with 0.1 M sodium nitrate was used as the mobile phase, at 40°C with a flow rate of 1 mL / min. A pullulan calibration kit was used as standards to calibrate the system and serve as quality control.
[0185] Viscosity of freshly collected S2 was assessed using a rotational viscometer (ViscoQC 100, Anton Paar, Graz, Austria) at 20°C.
[0186] Minerals and hazardous heavy metal elements (As, Cd, Cr, Pb) were detected in each fraction using inductively coupled plasma optical emission spectroscopy (ICP-OES) (iCAP 6500, Thermo Fisher Scientific, Waltham, MA). Briefly, samples from the simplifiedAttorney Docket No.:2024-027-01 green biorefinery were oven-dried and ground. The fine powders were weighed and placed into digestion tubes with 5 mL plasma pure HNO3. Samples were digested in a hot block at 115°C for 45 minutes. After cooling, the samples were further digested with an additional ImL of FhChfor 20 minutes at 115 °C. The digests were then diluted to 50 mL using DI water. To validate the measurements, standard reference materials (NIST-SRF 1570a and 1547, Metuchen, NJ) were prepared and analyzed by the same procedure. Blank and spiked samples at different levels were used for the calibration and Yttrium (Y) was used continuously as an internal standard.
[0187] Ultrasound was applied during the acid pre-treatment step. Box-Behnken Design (BBD) was applied to optimize the pre-treatment step only. The alkali conversion step which involves usage of Na2CC>3 was kept consistent throughout all the groups. The independent variables studied during the pre-treatment step were sonication amplitude (A), sonication time (B), and pH of the extracting media (C). Their ranges were determined based on previous studies of seaweed biorefinery. Conditions of each factor and the experimental design are shown in Table 1, including 5 replicates of the center points. All factors and responses were scaled to a standardized range of 0-1 to ensure that the impacts of different factors were represented equally, regardless of their original magnitudes. Statistical analysis was performed using Python programming with Jupyter Notebook to evaluate the significance of the models and the effects of the independent variables on the response variables. Analysis of variance (ANOVA) was conducted using a Fisher’s F-test. The p-value and F-value were used to assess model adequacy and significance. The models for energy output of the sonicator, viscosity, and the yield of the sodium alginate (S2) were found to be significant.
[0188] To identify the optimal conditions for maximum sodium alginate (S2) yield, bound- constrained numerical optimization was performed on the fitted second-order response surface model using Python’s SciPy library. The objective was to maximize the alginate yield, and constraints were applied to keep pH within the range of 2-7 and energy within 5.2-552.7 kJ. The optimization results were used to identify the predicted maximum yield and corresponding input conditions.
[0189] Results
[0190] The simplified two-stage green biorefinery extraction process and conventional extraction are compared in Figure 1A and Figure IB. The simplified green biorefinery is aAttorney Docket No.:2024-027-01 streamlined adaptation of the conventional process, designed to simplify operations while maintaining efficiency. This approach was chosen because alginate, initially present in the form of insoluble calcium alginate within the matrix of sugar kelp cell walls, needs to be converted into its soluble form, sodium alginate, for extraction and utilization. Although direct conversion of calcium alginate to sodium alginate is possible through ion exchange, researchers have found that an intermediate step — first converting calcium alginate into alginic acid in an acidic environment and then converting alginic acid into sodium alginate — improves efficiency and yields. This two-step conversion ensures better accessibility and recovery of the alginate. Studies have demonstrated that at least two stages are critical for maximizing sodium alginate conversion: an acidic pre-treatment stage and an alkaline extraction stage. Acidic pre-treatment facilitates hydrolysis under acidic conditions, reducing viscosity and improving accessibility for downstream processing. The alkaline extraction stage then converts alginic acid into sodium alginate, rendering it soluble.
[0191] In the simplified green biorefinery, solvent rehydration, which is a conventional step used for decolorization and increasing tissue permeability, was eliminated to reduce time and reagent use. Instead, an ultrasound module was introduced to compensate for the absence of solvent rehydration by providing the energy needed to disrupt cell wall integrity, making structural molecules more available for extraction. The ultrasound-assisted acidic fractionation stage was to selectively extract acid-soluble fractions, primarily fucoidan and laminarin, while leaving acid-insoluble fractions like alginic acid and cellulose intact.
[0192] The insoluble fraction from the first stage then proceeded to the alkaline extraction stage to convert alginic acid into sodium alginate. Sodium alginate can then deem soluble and be separated from the alkaline-insoluble fraction, predominantly cellulose. To minimize waste and maximize biomass utilization, only essential refining steps were employed, simplifying the process and enhancing sustainability. The simplified green biorefinery yielded three distinct fractions: SI, rich in fucoidan and laminarin; S2, rich in sodium alginate; and P2, rich in cellulose. Key process responses including ultrasound energy input (J), the viscosity of sodium alginate (S2), and the yields of all fractions (SI, S2, and P2), are summarized in TableAttorney Docket No.:2024-027-01
[0193] The simplified green biorefinery successfully eliminates the reliance on harsh chemicals traditionally used in conventional processes, such as HC1 and sulfuric acid. By eliminating the need for extensive purification steps, this innovative approach achieves a reduction of >85 % in unit operations while also eliminating the use of organic solvents like ethanol (Figure 1A and Figure IB). By eliminating harsh chemicals such as HC1 and organic solvents such as ethanol, the process reduces material costs and the need for complex handling,Attorney Docket No.:2024-027-01 storage, and disposal protocols. To further evaluate the advantages of the green biorefinery method, an HCl-based extraction was conducted under comparable conditions. The sodium alginate (S2) yield from the HC1 method was 73.0 %, closely matching the highest yield obtained using the ultrasound-assisted green extraction. Additionally, the HCl-extracted alginate exhibited a viscosity of 4899 mPa-s, which was moderate compared to the viscosities achieved in this study but lower than those observed in groups with similar S2 yields. This suggests that HC1 induced more extensive hydrolysis than the green solvents. These findings confirm that the green biorefinery approach can achieve comparable extraction efficiency while minimizing the use of harsh chemicals and reducing the need for additional neutralization and purification steps.
