Modified citrus fiber product

Abstract

The present invention relates to a modified citrus fiber product, wherein the modified citrus fiber product has a gel strength of from 30 SAG to 100 SAG and a degree of esterification of from 30% to 100%. The invention also relates to a method for producing said modified citrus fiber product. The present invention avoids the use of an activation step involving the conversion of trapped water-insoluble pectin to free water-soluble pectin using chemicals (e.g., acids) while still obtaining a suitable amount of free water-soluble pectin to produce a citrus fiber product having a gel strength (SAG) of between 30 SAG and 100 SAG. Avoiding such an activation step ensures that the intrinsic factors of the pectin contained in the modified citrus fiber product are comparable to those found in the natural citrus fiber source.

Description

[0001] Cross-reference to related applications

[0002] This application claims the benefit of European Application No. 23201623.8, filed on 4 October 2023, the disclosure of which is incorporated herein by reference in its entirety. Technical Field

[0003] This invention relates to a modified citrus fiber product, a method for producing the modified citrus fiber product, compositions and consumer products comprising the modified citrus fiber product, and the use of said modified citrus fiber product. In particular, this invention relates to a modified citrus fiber product and a method for producing said modified citrus fiber product, wherein the modified citrus fiber product has a gel strength (°SAG) greater than that of natural citrus fibers found in citrus fiber sources (e.g., citrus peel) and a degree of esterification substantially the same as that of natural citrus fibers found in citrus fiber sources. Background Technology

[0004] Citrus fiber is a dietary fiber derived from citrus fruits, particularly from citrus peels. Citrus fibers, in various forms, are widely used in industries such as food and consumer goods due to their thickening, water-absorbing, swelling, emulsifying, and texturizing properties.

[0005] Citrus fiber is primarily composed of water-soluble and water-insoluble fibers. Water-insoluble fibers include cellulose and hemicellulose, while water-soluble fibers include pectin. In solution, pectin concentration is positively correlated with the gelling ability of the solution. Other intrinsic factors, such as the degree of pectin esterification, also actively contribute to the gelation of the solution. Therefore, although important, the amount of pectin is not the sole factor determining the gelling ability of a pectin-containing solution. Thus, pectin-containing products require a balance between the amount of pectin obtained from the pectin source and the need to maintain the inherent properties of pectin, such as the degree of esterification, to ensure that the pectin-containing product exhibits optimal gelling properties.

[0006] Natural citrus fiber typically contains about 20% to 40% pectin, with the remainder consisting of insoluble citrus fibers (cellulose and hemicellulose) and other components. However, most of the pectin found in citrus peel is trapped / mixed with other insoluble components of the cell walls of the citrus peel, such as cellulose and hemicellulose. This "trapped pectin" cannot break free from the cellulose matrix of the cell walls and diffuses and dissolves in water. A small fraction of the total pectin content in citrus peel is freely available ("free pectin"), i.e., not trapped / mixed with other insoluble fibers, and therefore readily soluble in water. The amount of free / soluble pectin and its inherent properties (such as the degree of esterification) determine the gel strength (°SAG) of pectin-containing products, and therefore efforts have been made to produce citrus fiber products with high free / soluble pectin content while retaining inherent properties (such as the degree of esterification of free / soluble pectin).

[0007] In an attempt to release trapped pectin, some citrus fiber products have been produced by placing citrus peels or pulp in water, followed by drying and grinding the peels. Because no "activation" step occurs to convert the trapped pectin into free pectin, the resulting ground citrus fiber has a water-soluble pectin content similar to that of natural citrus peels. Most of the pectin remains trapped within the cellulose / hemicellulose matrix, meaning that the citrus fiber product obtained by this method has a low free water-soluble pectin content. Consequently, the gel strength of the citrus fiber product obtained by this method is low.

[0008] Attempts have also been made to extract pectin from citrus peels, i.e., to remove pectin from citrus fiber sources. This involves using acid extraction methods (such as acid hydrolysis) to extract most of the pectin from the citrus peel. The extracted pectin will be water-soluble because it is extracted from the environment of the citrus peel, which traps the pectin and prevents it from dissolving. The resulting citrus fiber product (i.e., the component of the citrus peel remaining after pectin extraction) can potentially be processed, dried, and ground. However, due to the depletion of the pectin contained within the citrus peel before processing, almost no water-soluble pectin is present in this citrus fiber product. Therefore, even though the viscosity from the insoluble fiber portion can be increased through processing, the gelling ability of the citrus fiber product obtained by this method is low.

[0009] In the context of citrus fiber products, further attempts to increase the amount of "free pectin" involve activation steps to release pectin trapped in the cellulose / hemicellulose matrix and recover both free pectin and cellulose / hemicellulose together. Such activation steps involve immersing citrus peel in an acidic environment with or without additional chemicals such as solvents. The acid treatment partially degrades cellulose / hemicellulose and pectin in the cell walls of the citrus peel, causing the water-insoluble pectin trapped within the peel to be converted into free, water-soluble pectin. The activated citrus peel is then dried and milled to produce the citrus fiber product. While this acid activation can increase the amount of "free pectin" in the final citrus fiber product, the inherent properties of free soluble pectin, particularly the degree of esterification, are affected by the acid's influence on the pectin structure. Therefore, while acid activation of citrus peel can increase the amount of "free pectin" in the final citrus fiber product, the internal properties of this "free pectin" (i.e., the degree of esterification) are impaired, resulting in lower gelling properties compared to natural free pectin. Furthermore, citrus fiber products cannot be considered "label-friendly" because the inherent properties of the pectin contained in these products (such as the degree of esterification) have been altered to such an extent that they no longer resemble natural pectin from citrus peel, but rather pectin extracted through conventional acid extraction.

