Polysaccharide composition
High-pressure treatment of polysaccharides addresses the limitations of chemical methods by achieving controlled molar mass distribution and dispersity, producing environmentally friendly polysaccharides with improved functional properties.
Patent Information
- Application Number
- PCT/US2025/030588
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-05-30
- Filing Date
- 2025-05-22
- Publication Date
- 2026-01-02
AI Technical Summary
Existing methods for depolymerizing polysaccharides, such as carrageenan, rely on chemicals like hydrogen peroxide or hydrogen chloride, which are not environmentally friendly and difficult to control, leading to low molar mass polysaccharides and compliance issues with regional regulations, while high-pressure homogenization methods do not effectively manage molar mass distribution.
A method involving high-pressure treatment of an aqueous polysaccharide solution, preferably carrageenan, without insoluble fibers, at controlled pressures and temperatures to achieve targeted weight average molar masses and dispersity, using dynamic high-pressure homogenization or microfluidization.
The method produces polysaccharides with controlled molar mass distribution, achieving a dispersity of 1.70 or less and limiting low molar mass polysaccharides to less than 5%, resulting in more natural and effective polysaccharide compositions with enhanced functional properties.
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Figure US2025030588_02012026_PF_FP_ABST
Abstract
Description
POLYSACCHARIDE COMPOSITIONCROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of European Patent Application 24179099.7 filed May 30, 2024, which is incorporated by reference herein in its entirety.TECHNICAL FIELD
[0002] The present invention relates to the field of polysaccharides for use as hydrocolloids. More specifically, the present invention relates to a non-chemical method of depolymerizing polysaccharides during a hydrocolloid production process, and polysaccharide compositions produced therefrom.BACKGROUND
[0003] Polysaccharides are widely used as hydrocolloids in, for example, the food and beverage, feed and pet food, pharmaceutical, cosmetic, and technical industries (such as paper, paint, enhanced oil recovery, etc.). The functionality of polysaccharides, e.g. as texturizers, depends in part upon their molar mass (M), especially their weight average molar mass (Mw), which is sometimes referred to as ‘'average molecular weight’’. The weight average molar mass may be altered to adapt the functionality of polysaccharides for different applications.
[0004] Depolymerization is a process whereby macromolecules are broken down into smaller ones, which is correlated with a reduction in Mw and Mn (number average molecular weight). According to the structure of the macromolecules and their organization, depolymerization can impact functional properties.
[0005] Carrageenan is a widely used seaweed-derived polysaccharide. Various methods have been used to depolymerize carrageenans. The most common approach is to use chemicals, such as Hydrogen Peroxide or Hydrogen Chloride, to depolymerize carrageenan at plant scale.
[0006] However, consumer preference is increasingly towards natural products that use fewer or no chemicals in their production. Moreover, chemical depolymerization methods can be sensitive to heavy metals and are difficult to control in order to obtain a specific weight average molar mass. Another drawback is that an excess of chemicals induces the production of low molar mass carrageenan (less than 50 000 g / mol). According to some regional regulations, the amount of low molar mass carrageenan in a carrageenan powder for food applications may not exceed 5%.
[0007] High pressure treatments, such as high pressure homogenization, are known. Natural seaweed composite material produced by methods comprising high pressure homogenization areknown. High pressure homogenization has been performed on a slurry of carrageenan and insolubles, such as fibre, to promote carrageenan extraction from the seaweed matrix, not to impact the molar mass of the polysaccharides.
[0008] Accordingly, there remains a demand in industry for a method of depolymerizing polysaccharides which does not require the use of chemicals, and which avoids the problems mentioned above. Associated with this is a demand for more natural polysaccharide compositions.SUMMARY OF THE INVENTION
[0009] The present invention meets the above demands. The invention relates to a method for producing a polysaccharide composition, comprising: obtaining an aqueous solution comprising a polysaccharide and at least one other soluble compound; and subjecting the aqueous solution to high pressure treatment.
[0010] In some embodiments, the at least one other soluble compound is selected from salts, pigments, acids, bases, proteins, sugars, oligosaccharides, other polysaccharides, or combinations thereof.
[0011] In some embodiments, the aqueous solution does not contain insoluble fibres or compounds. In other embodiments, the aqueous solution may contain only trace amounts of insoluble fibres or compounds.
[0012] In some embodiments, the aqueous solution is an intermediate product formed during a hydrocolloid production process, or a derivative thereof, optionally wherein the intermediate product is selected from a syrup, filtrate, fermentation broth, or a derivative thereof.
[0013] In some embodiments, the concentration of the polysaccharide in the aqueous solution is from 0. 1 to 6% by weight, preferably from 0.5 to 4% by weight.
[0014] In some embodiments, the aqueous solution is subjected to multiple consecutive high pressure treatments.
[0015] In some embodiments, the high pressure treatment is performed at an inlet pressure of from 0.1 to 100 MPa (1 to 1000 bar), preferably from 20 to 80 MPa (200 to 800 bar).
[0016] In some embodiments, the high pressure treatment is performed at a temperature of from 10°C to 140°C, preferably from 25°C to 140°C, more preferably from 25°C to 100°C, or most preferably from 50°C to 100°C.
[0017] The present invention further relates to a polysaccharide composition obtained using the method of the invention.
[0018] The present invention further relates to the use of high pressure treatment to depolymerize a polysaccharide during a hydrocolloid production process.
[0019] In some embodiments, the polysaccharide is a non-associative polysaccharide.
[0020] In some embodiments, the polysaccharide is extracted from biomass or obtained via fermentation.
[0021] In some embodiments, the polysaccharide is carrageenan.
[0022] The present invention further relates to a carrageenan composition having a dispersity of 1.70 or less, optionally wherein:• the composition has a weight average molar mass of 450 000 g / mol or less; and / or• less than 5% of the carrageenan molecules in the composition have a molar mass below 50 000 g / mol.
[0023] In some embodiments, no more than 12% of the carrageenan molecules in the composition have a molar mass of 100 000 g / mol or less.
[0024] In some embodiments, the carrageenan composition is a depolymerized carrageenan composition.DESCRIPTION OF THE DRAWINGS
[0025] FIG. 1 shows Brookfield viscosity change depending on the number of consecutive cycles. The trials are achieved for two pressures: 25 MPa and 85 MPa (250 and 850 bar). No salt was added.
[0026] FIG. 2 shows percentage of Brookfield viscosity loss according to the reference depending on the number of consecutive cycles. The filled symbols for the value obtained without salt, the empty symbols with salt.
[0027] FIG. 3a shows Brookfield viscosity change depending on the number of consecutive cycles at 250 bar. The filled symbols represent the value obtained without salt, the empty symbols with salt.