[0194] The streamlined workflow also lowers energy demands by simplifying steps such as extensive purification and solvent recovery. From a workplace safety perspective, avoidance of hazardous chemicals minimizes the risks of chemical exposure, spills, or fire hazards. This is especially critical in scale-up production, where the handling of large quantities of toxic, flammable, or corrosive substances magnifies potential hazards. Furthermore, the simplified workflow minimizes the complexity of equipment handling and operational procedures, reducing the likelihood of human error or equipment malfunctions. These factors collectively contribute to lower operational costs and improved workplace safety, making the process particularly suitable for scaled-up production environments. Moreover, the biorefinery process is designed with an application-oriented focus, ensuring that the resulting product meets the stringent requirements for use as food additives while maintaining properties comparable to those of conventionally produced sodium alginate. This advancement highlights the potential for sustainable and cost-effective alternatives in alginate production without compromising quality or functionality.
[0195] Samples collected from Treatment 13-17, which are the repeated central points, were used as representatives for further analysis. Elemental analysis results of the raw material and all fractions are presented in Table 3.Attorney Docket No.:2024-027-01
[0196] The moisture and ash contents of the dried seaweed were 6.54 ± 0.60 % and 22.59 ± 1.37 %, respectively, closely aligned with previous reports, where moisture at 7.4 ± 1.00 % and ash at 25.9 ± 0.1 % were observed. The yield of sodium alginate extracted in this example accounted for an average of 79.10 % of the total carbohydrates reported in other studies on the same species. This confirms that the primary carbohydrate constituent in sugar kelp is sodium alginate, consistent with prior characterization research conducted on the same species.
[0197] Moisture contents of the three fractions were similar, at 7.52 ± 1.47 % for SI (fucoidan / laminarin), 11.62 ± 0.43 % for S2 (sodium alginate), and 10.10 ± 2.87 % for P2 (cellulose). Ash contents of S 1 and P2 were 48.96 ± 1.76 % and 29.31 ± 2.96 %, respectively. The high ash content in SI should primarily be from the existing free salt in seaweed, since SI was fractionated during the first step. Despite cations that got bonded to insoluble compounds such as cellulose and phlorotannin, most free ions should be removed from P2, resulting in the lowest ash content.
[0198] It is noteworthy that the ash content of sodium alginate was 53.02 ± 0.62 %, similar to what extracted from the same species but higher than that of the commercially purchased sodium alginate at 22.45 ± 0.2 %. This ash content of commercially purchased sodium alginate can be attributed to sodium alginate being a sodium salt. Unbumed organic matter and residual N zCCh also contributes to ash content. Due to reduced purification steps in the simplified biorefinery, the ash and sodium content can be a result of excess N zCCh. Commercial sodiumAttorney Docket No.:2024-027-01 alginate typically has a purity of approximately 80 %, as indicated in their certificates of analysis. Remarkably, the purity of sodium alginate was measured at 61.44 ± 4.83 % using the conventional ethanol precipitation method, achieved without the need for extensive purification. This demonstrates the efficiency of the simplified biorefinery in obtaining sodium alginate with minimal processing.
[0199] Accumulation of heavy metals in marine-based materials, such as carrageenan, is a rising concern, particularly when these materials are used in foods or nutritional supplements. Therefore, inductively coupled plasma mass spectrometry (ICP-MS) was performed for quality assurance of raw materials and to monitor heavy metal migration during the extraction process. Arsenic (As), Cadmium (Cd), Chromium (Cr), Lead (Pb), and Mercury (Hg) are the most common heavy metals in marine environments known to pose human health risks. Among these four were analyzed across all fractions and compared to raw material. In sugar kelp powder, which was dried from food-grade seaweed and served as the raw material, the following levels were detected: As at 31.74 ppm, Cd at 1.12 ppm, Cr at 0.28 ppm and Pb at 0.83 ppm. Comparing raw material and all extracted fractions, Cd, Cr and Pb levels in all extracted fractions were close to the lower detection limit, indicating minimal content of these heavy metals. Significant accumulation of all four heavy metals tested was observed in cellulose (P2), with detected levels of As at 28.74 ppm, Cd at 0.55 ppm, Cr at 0.37 ppm, and Pb at 0.42 ppm. The ICP-MS analysis confirmed reduced levels of heavy metals in fucoidan / laminarin (SI) and sodium alginate (S2) compared to the raw material, demonstrating an improved safety profile for these fractions when considered for use in foods or nutritional supplements.
[0200] The FTIR transmission spectra of the three fractions achieved in the simplified biorefinery were compared to spectrum of conventional sodium alginate within the fingerprint region with wavenumbers ranging between 400 and 1800 cm'1(Figure 17). Characteristic peaks for sodium alginate at 809, 1023, 1404, and 1591 cm'1were observed in both the spectra of conventional sodium alginate and S2 (sugar kelp extracted sodium alginate), confirming that S2 is primarily composed of sodium alginate. In contrast, these characteristic peaks were absent in the spectra of the other two fractions, validating their low sodium alginate content. This differentiation in the spectra highlights the effectiveness of the biorefinery process in isolating sodium alginate from other components of sugar kelp.Attorney Docket No.:2024-027-01
[0201] The noisy spectrum of P2 aligns with the hypothesis that, in addition to cellulose, other insoluble compounds such as proteins and polyphenols from sugar kelp presents in the same fraction. The overlapping signals from these components result in a noisy spectrum lacking sharp peaks. SI exhibited strong peaks near 1020 and 1080 cm1, which are characteristic of D-mannitol. In conventional biorefineries, D-mannitol would typically be discarded during blanching, which is commonly employed in pre-processing. These findings underscore the potential of the simplified biorefinery described in this study not only for sodium alginate fractionation but also for improving the utilization of other soluble compounds present in sugar kelp, offering an expanded scope of applications for this renewable resource.