[0010] WO 2018 / 149893 A1 discloses treating pectin-containing biomass with an activating solution containing alcohol and acid to convert entrapped water-insoluble pectin into free soluble pectin. Due to the acidic treatment of natural citrus peel, the resulting citrus fiber has a higher amount of freely available water-soluble pectin. However, a problem with this method is that the inherent properties of the released pectin, such as the degree of esterification, are reduced compared to natural pectin from citrus peel. Therefore, the resulting citrus fiber product is not "label-friendly".

[0011] US 5,567,462 discloses a method for obtaining citrus fiber products by combining citrus peel with an acidic or alkaline aqueous solution under conditions that at least partially dissolve the pectin present in the peel. An alcohol is then used to precipitate the pectin, and the resulting fiber is then dried. While this treatment can produce a greater quantity of freely available water-soluble fiber, again due to the acidic treatment of the natural citrus peel, the inherent properties of the released pectin (such as the degree of esterification) are reduced compared to natural pectin from the citrus peel. Therefore, the resulting citrus fiber product is not "label-friendly."

[0012] WO 91 / 15517 A1 discloses a method for obtaining citrus fiber by combining citrus peel with acid to release entrenched water-insoluble pectin. The resulting solution is then dried in a drying cabinet to obtain dried citrus fiber. Again, due to the acid treatment of natural citrus peel, a larger amount of freely available water-soluble pectin is released, but the inherent properties of the released pectin (such as the degree of esterification) are reduced compared to natural pectin from citrus peel. Therefore, the resulting citrus fiber product is not "label-friendly".

[0013] Therefore, there is a need for a citrus fiber product having a higher amount of free soluble pectin compared to that found in natural citrus peel, while retaining the inherent properties of pectin (such as esterification degree) to resemble those found in natural citrus peel. Due to the higher amount of soluble pectin and the retained esterification degree, any such citrus fiber product would have improved gelling properties compared to citrus fiber products produced simply by grinding citrus peel. Retaining those typical inherent properties found in citrus peel (such as esterification degree) also ensures that the citrus fiber product is “label-friendly,” unlike citrus fiber products using acid-based activation steps. A method for obtaining said citrus fiber product from a citrus fiber source is also needed. This invention provides such improved citrus fiber products and methods for producing them, and thus solves the problems associated with the prior art. Summary of the Invention

[0014] In one embodiment, the present invention provides a modified citrus fiber product wherein the citrus fibers have a gel strength of 30°SAG to 100°SAG and a degree of esterification (DE) of 30% to 100%. Compared to what is seen in citrus fiber sources, the modified citrus fiber product contains an increased amount of freely available water-soluble citrus fiber (pectin), meaning that the modified citrus fiber of the present invention has improved gelling properties. Furthermore, the DE of the modified citrus fiber is comparable to that of natural citrus fiber found in citrus fiber sources, thus the inherent properties of the pectin contained in the modified citrus fiber product are substantially the same (if not different) as those found in citrus fiber sources (e.g., citrus peel). Therefore, the present invention provides an improved citrus fiber product by striking a balance between having an increased water-soluble pectin content compared to citrus fiber sources while retaining the inherent properties (such as DE) of the citrus fiber sources. Thus, the modified citrus fiber product is a label-friendly citrus fiber product with improved gelling properties.

[0015] In another embodiment, the present invention provides a method for producing modified citrus fiber products, the method comprising:

[0016] • Combining citrus fiber sources with water to form an aqueous mixture; and

[0017] • Heating the aqueous mixture to a temperature of 60°C to 150°C; and

[0018] • Dry the aqueous mixture to obtain a modified citrus fiber product.

[0019] The modified citrus fibers have a gel strength of 30°SAG to 100°SAG and an esterification degree of 30% to 100%.

[0020] This invention avoids the use of harsh activation steps (such as acid treatment) to produce modified citrus fiber products from citrus fiber sources (e.g., citrus peel). The method of this invention uses only a thermomechanical activation step to release pectin trapped in the cellulose matrix, meaning a higher proportion of free water-soluble pectin is freely available and soluble in water. Therefore, the method of this invention produces citrus fiber products with improved gelling properties compared to citrus fiber products that do not utilize an activation step to convert trapped water-insoluble pectin into free soluble pectin. Consequently, the resulting modified citrus fiber product contains a certain amount of free water-soluble citrus fiber (e.g., pectin) with a gelling strength of 30°SAG to 100°SAG, which is higher than the gelling strength of citrus fiber products that do not utilize an activation step to convert trapped water-insoluble pectin into free soluble pectin. Because this method avoids the use of chemicals (e.g., acids) to convert entrapped water-insoluble pectin into free soluble pectin, the intrinsic properties of pectin (such as DE) in the resulting citrus fiber product are substantially the same (if not different) as those of pectin found in citrus fiber sources. Therefore, the present invention relates to an improved method for producing label-friendly citrus fiber products with improved gelling properties.

[0021] In a preferred aspect, the modified citrus fiber product contains pectin with a DE value between 30% and 90%, 30% and 85%, 30% and 80%, 30% and 70%, 30% and 60%, 30% and 50%, 30% and 40%, 40% and 100%, 50% and 100%, 60% and 100%, 70% and 100%, 80% and 100%, or any value within these ranges. In a particularly preferred aspect, the DE is 65% or higher. In an equally preferred aspect, the DE is 70% or higher.