[0028] FIG. 3b shows Brookfield viscosity change depending on the number of consecutive cycles at 850 bar. The filled symbols represent the value obtained without salt, the empty symbols with salt.
[0029] FIG. 4 shows Intrinsic viscosity' change depending on the number of consecutive cycles, without KC1, at 250 or 850 bar.
[0030] FIG. 5 shows Percentage of Intrinsic viscosity loss according to the reference depending on the number of consecutive cycles. The filled symbols represent the value obtained without salt, the empty symbols with salt.
[0031] FIG. 6a shows Brookfield viscosity change for 1.5% carrageenan solution without KC1 as a function of pressure (only 1 cycle). Each arrow corresponds to the percentage of loss regarding the reference (0 bar).
[0032] FIG. 6b shows Haake viscosity change for 1.5% carrageenan solution without KC1 as a function of pressure (only 1 cycle). Each arrow corresponds to the percentage of loss regarding the reference (0 bar).
[0033] FIG. 6c shows Intrinsic viscosity change for 1.5% carrageenan solution without KC1 as a function of pressure (only 1 cycle). Each arrow corresponds to the percentage of loss regarding the reference (0 bar).
[0034] FIG. 7 shows Intrinsic viscosity’ change for 1%, 1.5%, and 2% carrageenan solutions without KC1 as a function of pressure (only 1 cycle).
[0035] FIG. 8 shows Intrinsic viscosity change for 1%, 1.5%, and 2% carrageenan solutions with 2 g / L KC1 as a function of pressure (only 1 cycle).
[0036] FIG. 9 shows Flow curves of the 1.5% carrageenan solutions without KC1 after HPH treatment. Several inlet pressures are studied: 0, 20, 40, 60, 80 MPa (0 bar, 200 bar, 400 bar, 600 bar, and 800 bar).
[0037] FIG. 10 shows Flow curves of the 1.5% carrageenan solutions containing 2 g / L KC1 after HPH treatment. Several inlet pressures are studied: 0, 20, 40, 60, 80 MPa (0 bar, 200 bar, 400 bar, 600 bar, and 800 bar).
[0038] FIG. Ila shows Brookfield viscosity change for an industrial syrup (after carrageenan extraction from seaweed and filtration) as a function of pressure (only 1 cycle). Each arrow corresponds to the percentage of loss regarding the reference (0 bar).
[0039] FIG. 11b shows Haake viscosity change for an industrial syrup (after carrageenan extraction from seaweed and filtration) as a function of pressure (only 1 cycle). Each arrow corresponds to the percentage of loss regarding the reference (0 bar).
[0040] FIG. 11c shows intrinsic viscosity change for an industrial syrup (after carrageenan extraction from seaweed and filtration) as a function of pressure (only 1 cycle). Each arrow corresponds to the percentage of loss regarding the reference (0 bar).
[0041] FIG. 12 shows Flow curves of an industrial syrup after HPH treatment. Several inlet pressures are studied: 0. 20. 40, 60, 80 MPa (0 bar, 200 bar, 400 bar, 600 bar, and 800 bar).
[0042] FIG. 13 shows overlapping chromatograms of samples treated by acidic (HC1) depolymerization (pH 4 at 80°C) for 0 min, 10 min, 1 h, and 2 h. Other parameters: 10 g / L carrageenan, 5 g / L KC1, atmospheric pressure.
[0043] FIG. 14a shows overlapping chromatograms of samples treated by HPH for 0 cycle, 1 cycle, 3 cycles, and 5 cycles. Other parameters: 1 g / L carrageenan, 5 g / L KC1, 200 bar.
[0044] FIG. 14b shows overlapping chromatograms of samples treated by HPH for 0 cycle, 1 cycle, 3 cycles, and 5 cycles. Other parameters: 1 g / L carrageenan. 5 g / L KCL 800 bar.
[0045] FIG. 15a shows overlapping chromatograms of samples treated by HPH for 0 cycle, 1 cycle, 3 cycles, and 5 cycles. Other parameters: 10 g / L carrageenan, 5 g / L KC1, 200 bar.
[0046] FIG. 15b shows overlapping chromatograms of samples treated by HPH for 0 cycle, 1 cycle, 3 cycles, and 5 cycles. Other parameters: 10 g / L carrageenan, 5 g / L KC1, 800 bar.
[0047] FIG. 16 shows overlapping chromatograms of samples treated by HPH for 0 cycle, 1 cycle, 3 cycles, and 5 cycles. Other parameters: 5.5 g / L carrageenan, 5 g / L KC1, 500 bar.
[0048] FIG. 17 shows overlapping chromatograms of samples treated by HPH for 0 cycle or 1 cycle. HPH at 200 bar (solid line) or 800 bar (red triangle). Other parameters: -5 g / L carrageenan, 65-70°C, after carrageenan extraction from seaweed and filtration.
[0049] FIG 18: shows intrinsic viscosity change of the 1.5% iota carrageenan solutions with 2 g / L KC1 (KC12) or without KC1 (KC10) after HPH treatment (only 1 cycle). Several inlet pressures are studied: 0, 20, 40, 60, 80 MPa (0 bar, 200 bar, 400 bar, 600 bar, and 800 bar).
[0050] FIG 19a: shows Brookfield viscosity change of the 1% lambda carrageenan solutions with 2 g / L KC1 after HPH treatment (only 1 cycle). Several inlet pressures are studied: 0, 20, and 80 MPa (0 bar, 200 bar, and 800 bar).
[0051] FIG 19b: shows intrinsic viscosity change of the 1% carrageenan solutions with 2 g / L KC1 after HPH treatment (only 1 cycle). Several inlet pressures are studied: 0, 20, and 80 MPa (0 bar, 200 bar, and 800 bar).
[0052] FIG 20a: shows overlapping chromatograms of a first cottonii sample treated by HPH for 0 cycles, 1 cycle, or 2 cycles. Other parameters: -8-10 g / L carrageenan, 90°C, 800 bar, after carrageenan extraction from seaweed and filtration.
[0053] FIG 20b: shows overlapping chromatograms of a third cottonii sample treated by HPH for 0 cycles, 1 cycle, or 2 cycles. Other parameters: -8-10 g / L carrageenan, 90°C, 800 bar, after carrageenan extraction from seaweed and filtration.
[0054] FIG 21: Shows how using the signal from DRI, the peak of the carrageenan is integrated.DETAILED DESCRIPTION OF THE INVENTION
[0055] In the following, the elements of the present invention will be described. These elements may be listed with specific embodiments; however, it should be understood that they may be combined in any manner and in any number to create additional embodiments. Thus, any permutations and combinations of the described elements should be considered as being disclosed herein unless the context dictates otherwise.