[0202] Viscosity measurements in this study serve as a proxy for molecular weight and structural characteristics, enabling differentiation among alginate fractions and providing insights into their functional properties. It offers several advantages, including quick testing, minimal equipment requirements, and ease of operation. Among the available methods, rotary viscometer is the most accessible tool for evaluating the primary properties of sodium alginate, while other advanced techniques provides deeper insights at the molecular level. These include rheometer to analyze flow behavior and intrinsic viscosity, nuclear magnetic resonance (NMR) to determine structural composition, differential scanning calorimetry (DSC) to understand thermal behavior, and electron microscopy (SEM) to visualize the microstructure and arrangement of gel networks.
[0203] Molecular weights of the treatment with the highest viscosity (Treatment 5: 20 % amplitude, 32.5 min, pH 2) and the lowest viscosity (Treatment 2: 100 % amplitude, 5 min, pH 4) were evaluated using size exclusion chromatography (SEC) and compared with commercially purchased sodium alginate (Figure 18). Despite their distinct viscosities, the molecular weight profiles of the highest and lowest viscosity samples overlapped across the entire range. However, differences in the distribution and relative intensities of peaks contributed to their varying viscosities. The low viscosity sample (S2 T2) exhibited a stronger peak in the low molecular weight range, whereas the high viscosity sample (S2 T5) showed more pronounced peaks in the high molecular weight range. In contrast, commercially purchased sodium alginate was produced through extensive purification and displayed a single peak within a narrower molecular weight range.Attorney Docket No.:2024-027-01
[0204] The molecular weight distribution confirmed that viscosity is a reliable indicator of an overall molecular weight, though it does not necessarily imply that the molecular weight profile varies to the same extent as the viscosity. A higher molecular weight within the same composition correlates with increased viscosity. However, high viscosity is not always coupled with a uniform shift towards higher molecular weights. It may also result from changes in the relative abundance of multiple peaks in the distribution. Therefore, viscosity can serve as a useful parameter for quality control in a well-established system but should be complemented with additional analyses when evaluating a new system.
[0205] In order to achieve an optimized condition for the simplified biorefinery, a series of experimental conditions were designed using BBD, an RSM tool that efficiently explores the effects of multiple variables while minimizing experimental runs. The BBD employed in this example, included three independent variables: ultrasound amplitude (10-100%), ultrasound time (5-60 min), and pH of the extraction medium (2-7). These variables were selected based on their known influence on the outcomes of the biorefinery, as observed in earlier experiments. The experimental design matrix, as listed in Table 1, consisted of 17 runs, incorporating all combinations of the selected variables within the defined ranges, along with 5 replicates of the center point to understand experimental error and model predictability. The response variables evaluated were the yield of fucoidan / laminarin (SI), sodium alginate (S2) and cellulose (P2), as well as the viscosity of sodium alginate, which serves as a convenient and rapid testing parameter effectively indicating molecular weight. SI yield ranged from 10.7% at 10% amplitude, 32.5 minutes, pH 2, to 35.8 % at 50% amplitude, 60 minutes, pH 2. The yield of sodium alginate varied between 31.7% at 50% amplitude, 5 minutes, pH 7, and 75.8% at 50% amplitude, 60 minutes, pH 2. Similarly, P2 yield spanned from 36.3% at 100% amplitude, 32.5 minutes, pH 2, to 72.7% at 20% amplitude, 5 minutes, pH 4. Viscosity values for sodium alginate showed a wide range, with the maximum of 5399 mPa-s observed at 10 % of amplitude for 32.5 minutes in pH 2. And the minimum of 50.5 mPa-s at 100% amplitude for 5 minutes in pH 4.
[0206] As shown in Table 4, among all responses evaluated, significant models were obtained for only three responses: power (Rl), viscosity of product (R2), and sodium alginate yield (R4).Attorney Docket No.:2024-027-01
[0207] This limited success can be attributed to a lack of control over certain aspects of the process. For instance, the yield of fucoidan / laminarin (SI) could be largely influenced by loose powders during processing. The variance in this fraction could get diminished by the significant presence of solid particles that passed through the 200-mesh strainer used for separation in the lab setting. Similarly, the yield of cellulose (P2) could be strongly affected by the residual sodium alginate that remained unseparated due to the high viscosity of the mixture. Additionally, the hygroscopic nature of sodium alginate altered the final moisture content, introducing further inaccuracies into the analysis. The final equations for significant responses, based on scaled data and obtained via backward elimination of insignificant factors (p >0.05), are as follows:
[0208] Viscosity of product = = 0.747 - 0.65271 - 0.377B - 1.108C - 0.042AB +0.99271C + 0.829BC
[0209] Yield of S2 = 0.311 + 0.123A + 0.397B - 0.425CAttorney Docket No.:2024-027-01
[0210] These equations demonstrate that yield and viscosity were influenced by all three pretreatment variables: sonication amplitude (A), sonication time (B), and pH (C). The quadratic interaction terms reveal curvature in the response fimctions, allowing for an accurate approximation of the optimal conditions. For viscosity, pH (C) had the most significant linear impact, while the interaction between sonication amplitude (A) and pH (C) exerted the strongest combined effect. In contrast, for the yield of sodium alginate, pH (C) also showed the greatest linear influence, but all interactive effects were found to be insignificant following backward elimination. Amplitude is a key factor in determining cavitation intensity, which influences the disruption of cell walls and release of components. Sonication time, while less influential when paired with prolonged contact time, interacts with amplitude to modulate energy input. Energy density, defined as the energy applied per unit suspension volume, was identified as the most robust variable for predicting outcomes, emphasizing its utility in standardizing processes across instruments. In this case, sonication amplitude (A) and sonication time (B) are the only factors that affect ultrasound energy, and ultrasound energy is exclusively influenced by sonication amplitude (A) and sonication time (B) with a 0.975 R2 value. Although the actual treatment time theoretically interacts with pH (C) in influence the responses, the sonication time (B) ranging from 5 min to 60 minutes could be considered negligible considering the prolonged pre-soak times (20 ± 4 h) before sonication. It was consequently considered that energy could be adopted as a factor, namely factor D, as a representative factor for sonication amplitude (A) and sonication time (B) without losing information with respect to other variables. A new set of second-order polynomial equations was developed with energy (D) and pH (C) as variables:
[0211] Viscosity of product = 0.7899 - 2.013C - 1.907D + 2.331CD 4- 1.170C24- 0.801D2
[0212] Yield of S2= 0.394 - 1.085C 4- 1.590D - 0.204CD 4- 0.687C2- 1.019D2.