[0022] In a preferred aspect, the modified citrus fiber product has a gel strength of 40°SAG to 90°SAG, 40°SAG to 80°SAG, 40°SAG to 70°SAG, 40°SAG to 60°SAG, or 40°SAG to 50°SAG. In a particularly preferred aspect, the modified citrus fiber product has a gel strength between 60°SAG and 90°SAG.

[0023] In a preferred aspect, the modified citrus fiber product contains 10% to 40% by weight of water-soluble pectin relative to the total weight of the modified citrus fiber product. In another preferred aspect, the modified citrus fiber product contains 20% by weight of water-soluble pectin relative to the total weight of the citrus fiber product. Even more preferably, the modified citrus fiber product contains between 30% and 40% by weight of water-soluble pectin relative to the total weight of the citrus fiber product. The freely available water-soluble pectin content of the modified citrus fiber product of the present invention is greater than that commonly found in natural citrus fiber. Therefore, the present invention will have improved gel strength compared to citrus fiber products produced by methods that do not utilize an activation step to convert entrapped water-insoluble pectin into free soluble pectin (such as simply grinding citrus peel after it has been placed in water and subsequently dried). Furthermore, unlike citrus fiber products obtained using harsh, acid-based activation steps, the modified citrus fiber products of this invention represent label-friendly products because the inherent properties of pectin in the modified citrus fiber products are substantially the same (if not different) as those found in citrus fiber sources.

[0024] In a preferred aspect of the invention, the mixture is heated to a temperature between 65°C and 105°C. Most preferably, the mixture is heated to 80°C. This temperature enhances the conversion of trapped water-insoluble pectin to free water-soluble pectin without requiring a harsh chemical-based (e.g., acid treatment) activation step to release the trapped water-insoluble pectin. As described in any aspect herein, heating includes heating via thermal conduction (e.g., using a double-jacketed system with hot water, steam, oil, or electricity), direct steam introduction (e.g., steam injection), mechanical shear / friction (e.g., extrusion), or a combination of two or more of these methods. In a preferred aspect of the invention, the mixture is heated via steam injection.

[0025] In a preferred aspect, the heating step of the above method is performed under shear. In a preferred aspect, the mixture is sheared at a speed between 0 and 20,000 rpm. Most preferably, the mixture is sheared at a speed between 80 and 250 rpm. In another preferred aspect, the shearing of the mixture is sustained for a period ranging from 1 minute to 7 hours, and most preferably for a period ranging from 3 hours to 5 hours. Shearing the mixture at any speed for any period of time further helps to convert the entrapped water-insoluble pectin into free water-soluble pectin, thereby increasing the amount of pectin in the modified citrus fiber product compared to the amount of pectin found in citrus fiber sources.

[0026] In a preferred aspect, the pectin included in the modified citrus fiber product has a degree of esterification (DE) within 10% of the degree of esterification of the citrus fiber source. In an even more preferred aspect, the pectin included in the modified citrus fiber product has a degree of esterification substantially the same as that of the citrus fiber source. In the context of the DE of the pectin included in the modified citrus fiber product of the present invention, the term "substantially the same" means that the degree of esterification of the pectin molecules is within ±0.1% to 5% of the DE of the pectin found in the citrus fiber source.

[0027] In a preferred aspect, no compounds are added and / or enriched prior to the step of heating the aqueous mixture to a temperature between 60°C and 150°C. Specifically, in the context of this invention, only water needs to be added to the citrus fiber source. No other substances are added to or removed from the mixture. The absence of added / enriched compounds ensures uninterrupted flow, as only the addition and subsequent evaporation of water are required to produce the modified citrus fiber product. The evaporated water produced by step c) of the method of this invention can then be condensed and recycled, and used in step (a) of the invention in further applications of the method. In an alternative embodiment, the heated mixture can be pressed to separate the solid and liquid components of the mixture. The liquid component of the mixture can then be recycled and used in step (a) of the method in further applications of the method. Therefore, the method of this invention has the advantage of minimizing water use while promoting product drying.

[0028] In a preferred aspect, the method does not include a chemical modification step, and in particular, it does not include acid hydrolysis. Specifically, chemicals (e.g., acids) are not used to convert entrapped water-insoluble pectin into free soluble pectin. The absence of chemical activation (e.g., acid hydrolysis) ensures that the water-soluble pectin obtained in the modified citrus fiber product has high quality, because the inherent properties of the pectin in the citrus fiber product are not impaired by acid-induced changes in the structure and function of the pectin. Therefore, advantageously, the method of the present invention results in high-quality, label-friendly modified citrus fiber products.

[0029] In a preferred aspect of the invention, the method further includes the step of pulverizing the modified citrus fiber product. Pulverization can be carried out by any suitable means known in the art, such as milling or grinding. This step reduces the particle size distribution to within limits acceptable to the end user. After pulverization, the modified citrus fiber product can be sorted or graded as needed, for example, by sieving.

[0030] In a preferred aspect, the water-to-fiber source ratio in step (a) of the method is from 95:5 (w / w) to 20:80 (w / w). Alternatively, the water-to-fiber source ratio in step (a) of the method is from 95:5 (w / w) to 60:40 (w / w), preferably from 80:20 (w / w) to 70:30 (w / w). In a particularly preferred aspect, the water-to-fiber source ratio in step (a) of the method is 50:50 (w / w). In a particularly preferred aspect, the water-to-fiber source ratio in step (a) of the method is 20:80 (w / w).