[0056] All examples, or exemplary language (e.g., "such as"), provided herein are / is merely intended to better illustrate the present invention and does not limit the scope of the invention which will be limited only by the appended claims. No language used in the specification should be construed as indicating any non-claimed element essential to the practice of the invention. Process steps described herein can be performed in any suitable order unless otherwise specified herein or clearly contradicted by the context.
[0057] The words "comprising", "having", "containing", and "including", and other forms thereof, are intended to be equivalent in meaning and be open ended in that an item or items following any one of these words is not meant to be an exhaustive listing of such item or items, or meant to be limited to only the listed item or items. For each of the aspects and embodiments described herein by using any one of these words, an alternative aspect or embodiment with an exhaustive listing of the respective item or items (i.e., following the words "consisting of or "is / are", for example) is also encompassed by the present disclosure.
[0058] As used herein, the term "and / or" includes the meaning of "and", "or", and "all or any other combination of the elements connected by said term".
[0059] As used herein, the words "a", "an", and "the" are meant to cover both the singular and plural form of the item following these words, unless the context clearly indicates otherwise.
[0060] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by a person skilled in the art.
[0061] As used herein, the term "about" means within 15%, preferably within 10%. more preferably within 5% of a given value or range. It also includes the concrete value, e.g., "about 20" includes the value of 20.
[0062] Polysaccharides can be classed as associative or non-associative. The terms ‘‘associative” and “non-associative” refer to the behaviour of polysaccharides in solution. In the case of associative polysaccharides, several (at least 2) polysaccharide chains physically-hnk together in solution (“physically -linked” means that crosslinking is due to electrostatic charges, hydrogenbonding or van-der-Waals bonds, rather than chemical bonds). Temperature can influence theassociative behavior of polysaccharides. For example, Kappa-carrageenan and lota-carrageenan are associative polysaccharides from 0°C to the gelation temperature (about 40-60°C), whereas Kappa-carrageenan and lota-carrageenan are non-associative polysaccharides from gelation temperature (about 40-60°C) to 120°C. Lambda-carrageenan is a non-associative polysaccharide within the range of 0°C to 120°C. Preferably, the polysaccharide used in the method of the invention is non-associative at or within the temperature range used for the high-pressure treatment (see below).
[0063] The polysaccharide used in the present invention is preferably a hydrocolloid. As defined herein, hydrocolloids are polysaccharides which, when used as ingredients in a composition, impart functional properties to the composition, such as thickening, stabilizing or gelling. Whilst the term hydrocolloid is also sometimes used to refer to a colloidal system (e.g. gel) formed by such ingredients, as used herein the term refers to the ingredients themselves.
[0064] The polysaccharide (e.g. hydrocolloid) used in the present invention may be of any origin. For example, it may be extracted from biomass (e.g. plant-derived, animal derived, or crustacean derived), or it may be obtained via fermentation (e.g. bacteria, fungi, or microalgae- denved).
[0065] The polysaccharide may be a mixture of polysaccharides. The mixture of polysaccharides may be of the same or different origin.
[0066] Preferably, the at least one polysaccharide is carrageenan. A number of different types of carrageenan are known, which have different chemical structures (e.g. Kappa. Lambda, Iota, etc.). The carrageenan used in the present invention may comprise a single carrageenan type or a mixture of two or more different carrageenan t pes. The carrageenan polymer chains may be homopolymers, heteropolymers, or a mixture thereof.
[0067] The term ‘"depolymerized” (e.g. “depolymerized composition”) as used herein, means that the polysaccharide(s) in question have been partially or fully broken down into smaller molecules (e.g. smaller polysaccharides). Such depolymerization is evident upon comparison of the Mw of the polysaccharide prior to undergoing a depolymerization process versus the Mw after undergoing a depolymerization process. A reduction in Mw after undergoing the depolymerization process indicates that depolymerization has occurred. Thus, the Mw of the final depolymerized polysaccharide composition is dependent, in part, upon the Mw of the starting material. In one non-limiting embodiment, the polysaccharide composition in accordance with the invention has a Mw of 450 000 g / mol or less. Preferably, the composition has a Mw of from 200 000 g / mol to 450 000 g / mol.
[0068] In contrast to prior art chemical depolymerization methods, the method of the invention does not produce low molar mass chains (<50 000 g / mol) resulting in a greater control over the depolymerization of the polysaccharides such that a narrower molar mass dispersity is achieved. In other words, the inventive method allows the molar mass of the polysaccharides to be more finely tuned than is possible with prior art methods.
[0069] In one aspect, the invention relates to a method for producing a polysaccharide composition, comprising: obtaining an aqueous solution comprising a polysaccharide and at least one other soluble compound; and subjecting the aqueous solution to high pressure treatment.
[0070] In some embodiments, the aqueous solution consists of a polysaccharide and at least one other soluble compound. Preferably, the aqueous solution consists of carrageenan and at least one other soluble compound.
[0071] The step of obtaining an aqueous solution comprising a polysaccharide and at least one other soluble compound preferably involves obtaining an intermediate product formed during a hydrocolloid production process, or a derivative thereof. In some embodiments, the intermediate product is selected from a syrup, filtrate, fermentation broth, or a derivative thereof. Preferably, the intermediate product is a syrup or filtrate. In this way, the depolymerization method of the invention can advantageously be performed in-line during a hydrocolloid production process for optimal cost effectiveness.
[0072] Preferably, the aqueous solution is an aqueous carrageenan solution obtained during carrageenan production after seaweed extraction and soiid / liquid separation (e g. filtration). This aqueous carrageenan solution is sometimes referred to as “industrial syrup” or “seaweed juice”. The aqueous carrageenan solution also contains soluble compounds from seaweed. Since the solution is obtained after filtration it contains little or no insoluble compounds or fibres (e.g. sand, cellulose etc.).
[0073] In some embodiments, the at least one soluble compound in the aqueous solution is selected from salts, pigments, acids, bases, proteins, sugars, oligosaccharides, other polysaccharides, or combinations thereof.
[0074] In some embodiments, the concentration of the polysaccharide in the aqueous solution is from 0.1 to 6% by weight, preferably from 0.5 to 4% by weight. In some embodiments, the concentration of carrageenan in the aqueous solution is from 0.5 g / L to 30 g / L.
[0075] In some embodiments, the polysaccharide in the aqueous solution prior to being subjected to high pressure treatment has a weight average molar mass greater than 450 000 g / mol, preferably greater than 500 000 g / mol. Preferably the polysaccharide in the aqueoussolution prior to being subjected to high pressure treatment has a weight average molar mass of from 451 000 g / mol to 1 300 000 g / mol, more preferably from 500 000 g / mol to 1 300 000 g / mol, most preferably 900 000 g / mol to 1 300 000 g / mol.