[0213] With energy (D) introduced as a new factor, the updated model revealed that pH (C) remained the factor with the greatest linear impact on product viscosity. In contrast, energy (D) emerged as the factor with the greatest linear impact on the yield of sodium alginate, replacing pH (C), which previously showed the strongest influence on yield before the inclusion of sonication energy in the model. In practice, lower viscosity is often preferred to facilitate easierAttorney Docket No.:2024-027-01 separation, drying, and to meet the requirements of diverse applications. Lower viscosity could be achieved with a combination of low pH (C) and high energy (D), due to the complementary effects of ultrasound-induced cell wall disruption and acid-induced hydrolysis. Conversely, some studies highlighted the benefits of high viscosity sodium alginate in specific applications, such as beverage, 3D culture for ex-vivo studies, and as bio-ink for tissue engineering scaffold.
[0214] Both low pH (C) with low energy (D) and high pH (C) with high energy (D) can lead to high viscosity. At low energy (D), the structural constraints of alginate remain largely intact, and alginate release is thus insufficient. This is evident in the low yield of sodium alginate under these conditions. On the other hand, at low pH (C), while acid facilitates cell wall disruption and the subsequent alginate release and improves yield, acid-induced hydrolysis becomes more pronounced, potentially offsetting the effects of the increased yield on viscosity. At high energy (D), alginate is more effectively released from the matrix, resulting in moderate yield. When pH (C) is high, low acidity inhibits acid-induced hydrolysis, resulting in high viscosity.
[0215] Sodium alginate yield remained relatively low at high pH (C), regardless of energy (D). This suggests that acidity must exceed a certain threshold to effectively release alginate from the matrix. In contrast, a 0.2 M HC1 wash achieved comparable yields with increased viscosities. Similarly, energy (D) showed a threshold effect, where change in acidity only began to improve yield after sufficient energy input was applied. Comparing Tables 5 and 4, the introduction of the new factor improved the F- values and -values of both models, indicating a better model fit.Atorney Docket No.:2024-027-01
[0216] In the lack-of-fit (LOF) test shown in Table 6, the Prediction Residual Error Sum of Squares (PRESS) increased for the viscosity model but decreased for the yield model, reflecting reduced predictive performance for viscosity and improved predictive performance for yield.Attorney Docket No.:2024-027-01
[0217] Similarly, R2 and predicted R2 exhibited contrasting changes between the viscosity and yield models. However, the adjusted R2 values for both models were higher compared to the earlier models, demonstrating that the inclusion of energy (D) as a factor, instead of sonication amplitude (A) and sonication time (B), effectively eliminated unnecessary predictors. To determine the optimal extraction conditions, a bound-constrained optimization was performed on the fitted second order polynomial model for S2 yield using Python’s SciPy library. The objective was to maximize yield within the experimental ranges of pH (2 to 7) and energy (5.2 to 552.7 kJ). The optimization results showed that a maximum S2 yield of 76.4 % is achieved at pH 2 and sonication energy of 432.2 kJ. This result not only confirms the robustness of the model but also suggests that slightly higher yields may be achievable within the tested range compared to individual treatments. This numerical optimum, obtained through mathematical modeling, supports the practical feasibility of using ultrasound-assisted green extraction to achieve high yields without harsh chemical treatment.
[0218] The R2values for viscosity and sodium alginate yield were 0.77 and 0.73, respectively, indicating that approximately 23-27% of the variance remains unexplained. This shortfall is likely due to high variance in the responses and signal-to-noise ratios, as evidenced by significant differences in center point replicates (Treatment 13-17 in Table 2), where up to 43.05 % and up to 82.92 % differences can be seen in viscosity and yield of sodium alginate. While adopting energy as a factor offsets some noise, fluctuations in energy input still contributed to up to 68.09 % variation. For example, comparing Treatment 13 and 14, a 22.82 % difference in energy input resulted in only marginal differences in all responses. This suggested that the impact of different treatment conditions may be limited by intrinsic system variability. Furthermore, the recorded energy was the nominal output of the ultrasound, which often deviates significantly from actual energy output. Such discrepancy necessitates further stabilization. Calorimetric calibration, such as estimating energy input based on temperature changes within the cavitation field, may provide a more reliable measure of acoustic energy for consistent comparisons across studies. Due to the absence of a direct method for measuring acoustic energy, the actual energy input can be estimated either from the energyAttorney Docket No.:2024-027-01 consumption of the ultrasonic generator or from the heat generated within the cavitation field, with the latter being calculated based on temperature changes.