[0031] In another embodiment, a modified citrus fiber product obtained by the above method is provided. The modified citrus fiber product contains a higher concentration of free water-soluble pectin than that found in the citrus fiber source, and therefore exhibits superior gelling properties compared to citrus fiber products that do not utilize an activation step to release trapped water-insoluble pectin (e.g., products simply ground from the citrus fiber source). In particular, the modified citrus fiber product of the present invention has a gelling strength between 30°SAG and 100°SAG, while products that do not utilize an activation step to release trapped water-insoluble pectin have a gelling strength less than 30°SAG. Furthermore, since the activation step using chemicals (e.g., acids) is avoided, the inherent properties of the pectin in the modified citrus fiber product are substantially the same (if not different) as the inherent properties of the pectin found in the citrus fiber source. For example, the degree of esterification of the pectin found in the modified citrus fiber product of the present invention is within 5% to 10% of the degree of esterification of the pectin found in the citrus fiber source. Conversely, the degree of esterification of pectin in citrus fiber products obtained using chemical-based (e.g., acid-based) activation steps to release free soluble pectin is significantly lower than that found in citrus fiber sources. For example, the degree of esterification of such pectin is at least 5% lower than that found in citrus fiber sources, but more typically at least 10% lower.

[0032] In another embodiment, a composition is provided comprising a modified citrus fiber product and one or more additives or excipients, wherein the modified citrus fiber product has a gel strength of 30°SAG to 100°SAG and a degree of esterification of 30% to 100%.

[0033] In another embodiment, a consumer product is provided comprising a modified citrus fiber product or the above-described composition. In a preferred aspect, the consumer product is a food, beverage, or nutritional product. Incorporating the aforementioned modified citrus fiber product / composition ensures the production of a label-friendly consumer product because the inherent properties of the pectin contained in the modified citrus fiber product (such as the degree of esterification) are substantially the same (if not different) as the pectin found in citrus fiber sources.

[0034] In another embodiment, the use of the aforementioned modified citrus fiber products or compositions is contemplated. Preferably, the consumer products are food, beverage, or nutritional products. Using the modified citrus fiber products / compositions ensures the production of label-friendly consumer products because the inherent properties of the pectin contained in the modified citrus fiber products (such as the degree of esterification) are substantially the same (if not different) as the pectin found in citrus fiber sources. Attached Figure Description

[0035] To facilitate a clearer understanding of this disclosure, preferred embodiments will now be described by way of example only with reference to the accompanying drawings, in which:

[0036] Figure 1 This is a schematic diagram of a method that forms part of the present invention.

[0037] The accompanying drawings illustrate various embodiments of the system, method, and other aspects of this disclosure. Those skilled in the art will understand that the element boundaries (e.g., boxes, groups of boxes, or other shapes) shown in the figures represent one example of a boundary. In some examples, one element may be designed as multiple elements, or multiple elements may be designed as one element. In some examples, an element shown as an internal component of one element may be implemented as an external component of another element, and vice versa. Furthermore, elements may not be drawn to scale. A non-limiting and non-exhaustive description is provided with reference to the following drawings. Components in the drawings are not necessarily drawn to scale, but rather to illustrate principles.

[0038] The embodiments of this disclosure will be described more fully below with reference to the accompanying drawings, in which the same numerals represent the same elements and exemplary embodiments are illustrated. However, the embodiments of the claims may be embodied in many different forms and should not be construed as limited to the embodiments described herein. Detailed Implementation

[0039] The terms “comprising,” “having,” “containing,” and “including,” as well as their other forms, are intended to be equivalent in meaning and are open-ended, because one or more items following any of these terms do not imply an exhaustive list of such one or more items, or that they are limited to only the listed one or more items. It must also be noted that, unless the context explicitly indicates otherwise, the singular forms “a” and “the” as used herein and in the appended claims include plural references. Although any systems and methods similar to or equivalent to those described herein may be used in practicing or testing embodiments of this disclosure, preferred systems and methods are now described.

[0040] The following is a list of some terms used to describe the present invention:

[0041] Acid hydrolysis refers to a technique used to release water-soluble pectin. Acid hydrolysis disrupts the structure of the cellulose matrix containing trapped pectin, releasing free water-soluble pectin from the cellulose matrix. Acid hydrolysis also converts insoluble protopectin into water-soluble pectin and determines the total pectin content of citrus fiber sources (e.g., citrus peel). Therefore, acid hydrolysis is an effective method for increasing the amount of free pectin in solution. Acid hydrolysis also reduces the degree of esterification of pectin by at least 5% relative to the degree of esterification of pectin found in citrus fiber sources (e.g., citrus peel). Acid hydrolysis is an example of a harsh treatment used to release pectin from citrus fibers.

[0042] An “activation step” refers to any step in the production of citrus fiber products that attempts to convert trapped water-insoluble pectin into free water-soluble pectin. Examples of activation steps include incubating citrus fiber sources (e.g., citrus peel) in an acidic environment, which causes water-insoluble pectin to be converted into soluble pectin by altering the inherent properties of the pectin, such as reducing the degree of esterification of the pectin and disrupting the cellulose matrix of the trapped pectin.

[0043] "Chemical modification" refers to any modification to citrus fibers by adding chemicals during the production process. Examples include acid hydrolysis, contact with acids, contact with alkalis, etc. Chemical modification of citrus fibers is an example of harsh treatments used to release pectin from citrus fibers.