[0076] The present invention advantageously relies on the use of physical means for depolymerizing polysaccharides, rather than chemical means, so that the resulting product may be considered more natural. More specifically, the method of the invention uses high pressure treatment. The high pressure treatment used is preferably a dynamic high pressure treatment, such as high pressure homogenization or microfluidization or similar. Most preferably, the high pressure treatment is high pressure homogenization.
[0077] During a typical high pressure homogenization process a high-pressure cylinder pump constrains a polymer solution to pass through a narrow gap. The speed of the solution rises to several m / s and creates a highly turbulent flow. The pressure applied is converted into kinetic energy7and the fluid will suffer intense shear rate and turbulent flow. As a consequence, degradation of the macromolecules occurs.
[0078] In some embodiments, the aqueous solution is subjected to multiple consecutive high pressure treatments (a.k.a “cycles7’), for example 2. 3, 4 or more consecutive high pressure treatments. This may involve passing the aqueous solution multiple times through the same high pressure equipment or passing the aqueous solution through different high pressure equipment in sequence. As used herein, reference to multiple consecutive high pressure treatments is distinct from the application of back pressure. In some embodiments back pressure may be used.
[0079] In some embodiments, the high pressure treatment is performed at an inlet pressure of from 0.1 to 100 MPa (1 to 1000 bar), preferably from 10 to 90 MPa (100 to 900 bar), more preferably from 15 to 85 MPa (150 to 850 bar), even more preferably from 20 to 80 MPa (200 to 800 bar), most preferably at 80 MPa (800 bar). If the aqueous solution is subjected to multiple consecutive high pressure treatments, one or more of the treatments may be performed at different inlet pressures, or all of the treatments may be performed at the same inlet pressure. For example, a first high pressure treatment may be performed at 20 MPa (200 bar), and then a second high pressure treatment may be performed at 80 MPa (800 bar). Preferably, at least one cycle of the high pressure treatment is performed at an inlet pressure of 80 MPa (800 bar). More preferably, two or more cycles of the high pressure treatment are performed at an inlet pressure of 80 MPa (800 bar).
[0080] In some embodiments, the high pressure treatment is performed at a temperature of from 10°C to 140°C, preferably 25°C to 140°C, more preferably from 25°C to 100°C, or from 50°C to 100°C. The specific temperature used will depend in part upon the type of polysaccharideused. Preferably, the temperature selected is such that the polysaccharide is in a non-associative state. Where the polysaccharide is carrageenan, the temperature used for high pressure treatment is preferably from 10°C to 100°C for Lambda carrageenan, or from 50°C to 100°C for Iota or Kappa carrageenan. Where a mixture of different carrageenan types is used, the temperature for high pressure treatment is preferably from 10°C to 100°C.
[0081] For example, according to the method of the invention, high pressure homogenisation may be performed on an aqueous solution comprising from 0.5 g / L to 30 g / L Carrageenan and having an initial Mw prior to treatment of 500 000 g / mol or more, using at least 1 cycle with an inlet pressure of 50 MPa (500 bar) or more, preferably using at least 1 cycle with an inlet pressure of 80 MPa (800 bar) or more.
[0082] The method of the invention may comprise additional processing steps such as precipitation, gelling, washing, drying, or grinding, in order to recover the polysaccharide (e.g. carrageenan). The polysaccharide obtained by the method is preferably in powder form.
[0083] In a preferred embodiment, the invention relates to a method for producing a carrageenan composition, comprising: obtaining an industrial syrup comprising carrageenan and at least one other soluble compound; and subjecting the industrial syrup to high pressure homogenization.
[0084] The present invention further relates to a polysaccharide composition obtained or obtainable by the method of the invention. In addition to the benefits of producing natural carrageenan, it was surprisingly found that high pressure homogenization (HPH) treated carrageenan produces stronger gels than carrageenan that was depolymerized using a chemical means with the same Mw.
[0085] The present invention further relates to the use of high pressure treatment to depolymerize a polysaccharide during a hydrocolloid production process. In one embodiment the invention relates to the use of high pressure treatment to depolymerize carrageenan during a carrageenan production process.
[0086] The present invention further relates to a carrageenan composition having a dispersity of 1.70 or less.
[0087] The composition may have a weight average molar mass of 450 000 g / mol or less and / or less than 5% of the carrageenan molecules in the composition may have a molar mass below 50 000 g / mol. Preferably, the carrageenan composition is a depolymerized composition as defined above. The carrageenan composition is obtainable by the method of the invention because it enables greater control of molar mass dispersity than prior art methods.
[0088] '’Dispersity" (D) as used herein is synonymous with the alternative term “Polydispersity Index’’ which is sometimes used in the field of the invention.
[0089] D = Mw / Mn, where Mw is the weight average molar mass and Mn is the number average molar mass. When D tends to 1 it means that the population of molecules in the composition is monodisperse (i.e. they all contain the same number of repeating units).
[0090] Without being bound by theory, it is believed that applying high pressure treatment (e.g. high pressure homogenization) to the aqueous solution preferentially depolymerizes the macromolecules with the highest molar mass, thereby decreasing the dispersity of the carrageenan composition, while limiting the production of low molar mass molecules. This is thought to be in contrast with the mechanism of depolymerization using chemical means, e.g. HC1 or H2O2.
[0091] The dispersity of the depolymerized carrageenan composition is 1.70 or less, preferably 1.66 or less, more preferably 1.60 or less. Preferably, the dispersity of the depolymerized carrageenan composition is from 1.00 to 1.70, more preferably from 1.20 to 1.60.
[0092] In some embodiments, the composition has a weight average molar mass of 450 000 g / mol or less, or 400 000 g / mol or less, or 350 000 g / mol or less, or 300 000 g / mol or less. Preferably, the composition has a weight average molar mass of from 200 000 g / mol to 450 000 g / mol.
[0093] In some embodiments, less than 5% of the carrageenan molecules in the composition have a molar mass below 50 000 g / mol.
[0094] In some embodiments, no more than 12% of the carrageenan molecules in the composition have a molar mass of 100 000 g / mol or less. In other embodiments, no more than 11 %, or 10%, or 9%, or 8%, or 7%, or 6%, or 5% of the carrageenan molecules in the composition have a molar mass of 100 000 g / mol or less.
[0095] The composition may further comprise one or more other compounds selected from salts, pigments, acids, bases, proteins, sugars, oligosaccharides, other polysaccharides, or combinations thereof.
[0096] The composition may be in liquid or powder form.
[0097] Representative features of the present invention are set out in the following clauses, which stand alone or may be combined, in any combination, with one or more features disclosed in the text of the specification:
[0098] Clause 1 : A method for producing a polysaccharide composition, comprising: obtaining an aqueous solution comprising a polysaccharide and at least one other soluble compound; and subjecting the aqueous solution to high pressure treatment.