[0219] Compounds and materials are described using standard nomenclature. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as is commonly understood by one of skill in the art to which this invention belongs.
[0220] The following terms are used to describe the invention of the present disclosure. In instances where a term is not specifically defined herein, that term is given an art-recognized meaning by those of ordinary skill applying that term in context to its use in describing the present disclosure.
[0221] The use of the terms “a” and “an” and “the” and similar referents (especially in the context of the following claims) are to be construed to cover both the singular and the plural, unless otherwise indicated herein or clearly contradicted by context. By way of example, "an element" means one element or more than one element.
[0222] It should also be understood that, in certain methods described herein that include more than one step or act, the order of the steps or acts of the method is not necessarily limited to the order in which the steps or acts of the method are recited unless the context indicates otherwise. Furthermore, the terms first, second, etc., as used herein are not meant to denote any particular ordering, but simply for convenience to denote a plurality of, for example, layers.
[0223] The terms “comprising”, “having”, “including”, and “containing” are to be construed as open-ended terms (i.e., meaning “including, but not limited to”) unless otherwise noted.
[0224] The terms “about” or “approximately,” as used herein, is inclusive of the stated value and means within an acceptable range of deviation for the particular value as determined by one of ordinary skill in the art, considering the measurement in question and the error associated with measurement of the particular quantity (i.e., the limitations of the measurement system). For example, “about” can mean within one or more standard deviations, or within ± 10% or 5% of the stated value. Recitation of ranges of values are merely intended to serve as a shorthand method of referring individually to each separate value falling within the range, unless otherwise indicated herein, and each separate value is incorporated into the specification as if it were individually recited herein. The endpoints of all ranges are included within the range and independently combinable. All methods described herein can be performed in a suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of anyAttorney Docket No.:2024-027-01 and all examples, or exemplary language (e.g., “such as”), is intended merely to better illustrate the invention and does not pose a limitation on the scope of the invention unless otherwise claimed. No language in the specification should be construed as indicating any non-claimed element as essential to the practice of the invention as used herein.
[0225] The phrase "and / or," as used herein in the specification and in the claims, should be understood to mean "either or both" of the elements so conjoined, i.e., elements that are conjunctively present in some cases and disjunctively present in other cases. Multiple elements listed with "and / or" should be construed in the same fashion, i.e., "one or more" of the elements so conjoined. Other elements may optionally be present other than the elements specifically identified by the "and / or" clause, whether related or unrelated to those elements specifically identified. Thus, as a non-limiting example, a reference to "A and / or B", when used in conjunction with open-ended language such as "comprising" can refer, in one embodiment, to A only (optionally including elements other than B); in another embodiment, to B only (optionally including elements other than A); in yet another embodiment, to both A and B (optionally including other elements); etc.
[0226] As used herein in the specification and in the claims, "or" should be understood to have the same meaning as "and / or" as defined above. For example, when separating items in a list, "or" or "and / or" shall be interpreted as being inclusive, i.e., the inclusion of at least one, but also including more than one, of a number or list of elements, and, optionally, additional unlisted items. Only terms clearly indicated to the contrary, such as “only one of’ or "exactly one of," or, when used in the claims, "consisting of," will refer to the inclusion of exactly one element of a number or list of elements. In general, the term "or" as used herein shall only be interpreted as indicating exclusive alternatives (i.e., "one or the other but not both") when preceded by terms of exclusivity, such as "either," "one of," "only one of," or "exactly one of."
[0227] As used herein in the specification and in the claims, the phrase "at least one," in reference to a list of one or more elements, should be understood to mean at least one element selected from anyone or more of the elements in the list of elements, but not necessarily including at least one of each and every element specifically listed within the list of elements and not excluding any combinations of elements in the list of elements. This definition also allows that elements may optionally be present other than the elements specifically identified within the list of elements to which the phrase "at least one" refers, whether related or unrelated to thoseAttorney Docket No.:2024-027-01 elements specifically identified. Thus, as a nonlimiting example, "at least one of A and B" (or, equivalently, "at least one of A or B," or, equivalently "at least one of A and / or B") can refer, in one embodiment, to at least one, optionally including more than one, A, with no B present (and optionally including elements other than B); in another embodiment, to at least one, optionally including more than one, B, with no A present (and optionally including elements other than A); in yet another embodiment, to at least one, optionally including more than one, A, and at least one, optionally including more than one, B (and optionally including other elements); etc.
[0228] The phrase "one or more," as used herein, means at least one, and thus includes individual components as well as mixtures / combinations of the listed components in any combination.
[0229] Other than in the operating examples, or where otherwise indicated, all numbers expressing quantities of ingredients and / or reaction conditions are to be understood as being modified in all instances by the term "about," meaning within 10% of the indicated number (e.g., "about 10%" means 9%-l 1% and "about 2%" means 1.8%-2.2%).
[0230] All percentages and ratios are calculated by weight unless otherwise indicated. All percentages are calculated based on the total composition unless otherwise indicated. Generally, unless otherwise expressly stated herein, "weight" or "amount" as used herein with respect to the percent amount of an ingredient refers to the amount of the raw material comprising the ingredient, wherein the raw material may be described herein to comprise less than and up to 100% activity of the ingredient. Therefore, weight percent of an active in a composition is represented as the amount of raw material containing the active that is used and may or may not reflect the final percentage of the active, wherein the final percentage of the active is dependent on the weight percent of active in the raw material.