[0044] "Citrus fiber" broadly refers to the dietary fiber (including both insoluble and soluble fiber) contained in citrus fruits. Citrus fiber is the fiber contained in and obtained from fruits of the Citrus family (Citrus family), a large and diverse family of flowering plants. Citrus fruits are considered a special type of berry characterized by a leathery peel and a fleshy interior containing multiple sections filled with juice-filled sacs. Common varieties of citrus fruits include oranges, sweet oranges, Clementine, kumquats, tangerines, tangelos, satsumas, mandarins, grapefruits, citrons, pomelos, lemons, rough-skinned lemons, limes, and leech limes. Citrus fruits can be early-, mid-, or late-season. Citrus fruits also contain pectin, which is common in fruits but presents in particularly high concentrations in citrus fruits. Pectin is a gel-forming polysaccharide with a complex structure. It is essentially composed of methoxylated galacturonic acid, galacturonic acid, and rhamnose with side chains containing arabinose and galactose, linked by glycosidic bonds. The pectin content and degree of esterification of pectin in citrus fruits can vary seasonally, with ripe fruits containing less pectin than unripe fruits.

[0045] Citrus fiber is distinct from citrus pulp, which consists of intact juice sacs and is sometimes referred to as citrus vesicles, coarse pulp, floating matter, citrus cells, floating pulp, juice sacs, or pulp. Citrus fiber is also distinct from citrus pomace, which is the material containing the segment membranes and seeds of the citrus fruit. As used herein, "citrus peel" refers to the pectin and cellulose material contained in the outer part of the citrus fruit. It can be a waste product from the juice industry.

[0046] The citrus fiber in citrus fiber products is typically obtained from citrus fiber sources such as citrus peel, citrus pulp, citrus pomace, or combinations thereof. Furthermore, citrus fiber products may contain components of the primary cell walls of citrus fruits, such as cellulose, pectin, and hemicellulose, and may also contain proteins. Preferably, the citrus fiber source used to produce the modified citrus fiber products of the present invention does not undergo any substantial chemical modification; that is, the citrus fiber source is not subjected to any chemical modification process, such as esterification, derivatization, or enzymatic modification, or any combination thereof.

[0047] "Grinding" refers to the process of reducing the absolute particle size and particle size distribution of a substance. Exemplary machines that can be used to grind the modified citrus fiber products of the claimed invention include, but are not limited to, cutting mills, hammer mills, pin mills, jet mills, etc.

[0048] "Degree of esterification (DE)" refers to the amount of pectin esterified, expressed as a molar percentage. Pectin is rich in galacturonic acid. In nature, in citrus fruits, a large proportion of the carboxyl groups of galacturonic acid are esterified with methanol. The proportion of carboxyl groups esterified with methanol is related to the DE. DE decreases as pectin is extracted, especially if harsh activation techniques (such as acid hydrolysis) are used to convert water-insoluble pectin into free water-soluble pectin. Therefore, pectin extracted using acid-based techniques will tend to have a lower DE than natural pectin.

[0049] "Free pectin" refers to water-soluble pectin. Free pectin is the proportion of total pectin that is not retained in the cellulose matrix or is in an insoluble form (e.g., protopectin) and is therefore readily soluble in water at room temperature.

[0050] "Gel strength" refers to the ability of citrus fiber to gel under acidic and sugary conditions. The reference test is the SAG test (developed by the American Pectin Committee) to determine the grade strength of pectin under well-defined conditions of 65% sugar at pH 3 (Baker, GL (1959) "Pectin Standardization—Final Report of the IFT Committee," Food Technology, 13, 496-500), which is incorporated herein by reference. The quantity and mass (molar mass and DE) of water-soluble pectin determine the ability of citrus fiber products to gel under such conditions. Increased amounts of water-soluble pectin result in citrus fiber with high gel strength, while low levels of water-soluble pectin result in low gel strength. Gel strength is directly proportional to the amount of water-soluble pectin.

[0051] "Insoluble fiber" refers to the proportion of citrus fiber that is insoluble in water at room temperature. Typically, citrus fiber consists of about 60% insoluble fiber. Examples of insoluble fiber include cellulose and hemicellulose.

[0052] "Mixture" refers to any mixture or medium of ingredients. The term encompasses mixtures / mediums that are flowable or so viscous that they cannot flow easily, such as pastes. In the context of this invention, the water-to-fiber source ratio is in the range of 95:5 (w / w) to 20:80 (w / w), preferably in the range of 80:20 (w / w) to 70:30 (w / w). Particularly preferred aspects include a water-to-fiber source ratio in the range of 50:50. Particularly preferred aspects include a water-to-fiber source ratio in the range of 20:80.

[0053] "Natural citrus fiber" refers to citrus fiber found in citrus fiber sources (e.g., citrus peel, citrus pulp, citrus pomace, or a combination thereof). Natural citrus fiber has not been processed or exposed to methods associated with increasing the content of free water-soluble pectin.

[0054] "Nutritional supplement" refers to any substance that, as food or part of food, provides medical or health benefits (including the prevention and treatment of disease).

[0055] "Pectin" refers to the form of water-soluble fiber found in citrus fibers. Water-soluble pectin is expected to be soluble in water at room temperature. Pectin can be trapped within the cellulose matrix or exist in an insoluble form (protopectin). Acid hydrolysis disrupts the structure of the cellulose matrix to release free water-soluble pectin from it and also converts water-insoluble protopectin into water-soluble pectin. Therefore, acid hydrolysis is an effective activation step for increasing the amount of free pectin in solution.

[0056] The sugar-acid gel (SAG) test is used to determine the grade strength of pectin under specific conditions (65% sugar, pH 3.0). The obtained values ​​are expressed in °SAG.

[0057] "Shearing" generally refers to the mixing of components. All speeds and times are included in the term shearing. Non-limiting examples of equipment that can be used to generate the necessary shear are magnetic stirrers, mixers, agitators, stirrers, stretchers, and extruders. Other suitable means known in the art may also be used.