[0099] Clause 2: The method of clause 1, wherein the at least one soluble compound is selected from salts, pigments, acids, bases, proteins, sugars, oligosaccharides, other polysaccharides, or combinations thereof.Clause 3: The method of clause 1 or clause 2, wherein the aqueous solution does not contain insoluble fibres or compounds.Clause 4: The method of any preceding clause, wherein the aqueous solution is an intermediate product formed during a hydrocolloid production process, or a derivative thereof.Clause 5: The method of clause 4, wherein the intermediate product is selected from a syrup, filtrate, fermentation broth, or a derivative thereof.Clause 6: The method of any preceding clause, wherein the concentration of the polysaccharide in the aqueous solution is from 0. 1 to 6% by weight, preferably from 0.5 to 4% by weight.Clause 7: The method of any preceding clause, wherein the aqueous solution is subjected to multiple consecutive high pressure treatments.Clause 8: The method of any preceding clause, wherein the high pressure treatment is performed at an inlet pressure of from 0. 1 to 100 MPa (1 to 1000 bar), preferably from 20 to 80 MPa (200 to 800 bar).Clause 9: The method of any preceding clause, wherein the high pressure treatment is performed at a temperature of from 10°C to 140°C.Clause 10: A polysaccharide composition obtained using the method of any preceding clause.Clause 11 : Use of high pressure treatment to depolymerize a polysaccharide during a hydrocolloid production process.Clause 12: The method of any one of clauses 1 to 9, the composition of clause 10, or the use of clause 11, wherein the polysaccharide is a non-associative polysaccharide.Clause 13: The method of any one of clauses 1 to 9, the composition of clause 10 or the use of clause 11, wherein the polysaccharide is extracted from biomass or obtained via fermentation. Clause 14: The method of any one of clauses 1 to 9, the composition of clause 10, or the use of clause 11, wherein the polysaccharide is carrageenan.Clause 15: A carrageenan composition having a dispersity of 1.70 or less.Clause 16: The carrageenan composition of clause 15, wherein the composition has a weight average molar mass of 450 000 g / mol or less.Clause 17: The carrageenan composition of clause 15 or clause 16, wherein less than 5% of the carrageenan molecules in the composition have a molar mass below 50 000 g / mol.Clause 18: A carrageenan composition according to any one of clauses 15 to 17, wherein no more than 12% of the carrageenan molecules in the composition have a molar mass of 100 000 g / mol or less.
[0100] The present invention is further illustrated by the following examples, which are not to be construed as limiting the scope of the invention.EXAMPLESMaterials and Methods for Examples 1-4Materials:
[0101] The materials used in the examples below are as follows:• Carrageenan: “kappa like'’ from Cottonii (unless otherwise specified)• Reverse osmosis water• KC1: VWR (purity >99.5%)• Solution preparation: mechanical stirrer and water bath• Solution stirring: mechanical stirrer IKA RW20• High pressure homogeniser (HPH): APV 1000 (SPX flow)• Brookfield viscosity : Brookfield DV2T-LV• Industrial Syrup was collected on a Cargill Inc. carrageenan production line. The carrageenan concentration is about 1.37 % (determined by lab IPA recovery).• Haake viscosity: Haake VT-550Sample preparation:
[0102] The carrageenan powder was dispersed at room temperature in reverse osmosis water using a mechanical stirrer. Then the solution was heated up to 80°C under stirring. After about 10 min at 80°C the carrageenan solution was ready for use. The carrageenan solution was kept at 80°C throughout the experiments.
[0103] For trials with salt, the carrageenan solution was prepared starting from saline solution (2 g / L KC1) instead reverse osmosis water.
[0104] Industrial syrup was collected on a Cargill production line and frozen at -19°C before use. For the study, it was melted and heated up to 80°C.Intrinsic viscosity:
[0105] Intrinsic viscosity was measured using known chromatography methods. The sample preparation was adapted as follows. An aliquot of carrageenan solution (Table 1) was taken out and diluted with the proper amount of GPC eluent to reach the carrageenan concentration of 0.05% (optimal concentration for GPC analysis). 2 columns TSK GMPWXL 7.8x 300 mm are used in series. The following parameters are used:• Flow: 0.6 mL / min• Mobile phase: 0. 1 M LiNCb, 1 g / L EDTA, pH 7• Oven temperature: 60°C• Injection volume: 0.2 mL• Prefilter: 0.1 pm• GPC software: Astra or Omnisec
[0106] The value of dn / dc used is 0. 115.
[0107] The Intrinsic viscosity is determined by integration of the chromatograms.
[0108] Reduction in Intrinsic viscosity indicates depolymerization.Brookfield viscosity at 75°C determination:
[0109] The solution sample was heated up to 75°C whilst stirring. The Brookfield viscosity was measured with a Brookfield DV2T-LV viscosimeter at 30 rpm. The viscosity of the solutions was directly measured (1, 1.5, 2% in carrageenan concentration) using suitable spindle.
[0110] Reduction in Brookfield viscosity indicates depolymerization.Table 1 : Sampling conditions for GPC analysis.Haake Analysis:
[0111] Two types of analysis were performed with the Haake VT-550:• Ameasure of viscosity' was done at 80°C. The shear rate was set up at 10 s’1. There were 5 minutes of stabilization and then the viscosity was recorded during 2 minutes with one measure per second. The results presented are an average of these 120 measures. A reduction in viscosity indicates depolymerization.• To characterize the solution obtained, a flow curve was recorded. The device scans a range of 1 to 1000 s’1upon 180 seconds. 300 measures are recorded on logarithmic scale.
[0112] For all the experiment the mobile NV was used. This mobile is used to measure the low viscosities.Rate of Loss calculation:
[0113] The rate of loss is calculated using the initial viscosity before the HPH experiment as a reference:Materials and Methods for Examples 5 to 12Materials:
[0114] The materials used in the examples below are as follows:• Carrageenan: “hybrid like” from Iridaea or Gigartina (unless otherwise specified)• Reverse osmosis water• KC1, NaOH, Na2CCh high purity• Solution preparation: mechanical stirrer and water bath• Solution stirring: mechanical stirrer IKA RW20• High pressure homogeniser (HPH): APV 1000 (SPX flow)• Brookfield viscosity: Brookfield DV2T-RVCarrageenan solution preparation:
[0115] The carrageenan powder was dispersed at room temperature in saline solution (usually 5 g / L KC1 in reverse osmosis water) using a mechanical stirrer.
[0116] The solution stays under mechanical stirring until complete dissolution.
[0117] For some trials, the solution was then heated up to the desired temperature.Brookfield viscosity at 25°C determination:
[0118] The Brookfield viscosity7was measured with a Brookfield DV2T-RV viscosimeter at 30 rpm. The viscosity' of the solutions was directly measured using suitable spindle.