[0231] All ranges and amounts given herein are intended to include subranges and amounts using any disclosed point as an end point. Thus, a range of "1% to 10%, such as 2% to 8%, such as 3% to 5%," is intended to encompass ranges of "1% to 8%," "1% to 5%," "2% to 10%, " and so on. All numbers, amounts, ranges, etc., are intended to be modified by the term "about," whether or not so expressly stated. Similarly, a range given of "about 1% to 10%" is intended to have the term "about" modifying both the 1% and the 10% endpoints. Further, it is understood that when an amount of a component is given, it is intended to signify the amount of the active material unless otherwise specifically stated.Attorney Docket No.:2024-027-01
[0232] As used herein, “optional” or “optionally” means that the subsequently described event or circumstance may or may not occur, and that the description includes instances where said event or circumstance occurs and instances where it does not.
[0233] All methods described herein can be performed in a suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (e.g., “such as”), is intended merely to better illustrate the invention and does not pose a limitation on the scope of the invention unless otherwise claimed. No language in the specification should be construed as indicating any non-claimed element as essential to the practice of the invention as used herein. Unless defined otherwise, technical and scientific terms used herein have the same meaning as is commonly understood by one of skill in the art of this disclosure.
[0234] Furthermore, the disclosure encompasses all variations, combinations, and permutations in which one or more limitations, elements, clauses, and descriptive terms from one or more of the listed claims are introduced into another claim. For example, any claim that is dependent on another claim can be modified to include one or more limitations found in any other claim that is dependent on the same base claim. Where elements are presented as lists, e.g., in Markush group format, each subgroup of the elements is also disclosed, and any element(s) can be removed from the group.
[0235] All compounds are understood to include all possible isotopes of atoms occurring in the compounds. Isotopes include those atoms having the same atomic number but different mass numbers and encompass heavy isotopes and radioactive isotopes. By way of general example, and without limitation, isotopes of hydrogen include tritium and deuterium, and isotopes of carbon includenC,13C, and14C. Accordingly, the compounds disclosed herein may include heavy or radioactive isotopes in the structure of the compounds or as substituents attached thereto. Examples of useful heavy or radioactive isotopes include18F,15N,18O,76Br,125I and131I.
[0236] While the invention has been described with reference to an exemplary embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosedAttorney Docket No.:2024-027-01 as the best mode contemplated for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Any combination of the above-described elements in all possible variations thereof is encompassed by the invention unless otherwise indicated herein or otherwise clearly contradicted by context.Incorporation by Reference
[0237] All U.S. and PCT patent publications and U.S. patents mentioned herein are hereby incorporated by reference in their entirety as if each individual patent publication or patent was specifically and individually indicated to be incorporated by reference. In case of conflict, the present application, including any definitions herein, will control.Other Embodiments
[0238] Those skilled in the art will recognize or be able to ascertain using no more than routine experimentation many equivalents to the specific embodiments described herein. The scope of the present embodiments described herein is not intended to be limited to the above Description, but rather is as set forth in the appended claims. Those of ordinary skill in the art will appreciate that various changes and modifications to this description may be made without departing from the spirit or scope of the present invention, as defined in the following claims.
[0239] For reasons of completeness, various aspects of the disclosure are set out in the following numbered clauses:
[0240] Clause 1. A composition comprising: (1) a seaweed extract comprising sodium alginate; (2) at least one vegetable oil, at least one algal oil, or a combination thereof; and (3) at least one plant extract, wherein the plant extract is a spice extract or an essential oil.
[0241] Clause 2. The composition of clause 1, wherein the seaweed is a brown seaweed.
[0242] Clause 3. The composition of clause 1 or clause 2, wherein the seaweed isSaccharina latissima.
[0243] Clause 4. The composition of any of clauses 1-3, wherein the at least one vegetable oil is wheat bran oil, rice bran oil, coconut oil, soy oil, canola oil, avocado oil, olive oil, sunflower flower, peanut oil, or any combination thereof.
[0244] Clause 5. The composition of any of clauses 1-4, wherein the at least one algal oil is a Schizochytrium oil, a Crypthecodinium cohnii oil, a Nannochloropsis oil, a Chlorella oil, aAttorney Docket No.:2024-027-01Botryococcus braunii oil, a Dunaliella tertiolecta oil, a Pleurochrysis carterae oil, or any combination thereof.
[0245] Clause 6. The composition of any of clauses 1-5, wherein the at least one plant extract is a spice extract.
[0246] Clause 7. The composition of clause 6, wherein the at least one spice extract is a vanilla extract, a cinnamon extract, a clove extract, a coriander extract, a cumin extract, a garlic extract, a ginger extract, a mustard extract, a nutmeg extract, a turmeric extract, a liquid spice oleoresins, or any combination thereof.
[0247] Clause 8. The composition of any of clauses 1-6, wherein the at least one plant extract is an essential oil.
[0248] Clause 9. The composition of clause 8, wherein the at least one essential oil is derived from bay leaf, holy basil, cilantro, lemongrass, marjoram, mint, oregano, parsley, peppermint, rosemary, savory, spearmint, thyme, amaranth, bergamot, cannabis, eucalyptus, grapefruit, lemons, lime, mandarin, neem, orange, pandan, rose, Wintergreen, or any combination thereof.
[0249] Clause 10. The composition of any of clauses 1-9, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract are each present in the composition in a ratio of 100: 10: 1 to 200: 10:1.
[0250] Clause 11. The composition of clause 10, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract are each present in the composition in a ratio of 100:20:2 to 200:10:1.
[0251] Clause 12. The composition of clause 11, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract are each present in the composition in a ratio of 100:20:2.
[0252] Clause 13. The composition of any of clauses 1-12, wherein the composition further comprises an emulsifier.