[0058] "Soluble fiber" refers to the portion of citrus fiber that is soluble in water at room temperature. Typically, citrus fiber consists of about 40% soluble fiber. An example of soluble fiber is pectin.

[0059] "Citrus fiber source" refers to any product from which citrus fiber can be obtained. Examples of citrus fiber sources include citrus peel, citrus pulp, citrus pomace, or combinations thereof. Citrus peel, citrus pulp, and citrus pomace can refer to the peel, pulp, or pomace of any citrus fruit, including but not limited to oranges, lemons, limes, Chinese mandarins, Clementi mandarins, grapefruits, etc.

[0060] "Retained pectin" refers to the proportion of total pectin that cannot freely dissolve in water. This pectin is typically retained within the cellulose matrix of citrus fiber sources and therefore cannot easily diffuse out and subsequently dissolve in water. Insoluble forms of pectin, such as protopectin, are also covered by this term.

[0061] The words “contains,” “has,” “includes,” and “include,” as well as their other forms, are intended to be equivalent in meaning and are open-ended, because one or more items following any of these words do not imply an exhaustive list of such one or more items, or that they are limited to only the one or more listed items.

[0062] Unless the context clearly indicates otherwise, the singular forms “an” and “the” as used herein, and similar indicators, include plural indicators in the context of describing an element (especially in the context of the appended claims). For example, reference to “substituent” covers a single substituent as well as two or more substituents, and so on. It should be understood that, unless otherwise indicated herein or clearly contradicted by the context, any term in the singular form may include its plural counterpart, and vice versa.

[0063] Furthermore, the phrase "consistently composed of..." will be understood to include those specifically listed elements and those additional elements that do not substantially affect the fundamental and novel characteristics of the invention. The phrase "consisting of..." does not include any unspecified elements.

[0064] Furthermore, in the context of describing features or aspects of this disclosure according to the Markush group, those skilled in the art will recognize that this disclosure is therefore also described according to any individual member or subgroup of the Markush group. Each of the narrower classes and subgenuses belonging to the general disclosure also constitutes part of this invention. This includes the general description of the invention, where a precondition or negative limitation is the removal of any subject matter from that genus, regardless of whether the removed material is specific.

[0065] Throughout this document, particularly in the provision of written descriptions, all values ​​expressed in range format should be interpreted flexibly to include not only the values ​​explicitly listed as limits of the range, but also all individual values ​​or subranges encompassed within that range, as if each value and subrange were explicitly listed. Any listed range can be readily identified as sufficiently descriptive and such that the same range can be decomposed into at least equal halves, thirds, quarters, fifths, tenths, etc. For example, the range “about 0.1% to about 5%” or “about 0.1% to 5%” should be interpreted to include not only about 0.1% to about 5%, but also the individual values ​​(e.g., 1%, 2%, 3%, and 4%) and subranges (e.g., 0.1% to 0.5%, 1.1% to 2.2%, 3.3% to 4.4%) within the indicated range. As those skilled in the art will understand, all language such as “at most,” “at least,” “greater than,” “less than,” etc., includes the listed numbers and refers to ranges that can subsequently be decomposed into subranges as discussed above. Finally, as those skilled in the art will understand, a range includes each individual member.

[0066] As used herein, the terms “for example,” “to illustrate,” “such as,” or “including” are intended to provide examples that further illustrate a more general subject. Unless otherwise stated, these examples are provided merely to aid in understanding the application of the descriptions in this disclosure and are not intended to be limiting in any way.

[0067] As used herein, “about” will be understood by one of ordinary skill in the art and will vary to some extent depending on the context in which it is used. If the use of the term is unclear to one of ordinary skill in the art, “about” will mean at most positive or negative 10% of that particular term, taking into account the context in which it is used.

[0068] Modified citrus fiber products

[0069] One aspect of the present invention relates to an improved modified citrus fiber product.

[0070] The modified citrus fiber product of the present invention has a fiber content and degree of esterification (DE) similar to those of citrus fibers contained within a citrus fiber source (i.e., within 10%). Due to the negative impact of chemicals / acids on the intrinsic factors and structural integrity of pectin, the DE of pectin contained in citrus fiber products that utilize chemical-based (e.g., acid-based) process steps to increase the amount of free water-soluble pectin is significantly lower than the DE of pectin found in citrus fiber sources. Furthermore, the modified citrus fiber product of the present invention has a higher free water-soluble pectin content than seen in citrus fiber products that do not utilize activation steps. Therefore, the modified citrus fiber product of the present invention represents a label-friendly citrus fiber product modified to increase the amount of free water-soluble available pectin.

[0071] Therefore, the modified citrus fiber product of the present invention represents an improvement over known citrus fiber products.

[0072] In some examples, the modified citrus fiber product contains 10% to 40% water-soluble pectin. Preferably, the modified citrus fiber product contains between 10% and 30%, 20% and 40%, or 30% and 40% water-soluble pectin. The amount of free water-soluble pectin contained in the modified citrus fiber product is greater than that present in citrus peel, but the inherent properties (such as the degree of esterification) of the free water-soluble pectin contained in the modified citrus fiber product are substantially the same (if not different) as those of pectin found in citrus peel. Surprisingly, the modified citrus fiber product exhibits improved properties (e.g., gel strength) compared to citrus fiber sources (e.g., citrus peel). For example, the modified citrus fiber product has a gel strength of 30 SAG to 100 SAG, preferably 45 SAG to 100 SAG, more preferably 45 SAG to 95 SAG, and even more preferably 50 SAG to 80 SAG. Therefore, the modified citrus fiber products of the present invention represent label-friendly citrus fiber products modified to increase the amount of freely available water-soluble pectin.