[0119] Reduction in Brookfield viscosity indicates depolymerization.GPC (Gel Permeation Chromatography) and sample preparation:
[0120] GPC sample preparation from a powder.100 mg of carrageenan powder is dissolved in 80 mL of ultra-pure water. The solution is stirred for 30 min at 60°C, and cooled down under stirring for another 30 min. The total mass of thesolution is then adjusted to 100 g with ultra-pure water. 5g of the prepared solution is mixed with 5 g of a twice-concentrated eluant solution (0.2 M Li NO? and 2 g / L EDTA, pH=9). The solution is filtered with a syringe-filter. The sample can then be analyzed via GPC.
[0121] GPC sample preparation from a solution.GPC sample is prepared by mixing an eluant-type solution (containing L1NO3 and EDTA at pH=9) and a carrageenan solution in the proper ratio to reach in the final vial: 0.05 wt. % of carrageenan, 0.1 M of LiNCh, 1 g / L EDTA at pH=9. The solution is filtered with a syringe-filter before being analyzed via GPC.
[0122] GPC conditions:• Eluant type: aqueous solution of 0. 1 M L1NO3 and 1 g / L EDTA at pH=9• Eluant flow: 0.5 mL / min• GPC: Agilent series 1260 Infinity for sampler and oven - Shimadzu LC-20AD SP for pump• Oven: 50°C• Columns: 2 consecutive columns, PSS Suprema Ultrahigh 8*300 mm 10 pm + 1 columns PSS Suprema 100A 10 pm 8*300 mm• Molar mass detector: Multi-angle laser light scattering (MALLS), Wyatt MALLS DAWN Temperature regulated 3500-D3TR, set at 50°C• Concentration detector: Differential Refractometric Index (DRI) detector, Wyatt T-rEX Optilab, set at 50°C• GPC software: Astra from WyattDetermination ofMw, Mn and Dispersity:
[0123] In order to determine the Mw. Mn and Dispersity (D), we need to consider the signals from both detectors (MALLS and DRI). Using the signal from DRI, the peak of the carrageenan is integrated as illustrated on FIG. 21 . The Mw, the Mn and the dispersity (D) could therefore be determined.Determination of % of carrageenan below 100000 or 50000 g / mol:
[0124] Contrary to the determination of Mw, Mn and Dispersity, a fitting is required to define the percentage of carrageenan below 100 000 or 50 000 g / mol. The curve of the molar mass as a function of the retention time is a straight line on most of the chromatograms but, for high retention time (corresponding to the low molar mass carrageenan) and because of the low concentration, this curve is less accurate. To overcome this limitation, a mathematic extrapolation is used to extend this curve by a theoretical straight line for high retention time allowing to determine the fraction of low molar mass carrageenan. The limit of quantification of the percentage of carrageenan below 50,000 g / mol and 100,000 g / mol is approximately 5%.EXAMPLE 1
[0125] Carrageenan solutions in accordance with the values in table 2 shown below were prepared using the sample preparation method described above. The carrageenan solutions were then subjected to high pressure homogenization. The inlet pressure was settled at either 25 or 85 MPa (250 or 850 bar). The carrageenan solution was subjected to from 0 to 4 consecutive cycles. After each homogenization cycle, the fluid sample was maintained at 80°C using a water bath to avoid carrageenan gelation and to control the experiment temperature. The Brookfield and intrinsic viscosities were measured before and after each cycle.
[0126] Three parameters were analyzed:• The inlet pressure (the back pressure was kept constant at 5 MPa (50 bar)),• The number of consecutive cycles,• The presence (or not) of salt.Table 2: Process conditions for the HPH treatment at 80°C.
[0127] The samples 250-KC10 and 850-KC10 permit to determine the impact of the pressure applied. The comparison between 250-KC10 and 250-KC12 and between 850-KC10 and 850- KC12 allows one to conclude on the salt effect.ResultsBrookfield viscosity:
[0128] In FIGs. 1 to 3b we can observe the change of the Brookfield viscosity values proportionally linked to the molar mass. We can conclude that:• There is the same tendency of the impact of the number of consecutive cycles whatever the experimental conditions. The higher the number of cycles, the lower the Brookfield viscosity of the solution.• The first HPH cycle is the most impacting (between 70% and 80% of the value after 4 consecutive cycles)• The higher the inlet pressure, the higher the depolymerization.• A limit value is reached depending on the number of consecutive cycles and the inlet pressure. The loss of viscosity is 90% for 850 bar and 55% at 250 bar after 3-4 consecutive cycles• The salt decreases the apparent viscosity of the carrageenan solution, following established theory, since the carrageenan chain is polyanion. However, it does not impact the effect of the HPH treatment as demonstrated by the rate of loss in viscosity when applying 850 bar and limited influence with 250 bar.Intrinsic viscosity:
[0129] The results obtained in FIGs. 4 and 5 confirm the conclusion disclosed by the Brookfield viscosity. The inlet pressure and the number of consecutive cycles promote the depolymerization. The salt has only a little impact for a low pressure.
[0130] Interestingly, the intrinsic viscosity decreases slower with the number of consecutive cycles than the Brookfield viscosity (FIG. 2 versus FIG. 5). In addition, the loss of the intrinsic viscosity seems to be less significant than the loss of Brookfield viscosity' (32% and 55% loss of intrinsic viscosity versus 52% and 90% loss of Brookfield viscosity applying 250 and 850 bar respectively).EXAMPLE 2
[0131] Carrageenan solutions and industrial syrup were prepared in accordance with the values in Table 3 shown below using the sample preparation methods described above. The carrageenan solutions and industrial syrup were then subjected to one cycle of high pressure homogenization at several inlet pressures: 0, 20, 40, 60, and 80 MPa (0, 200, 400, 600, and 800 bar). The back pressure was settled at 5 MPa (50 bar). The Brookfield, Haake and intrinsic viscosities were measured for each condition directly from the carrageenan solution.Table 3: Process conditions for the HPH treatment at 80°C.
[0132] The samples C1-KC10, C1.5-KC10, and C2-KC10 allow to determine the impact of the carrageenan concentration.
[0133] The presence of salt in a carrageenan solution usually decreases the apparent viscosity without impacting the molar mass of carrageenan. To conclude on the influence of the salt during the treatment C1-KC12, C1.5-KC12, and C2-KC12 were respectively compared with Cl- KC10, C1.5-KC10, and C2-KC10.ResultsImpact of Inlet pressure:
[0134] FIGs. 6a, 6b, and 6c report the Brookfield, Haake and intrinsic viscosities of the 1.5% carrageenan solutions without KC1.