[0253] Clause 14. The composition of clause 13, wherein the emulsifier is at least one lecithin, at least one quillaja saponin, at least one yucca saponin, at least one ginseng saponin, or any combinations thereof.Attorney Docket No.:2024-027-01
[0254] Clause 15. The composition of clause 13 or clause 14, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract, and at least one emulsifier are each present in the composition in a ratio of 100: 10: 1 : 1 to 200: 10: 1:1.
[0255] Clause 16. The composition of clause 15, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract, and at least one emulsifier are each present in the composition in a ratio of 100:20:2:2 to 200: 10: 1:1.
[0256] Clause 17. The composition of clause 16, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract, and at least one emulsifier are each present in the composition in a ratio of 100:20:2:2.
[0257] Clause 18. The composition of any of clauses 1-17, wherein the composition further comprises a solvent.
[0258] Clause 19. The composition of clause 18, wherein the solvent is water.
[0259] Clause 20. The composition of any of clauses 1-19, wherein the composition is in the form of an aqueous dispersion.
[0260] Clause 21. A method of coating biological material, the method comprising coating the biological material with an effective amount of the composition of any of clauses 1-20 to coat the biological material.
[0261] Clause 22. The method of clause 21, wherein the biological material is a plant, part of plant, a fruit, a vegetable, seed of a fruit, seed of a vegetable, a fungi, or any combination thereof.
[0262] Clause 23. A method of coating a fiber-based material, the method comprising coating the fiber-based material with an effective amount of the composition of any of clauses 1- 20 to coat the fiber-based material.
[0263] Clause 24. The method of clause 23, wherein the fiber-based material is a paper, paperboard, cardboard, molded fiber products, fiber board, tissue products, or any combination thereof.
[0264] Clause 25. The method of clause 23 or clause 24, wherein the fiber-based material is in the form of a bottle or a container.
[0265] Clause 26. A method of slowing the ripening of a perishable food product, the method comprising the step of coating a perishable food product with an effective amount of the composition of any of clauses 1-20 to coat the perishable food product.Attorney Docket No.:2024-027-01
[0266] Clause 27. The method of clause 26, wherein the perishable food product is a fruit, a vegetable, a seed of a fruit, a seed of a vegetable, a fungi, or any combination thereof.
[0267] Clause 28. A method for preparing a seaweed extract, the method comprising:
[0268] a) mixing brown seaweed with at least one food-grade acid to create a mixture, wherein the mixture has a pH of 2-4, and further wherein the treating of the brown seaweed with the at least one food-grade acid produces a by-product fraction and a fraction enriched with alginic acid;
[0269] b) separating the by-product fraction from the fraction enriched with alginic acid;
[0270] c) mixing the fraction enriched with alginic acid with at least one base to form a mixture, wherein the mixture has a pH of 8-12, and further wherein the treating of the fraction enriched with alginic acid with at least one base produces a by-product fraction and a sodium alginate product; and
[0271] d) separating the sodium alginate product from the by-product fraction of step c); and
[0272] e) recovering the sodium alginate product from step d).
[0273] Clause 29. The method of clause 28, wherein the food-grade acid is selected from the group consisting of: citric acid, acetic acid, carbonic acid, lactic acid, tartaric acid, ascorbic acid, phosphoric acid, fumaric acid, succinic acid, and hydrogen peroxide, or any combinations thereof.
[0274] Clause 30. The method of clause 28 or clause 29, wherein the base is a carbonate, a bicarbonate, a hydroxide, an oxide, or any combination thereof.
[0275] Clause 31. The method of clause 30, wherein the base is calcium carbonate, potassium carbonate, sodium carbonate, ammonium carbonate, calcium bicarbonate, potassium bicarbonate, sodium bicarbonate, ammonium bicarbonate, calcium hydroxide, potassium hydroxide, sodium hydroxide, magnesium hydroxide, calcium oxide, potassium oxide, sodium oxide, or any combination thereof.
[0276] Clause 32. The method of any of clauses 28-31, wherein the separating in step b) is performed using filtration.
[0277] Clause 33. The method of any of clauses 28-32, wherein the separating in step d) is performed using centrifugation.
[0278] Clause 34. The method of any of clauses 28-33, wherein the mixture in step a) is subjected to ultrasound.Attorney Docket No.:2024-027-01
[0279] Clause 35. The method of clause 34, wherein the mixing of step a) occurs for about 1 to about 24 hours at a temperature of about 20°C to about 80°C.
[0280] Clause 36. The method of any of clauses 28-35, wherein the mixing of step c) occurs for about 5 minutes to about 4 hours at a temperature of about 20°C to about 80°C.
[0281] Clause 37. The method of any of clauses 28-36, wherein the brown seaweed is Saccharina latissima.
[0282] Clause 38. A Saccharina latissima extract produced by the method of any of clauses 28-37.
Claims
Attorney Docket No.:2024-027-01CLAIMSWhat is claimed is:
1. A composition comprising: (1) a seaweed extract comprising sodium alginate; (2) at least one vegetable oil, at least one algal oil, or a combination thereof; and (3) at least one plant extract, wherein the plant extract is a spice extract or an essential oil.
2. The composition of claim 1, wherein the seaweed is a brown seaweed.
3. The composition of claim 1 or claim 2, wherein the seaweed is Saccharina latissima.
4. The composition of any of claims 1-3, wherein the at least one vegetable oil is wheat bran oil, rice bran oil, coconut oil, soy oil, canola oil, avocado oil, olive oil, sunflower flower, peanut oil, or any combination thereof.
5. The composition of any of claims 1-4, wherein the at least one algal oil is a Schizochytrium oil, a Crypthecodinium cohnii oil, a Nannochloropsis oil, a Chlorella oil, a Botryococcus braunii oil, a Dunaliella tertiolecta oil, a Pleurochrysis carterae oil, or any combination thereof.