[0073] Method for producing modified citrus fiber products

[0074] One aspect of the present invention relates to an improved method for producing modified citrus fiber products.

[0075] The method includes: a) combining a citrus fiber source with water to form an aqueous mixture; and b) heating the aqueous mixture to a temperature between 60°C and 150°C; and c) drying the aqueous mixture to obtain a modified citrus fiber product. The resulting modified citrus fiber product has a gel strength of 30 SAG to 100 SAG and a degree of esterification of 30% to 100%.

[0076] The method of this invention avoids the use of harsh activation methods that require treatment with chemicals (such as acids) to convert trapped water-insoluble pectin into free water-soluble pectin. In contrast, this invention uses only water and energy (i.e., a thermomechanical activation step) to modify natural citrus fibers found in citrus fiber sources (e.g., citrus peels). The use of acids (or any other chemicals) is avoided. The conversion of trapped water-insoluble pectin into free water-soluble pectin using only water, heat, and energy (a thermomechanical activation step) without the need for chemical activation means that intrinsic properties of the pectin found in citrus fiber sources (such as the degree of esterification) are thus preserved in the modified citrus fiber product. The modified citrus fiber products of this invention represent improved, label-friendly citrus fiber products.

[0077] While activation methods using harsh, high-volume chemicals may result in higher amounts of water-soluble fiber (i.e., pectin), the inherent properties (i.e., degree of esterification) of these water-soluble fibers are significantly reduced compared to pectin found in citrus fiber sources because the chemicals used to increase pectin yield alter the structure of the cellulose matrix and natural pectin. Because the degree of esterification of pectin found in products utilizing acid-based activation methods is significantly lower than that found in citrus fiber sources, these citrus fiber products are not label-friendly.

[0078] In contrast, this invention avoids the use of harsh activation methods, meaning that the released pectin, though present in smaller amounts, has a degree of esterification substantially the same as that of pectin found in citrus peels. Due to the higher pectin levels, the gel strength of the modified citrus fiber product obtained by the method of this invention is between 30°SAG and 100°SAG, while citrus fiber products obtained using methods that do not employ an activation step to release entrenched water-insoluble pectin are below 30°SAG. The fact that the degree of esterification of the modified citrus fiber product of the claimed invention is substantially the same as that of pectin found in citrus peels indicates that this invention relates to label-friendly citrus fiber products. Therefore, this invention provides a method for producing modified citrus fiber products having strong gel strength as indicated by high SAG values. The fact that the degree of esterification of the pectin contained in the citrus fiber product is substantially the same (if not different) as that found in citrus fiber sources (e.g., citrus peels) proves that the citrus fiber product is label-friendly.

[0079] Therefore, the method of the present invention relates to an improved method for producing modified, label-friendly citrus fiber products, which ensures that the intrinsic properties of the water-soluble citrus fiber (pectin) present in the modified citrus fiber product remain substantially the same (if not different) as those found in the pectin of natural citrus peel, but increases the amount of freely available water-soluble pectin by means of a thermomechanical activation method step that converts truncated water-insoluble pectin into free water-soluble pectin.

[0080] In one example, the heating step is performed under shear. Shear can be provided using any device that allows the water and citrus fiber source to mix. Examples include magnetic stirring, extrusion, or the use of a mixer. Shear has the advantage of mixing the citrus fiber source with water, which increases the amount of soluble citrus fiber and enhances functionality. In a preferred example, shear occurs at speeds up to 20,000 rpm, most preferably between 80 rpm and 250 rpm. In another preferred example, heating is performed with or without shear for up to 7 hours, most preferably between 3 and 5 hours. In some aspects, shear is performed using extrusion for up to five minutes. In some aspects, shear is performed using extrusion for less than five minutes. This ensures sufficient time for the trapped water-insoluble pectin to convert into free water-soluble pectin that can diffuse into the water. Those skilled in the art will readily understand that the intensity of shear, the shear time, and the water-to-fiber source ratio are interrelated and the conditions should be adjusted accordingly. For example, if the mixture is mixed under high shear, a shorter shear time is required, and vice versa.

[0081] In a preferred example, the mixture is heated to a temperature between 60°C and 150°C. The temperature should not exceed 150°C, as this may lead to degradation of the citrus fiber source.

[0082] In a preferred example, the water-to-fiber source ratio is in the range of 95:5 (w / w) to 20:80 (w / w). In another preferred example, the water-to-fiber source ratio is in the range of 80:20 (w / w) to 70:30 (w / w). In an even more preferred example, the water-to-fiber source ratio is in the range of 50:50 (w / w). In an even more preferred example, the water-to-fiber source ratio is in the range of 20:80 (w / w). This has the advantage that there is sufficient water to dissolve the released soluble citrus fibers converted from the entrapped insoluble source within the citrus fiber source, while there is not too much water in the mixture that could negatively affect the drying step. Those skilled in the art will be able to adjust the amounts of water and citrus fiber source accordingly. Those skilled in the art will also be able to select the most suitable shearing method to account for the volume of water present in the mixture.