[0135] In all cases, the higher the inlet pressure, the stronger the decrease in viscosity, the higher the degradation. The impact is higher on Haake and Brookfield viscosities than on the intrinsic viscosity. For Brookfield and Haake viscosities the values reach a plateau contrary to the intrinsic viscosity.
[0136] The same tendency is observed whatever the process conditions (1%, 1.5% and 2% in carrageenan and with (2 g / L) or without KC1) (FIG. 7).Impact of carrageenan concentration:
[0137] FIGs. 7 and 8 represent the intrinsic viscosity of the carrageenan solutions without and with 2 g / L KC1 respectively.
[0138] At low inlet pressure, there was no significant difference of the intrinsic viscosity according to the carrageenan concentrations. However, at high inlet pressure (600 and 800 bar), the higher the carrageenan concentration, the lower the degradation.
[0139] For the Brookfield and Haake viscosities the carrageenan concentration did not have a significant influence.Impact of salt (KC1):
[0140] There was no significant difference for the solutions with or without salt.
[0141] The same results are observed for Brookfield and Haake viscosities.
[0142] The same tendency is observed whatever the carrageenan concentrations.Flow behaviour:
[0143] FIGs. 9 and 10 show the flow curves of 1.5% carrageenan solutions respectively without and with 2 g / L KC1 according to several inlet pressures. At this carrageenan concentration at 80°C, the solutions present a behavior similar to Newtonian fluids with a viscosity level depending on the inlet pressure applied: the higher the inlet pressure, the lower the viscosity. The same tendency is observed for all carrageenan concentrations.Industrial syrup:
[0144] FIGs. Ila, 11b, and 11c report the Brookfield, Haake and intrinsic viscosities respectively of the industrial syrup after HPH treatment with several inlet pressures.
[0145] Advantageously, the same effect of the HPH is observable as described above for the model carrageenan solutions. The higher the inlet pressure, the higher the degradation. Once again the loss in intrinsic viscosity is lower than the losses in Haake and Brookfield viscosities.
[0146] FIG. 12 reports the flow curves of the industrial syrup exposed to several inlet pressures. Once again, the same behavior as the model solutions is surprisingly observed.
[0147] These results are surprising because the medium obtained from the hydrocolloid production process (i.e. the industrial syrup) is more complex (presence of salt, other components such as pigments, proteins etc.).
[0148] These results indicate that high pressure homogenization may be advantageously applied within the carrageenan production process to depolymerize the carrageenan.EXAMPLE 3
[0149] Example 2 was repeated using two samples of iota carrageenan (extracted from spinosum). Only solutions containing 1.5% carrageenan were considered. The intrinsic viscosities were measured for each condition directly from the carrageenan solution.
[0150] FIG. 18 shows the intrinsic viscosities of the 1.5% carrageenan solutions with 2 g / L KC1 (KC12) or without KC1 (KC10). In all cases, the higher the inlet pressure, the stronger the decrease in intrinsic viscosity7. The salt does not impact the effect of the HPH. By comparing the two iota extracts having different starting intrinsic viscosity, it appears that the higher the starting intrinsic viscosity, the stronger the effect of the HPH at similar inlet pressure.EXAMPLE 4
[0151] Example 2 was repeated using a lambda carrageenan (extracted from tretrasporophyte sarcothalia crispaia). however HPH treatment was performed at room temperature. The intrinsic viscosities and the Brookfield viscosity were measured for each condition directly from the carrageenan solution.
[0152] FIGs. 19a and 19b show the intrinsic viscosity7and the Brookfield viscosity7of the 1% carrageenan solutions with 2 g / L KC1. In all cases, the higher the inlet pressure, the stronger the decrease in intrinsic viscosity and Brookfield viscosity.
[0153] Based on the results of examples 1-4, whatever the carrageenan type (kappa, iota, lambda) HPH has the same advantageous effect.EXAMPLE 5 (COMPARATIVE)
[0154] Commercial samples of carrageenan were obtained and the Mn, Mw, D, % molecules <50,000 g / mol, and % molecules <100,000 g / mol were analyzed according to the methods recited above. The commercial samples included several types of carrageenan including kappa, iota, lambda, and hybrid. The commercial samples were not subjected to high pressure treatment. Results are shown in Table 4.Table 4: Analysis of commercial samples.EXAMPLE 6 (COMPARATIVE)
[0155] Carrageenan depolymerisation by Hydrogen Chloride.• Carrageenan solutions at 10 g / L and 5 g / L of KC1 are prepared under mechanical stirring.• A hydrochloric acid solution (Hydrochloric acid, fuming. 37% solution in water) is added to the carrageenan solution to reach pH 4.• The solution is then heated to 80°C. A reference is sampled.• Samples are collected after 10 min, 20 min. 30 min, 1 h and 2 h of reaction at 80°C.• Each collected sample was directly placed in an ice bath to stop the reaction. GPC samples are prepared from each collected samples (following the method described above).
[0156] Mn, Mw, Dispersity, % of molar mass < 50,000 or < 100,000 g / mol are reported in the table for the 10 g / L carrageenan and 5 g / L KC1. Chromatograms of some samples are reported in Table 5 and FIG. 13.Table 5: Depolymerization of carrageenan by HC1.
[0157] FIG. 13 shows a global shift of the distribution of the molar mass, attesting to a statistical depolymerization which tends to even depolymerize in priority the smallest molar mass.EXAMPLE 7
[0158] Carrageenan depolymerization using high pressure homogenization. Investigating the impact of pressure, the number of consecutive cycles, and carrageenan concentration.• Carrageenan solutions of varying concentrations (1, 5.5, or 10 g / L) with 5 g / L of KC1 were prepared under mechanical stirring.• The solutions were then passed through the HPH equipment at room temperature at the desired pressure. Where indicated, the solution was passed several times through the HPH equipment.• Each sample was collected and prepared according to the GPC method described.
[0159] Mn, Mw, Dispersity, % of molar mass < 50,000 or < 100,000 g / mol of the samples are reported in Tables 6-8 for the different carrageenan concentrations. Chromatograms of some samples are reported in FIGs. 14a, 14b, 15a, 15b, and 16.Table 6: HPH depolymerization of Carrageenan 1 g / LTable 7: HPH depolymerization of Carrageenan 10 g / Lnm: non measuredTable 8: HPH depolymerization of Carrageenan 5.5 g / Lnm: non measured
[0160] The following conclusions may be drawn from the data in Tables 6-9, which are indicative of the advantages of the invention.• The depolymerization of carrageenan is immediate after the HPH treatment; it does not require a specific time unlike other methods, e.g. HC1 depolymerization.• The higher the number of consecutive cycles, the harsher the depolymerization, and the lower the molar mass (Mw and Mn).• The higher the pressure, the harsher the depolymerization, and the lower the molar mass (Mw and Mn).• The lower the carrageenan concentration, the harsher the depolymerization, and the lower the molar mass (Mw and Mn).• Whatever the HPH conditions, the dispersity of the resulting sample is always below" 1.70 even after only one cycle, even at the lowest pressure, even at the highest carrageenan concentration. This dispersity is significantly lower than the reference (0 bar pressure).