6. The composition of any of claims 1-5, wherein the at least one plant extract is a spice extract.
7. The composition of claim 6, wherein the at least one spice extract is a vanilla extract, a cinnamon extract, a clove extract, a coriander extract, a cumin extract, a garlic extract, a ginger extract, a mustard extract, a nutmeg extract, a turmeric extract, a liquid spice oleoresins, or any combination thereof.
8. The composition of any of claims 1-6, wherein the at least one plant extract is an essential oil.
9. The composition of claim 8, wherein the at least one essential oil is derived from bay leaf, holy basil, cilantro, lemongrass, maijoram, mint, oregano, parsley, peppermint, rosemary, savory, spearmint, thyme, amaranth, bergamot, cannabis, eucalyptus, grapefruit, lemons, lime, mandarin, neem, orange, pandan, rose, Wintergreen, or any combination thereof.Attorney Docket No.:2024-027-0110. The composition of any of claims 1-9, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract are each present in the composition in a ratio of 100:10:1 to 200:10:1.
11. The composition of claim 10, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract are each present in the composition in a ratio of 100:20:2 to 200:10:1.
12. The composition of claim 11, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, and at least one plant extract are each present in the composition in a ratio of 100:20:2.
13. The composition of any of claims 1-12, wherein the composition further comprises an emulsifier.
14. The composition of claim 13, wherein the emulsifier is at least one lecithin, at least one quillaja saponin, at least one yucca saponin, at least one ginseng saponin, or any combinations thereof.
15. The composition of claim 13 or claim 14, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract, and at least one emulsifier are each present in the composition in a ratio of 100: 10: 1 : 1 to 200: 10: 1:1.
16. The composition of claim 15, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract, and at least one emulsifier are each present in the composition in a ratio of 100:20:2:2 to 200: 10: 1:1.
17. The composition of claim 16, wherein the sodium alginate, at least one vegetable oil and / or at least one algal oil, at least one plant extract, and at least one emulsifier are each present in the composition in a ratio of 100:20:2:2.
18. The composition of any of claims 1-17, wherein the composition further comprises a solvent.
19. The composition of claim 18, wherein the solvent is water.
20. The composition of any of claims 1-19, wherein the composition is in the form of an aqueous dispersion.Attorney Docket No.:2024-027-0121. A method of coating biological material, the method comprising coating the biological material with an effective amount of the composition of any of claims 1 -20 to coat the biological material.
22. The method of claim 21, wherein the biological material is a plant, part of plant, a fruit, a vegetable, seed of a fruit, seed of a vegetable, a fungi, or any combination thereof.
23. A method of coating a fiber-based material, the method comprising coating the fiberbased material with an effective amount of the composition of any of claims 1 -20 to coat the fiber-based material.
24. The method of claim 23, wherein the fiber-based material is a paper, paperboard, cardboard, molded fiber products, fiber board, tissue products, or any combination thereof.
25. The method of claim 23 or claim 24, wherein the fiber-based material is in the form of a bottle or a container.
26. A method of slowing the ripening of a perishable food product, the method comprising the step of coating a perishable food product with an effective amount of the composition of any of claims 1-20 to coat the perishable food product.
27. The method of claim 26, wherein the perishable food product is a fruit, a vegetable, a seed of a fruit, a seed of a vegetable, a fungi, or any combination thereof.
28. A method for preparing a seaweed extract, the method comprising: a) mixing brown seaweed with at least one food-grade acid to create a mixture, wherein the mixture has a pH of 2-4, and further wherein the treating of the brown seaweed with the at least one food-grade acid produces a by-product fraction and a fraction enriched with alginic acid; b) separating the by-product fraction from the fraction enriched with alginic acid; c) mixing the fraction enriched with alginic acid with at least one base to form a mixture, wherein the mixture has a pH of 8-12, and further wherein the treating of the fraction enriched with alginic acid with at least one base produces a by-product fraction and a sodium alginate product; andAttorney Docket No.:2024-027-01 d) separating the sodium alginate product from the by-product fraction of step c); and e) recovering the sodium alginate product from step d).
29. The method of claim 28, wherein the food-grade acid is selected from the group consisting of: citric acid, acetic acid, carbonic acid, lactic acid, tartaric acid, ascorbic acid, phosphoric acid, fumaric acid, succinic acid, and hydrogen peroxide, or any combinations thereof.
30. The method of claim 28 or claim 29, wherein the base is a carbonate, a bicarbonate, a hydroxide, an oxide, or any combination thereof.
31. The method of claim 30, wherein the base is calcium carbonate, potassium carbonate, sodium carbonate, ammonium carbonate, calcium bicarbonate, potassium bicarbonate, sodium bicarbonate, ammonium bicarbonate, calcium hydroxide, potassium hydroxide, sodium hydroxide, magnesium hydroxide, calcium oxide, potassium oxide, sodium oxide, or any combination thereof.
32. The method of any of claims 28-31, wherein the separating in step b) is performed using filtration.
33. The method of any of claims 28-32, wherein the separating in step d) is performed using centrifugation.
34. The method of any of claims 28-33, wherein the mixture in step a) is subjected to ultrasound.
35. The method of claim 34, wherein the mixing of step a) occurs for about 1 to about 24 hours at a temperature of about 20°C to about 80°C.
36. The method of any of claims 28-35, wherein the mixing of step c) occurs for about 5 minutes to about 4 hours at a temperature of about 20°C to about 80°C.
37. The method of any of claims 28-36, wherein the brown seaweed is Saccharina latissima.
38. A Saccharina latissima extract produced by the method of any of claims 28-37.
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