[0161] The chromatograms in FIGs. 14a. 14b, 15a. 15b, and 16 clearly demonstrate that the mode of depolymerization of HPH treatment is significantly different from that of traditional chemical depolymerization (e.g. by HC1). For HPH, only the biggest molecules (eluted at the shorter time) are broken down; the HPH does not impact the smaller molecules (eluted at the longer time). This depolymerization method is, as a consequence, particularly interesting for texturizer applications since it avoids generating low molar mass molecules which do not play a role in texture functionality.EXAMPLE 8
[0162] Investigating the impact of the initial molar mass of carrageenan. Samples were prepared according to Example 5 with varying initial molar mass of carrageenan. Results are show n in Table 9.Table 9: Impact of initial Mw of carrageenan.In conclusion, whatever the initial molar mass of the carrageenan, the effects of the HPH treatment are similar to what was described in Example 5.EXAMPLE 9
[0163] Further investigation into the impact of high carrageenan concentration and HPH treatment temperature. Samples were prepared in accordance with Example 5, with varying carrageenan concentrations of 0.5, 10, and 22.5 g / L. The solution at 0.5 g / L was processed at room temperature, whilst the solutions at 10 and 22.5 g / L were processed at 65-75°C. Results are shown in Table 10.Table 10: Impact of very low and very high carrageenan concentration.EXAMPLE 10
[0164] HPH treatment on extraction syrup / filtrate. Gigartina seaweed was extracted in water using salt (KC1) and soft alkali (Na2COs) at 70°C for 4 h under mechanical stirring. After dilution with hot water, the slurry was hot-filtered under vacuum through a cloth filter withfiltering aid supported in a Buchner funnel. The filtrate (liquid part) was treated by HPH at 70°C. Results are shown in Table 11 and FIG. 17. In this case the medium is the liquid fraction of the seaweed extraction (i.e. industrial syrup), which contains multiple water-soluble compounds in addition to carrageenan (estimated at -5 g / L), salt, alkali, coloring compounds, etc. Since it is after solid / liquid separation, the medium contains no significant fraction of insoluble compounds (such as sand, cellulose, etc.).Table 11: HPH on filtered Gigartina seaweed extract.EXAMPLE 11
[0165] HPH treatment on extraction syrup / filtrate. Cottonii seaweed was extracted in water using alkali (NaOH) at 90°C for 17 h under mechanical stirring. After dilution with hot water, the slurry was hot-filtered under vacuum through a cloth filter with filtering aid supported in a Buchner funnel. The filtrate (liquid part) was treated by HPH at 90°C. Results are shown in Table 12 and FIGs. 20a and 20b for the two samples respectively. This trial was conducted on two cottonii samples from different ongins. In this case, the medium is the liquid fraction of the seaweed extraction (i.e. industrial syrup), which contains multiple water-soluble compounds in addition to carrageenan (estimated at -8-10 g / L), salt, alkali, coloring compounds, etc. Since it is after solid / liquid separation, the medium contains no insoluble compounds such as sand, cellulose, etc. (trace amounts may be present).Table 12: HPH on filtered Cottonii seaweed extract.EXAMPLE 12
[0166] Comparison between HPH and chemical depolymerization. Kappa carrageenan (extracted from cottonii) was treated with hydrogen peroxide or HPH in order to reach approximately the same weight average molar mass. The samples were characterized in milk and KC1 solution. These results are shown in table 13.
[0167] The HPH treatment resulted in depolymerized carrageenan with significantly lower dispersity than was achieved using chemical treatment.Table 13: Carrageenan obtained after H2O2 vs. HPH treatment
[0168] Maximum gel strength and viscosity of the samples was tested. These results are shown in Table 14.Table 14: Properties of carrageenan obtained after H2O2 vs. HPH treatment
[0169] The results show that HPH treated Kappa carrageenan produces stronger gels than chemically treated Kappa carrageenan.
Claims
CLAIMS1. A method for producing a polysaccharide composition, comprising: obtaining an aqueous solution comprising a polysaccharide and at least one other soluble compound; and subjecting the aqueous solution to high pressure treatment.
2. The method of claim 1, wherein the at least one soluble compound is selected from salts, pigments, acids, bases, proteins, sugars, oligosaccharides, other polysaccharides, or combinations thereof.
3. The method of claim 1 or 2, wherein the aqueous solution does not contain insoluble fibres or compounds.
4. The method of any preceding claim, wherein the aqueous solution is an intermediate product formed during a hydrocolloid production process, or a derivative thereof.
5. The method of claim 4, wherein the intermediate product is selected from a syrup, filtrate, fermentation broth, or a derivative thereof.
6. The method of any preceding claim, wherein the concentration of the polysaccharide in the aqueous solution is from 0.1 to 6% by weight, preferably from 0.5 to 4% by weight.
7. The method of any preceding claim, wherein optionally the aqueous solution is subjected to multiple consecutive high pressure treatments.
8. The method of any preceding claim, wherein the high pressure treatment is performed at an inlet pressure of from 0.1 to 100 MPa (1 to 1000 bar), preferably from 20 to 80 MPa (200 to 800 bar).
9. The method of any preceding claim, wherein the high pressure treatment is performed at a temperature of from 10°C to 140°C.
10. A polysaccharide composition obtainable by or obtained using the method of any preceding claim.11 . Use of high pressure treatment to depolymerize a polysaccharide during a hydrocolloid production process.
12. The method of any one of claims 1 to 9, the composition of claim 10, or the use of claim 11, wherein the polysaccharide is a non-associative polysaccharide.
13. The method of any one of claims 1 to 9, the composition of claim 10 or the use of claim 11. wherein the polysaccharide is extracted from biomass or obtained via fermentation.
14. The method of any one of claims 1 to 9, the composition of claim 10, or the use of claim 11. wherein the polysaccharide is carrageenan.
15. A carrageenan composition having a dispersity of 1.70 or less.
16. The carrageenan composition of claim 15, wherein the composition has a weight average molar mass of 450 000 g / mol or less.
17. The carrageenan composition of claim 15 or claim 16, wherein less than 5% of the carrageenan molecules in the composition have a molar mass below 50 000 g / mol.
18. A carrageenan composition according to any one of claims 15 to 17, wherein no more than 12% of the carrageenan molecules in the composition have a molar mass of 100 000 g / mol or less.