[0083] In a preferred example, the pectin contained in the modified citrus fiber product produced using the method of the claimed invention has a degree of esterification (DE) within 5% of the degree of esterification of the source or citrus fiber. In another preferred example, the DE of the pectin is substantially the same as the DE of the pectin found in the citrus fiber source. Because the claimed invention avoids harsh activation techniques (e.g., the use of acids), the pectin structure and associated cellulose matrix are preserved, meaning that the degree of esterification of the pectin found in the modified citrus fiber product of the present invention is almost identical to that found in the pectin found in citrus peel. When compared to natural citrus fiber found in the citrus fiber source, the proportion of carboxyl groups of galacturonic acid esterified with methanol in the pectin contained in the modified citrus fiber product remains largely unchanged because harsh chemicals are avoided in the activation step. While any acid technique is expected to reduce the denaturation efficiency (DE) of the resulting citrus fiber product (by at least 5%), the DE of pectin in the modified citrus fiber product obtained using the method of this invention will be significantly higher than the DE of pectin in citrus fiber products obtained using harsh acid-based conditions, as these conditions negatively affect pectin structure. Because only thermomechanical activation steps are used in the method of this invention, the DE of pectin in the citrus fiber product obtained using this method is comparable to the DE of pectin found in natural citrus fibers, unlike citrus fibers obtained using acid activation steps (such as prior art methods).

[0084] In a preferred embodiment, the method of the present invention does not include a chemical modification step. These chemical modifications may include, but are not limited to, treatment with acid, treatment with alkali, acid hydrolysis, and enzymatic treatment (e.g., pectinase). These chemical modifications may also include esterification, derivatization, or enzymatic modification, and combinations thereof. Chemical modification is intended to include cross-linking, acetylation, organic esterification, organic etherification, hydroxyalkylation (including hydroxypropylation and hydroxyethylation), phosphorylation, inorganic esterification, ionic (cationic, anionic, nonionic, and zwitterionic) modification, succinate modification, and substituted succinate modification. Oxidation and bleaching are also included.

[0085] In a preferred example, the modified citrus fiber product is pulverized before thermomechanical treatment and / or after drying. Pulverization can be performed using any suitable equipment. For example, the citrus fiber product can be ground using a grinder and then sieved to obtain the modified citrus fiber product in powder form. The modified citrus fiber product can then be packaged, stored, and transported for final use. Examples of suitable apparatus for pulverizing modified citrus fiber products include, but are not limited to, cutting mills, hammer mills, pin mills, jet mills, centrifugal mills, etc.

[0086] The citrus fiber obtained by the method of this invention represents an improved modified citrus fiber product. Because harsh activation techniques (such as the use of chemicals, such as acids) are avoided, the pectin contained in the modified citrus fiber product does not chemically degrade compared to pectin found in natural citrus fiber sources (i.e., pectin found in citrus peels), and therefore the modified citrus fiber product obtained by the claimed method represents a simple, label-friendly citrus fiber because the inherent properties of the pectin contained in the modified citrus fiber product (such as the degree of esterification) are substantially the same (if not different) as the degree of esterification of pectin found in citrus fiber sources.

[0087] The modified citrus fiber products of this invention can be packaged as compositions (additives containing excipients) or consumer products. Preferably, the consumer products are food, beverages, cosmetics, or nutritional products.

[0088] Uses of modified citrus fiber products

[0089] Another aspect of the invention relates to the use of modified citrus fiber products.

[0090] The intended uses of the isolated citrus fibers from this invention include applications in the food, consumer goods, and health industries. Specifically, the isolated citrus fibers will be used due to their thickening, water-absorbing, swelling, emulsifying, texturing, and gelling properties.

[0091] Example

[0092] The invention will now be defined with reference to the following non-limiting embodiments.

[0093] Example 1 - Method for preparing modified citrus fiber products

[0094] The following outlines eight methods for producing modified citrus fiber products according to the claimed invention.

[0095] Example using a Sigma blade mixer MRL 5 from RMC Guittard :

[0096] • Weigh 300g of dried citrus peel.

[0097] • Add 1200g of boiling permeate water.

[0098] • Mix manually and transfer to a mixing tank at 85°C.

[0099] • Mix at 80 rpm for 5 hours.

[0100] • After 5 hours, recycle the paste and grind it to obtain small pieces.

[0101] • Dry in a ventilated oven at 60°C for 16 hours.

[0102] • Grind and sieve the sample to 250 μm.

[0103] The resulting modified citrus fiber product has a gel strength of 70°SAG to 80°SAG.

[0104] Example using a lab cheese stretcher from Blentech :

[0105] • Weigh 400g of dried citrus peel

[0106] • Add 600g of boiling water for infiltration

[0107] • Manually mix and transfer to an 80°C stretching tank (double-jacketed adjustment).

[0108] • Mix at approximately 250 rpm for 3 to 5 hours.

[0109] • Recycle the paste and grind it to obtain small pieces.

[0110] • Dry in a ventilated oven at 60°C for 16 hours.

[0111] • Grind and sieve the sample to 250μm.

[0112] The resulting modified citrus fiber product has a gel strength of 80°SAG to 90°SAG.

[0113] Example using a laboratory cheese stretcher (steam injection) from Blentech :

[0114] • 750g of dried citrus peel

[0115] • Add 320g of boiling water for infiltration

[0116] • Mix manually and transfer to an 80°C stretching tank.

[0117] • Mix at approximately 50 rpm for 1 hour, injecting steam to maintain temperature and reduce dry matter.

[0118] • After 1 hour, increase to approximately 250 rpm and maintain for 2 to 4 hours, using a double jacket to maintain the temperature.

[0119] • Recycle the paste and grind it to obtain small pieces.

[0120] • Dry in a ventilated oven at 60°C for 16 hours.

[0121] • Grind and sieve the sample to 250μm.

[0122] The resulting modified citrus fiber products have a gel strength of 80°SAG to 95°SAG.

[0123] Example using a KS mixer from Karl Schnell :

[0124] • Add 10,000g of soft water to the mixing tank and heat it to 85°C.

[0125] • Add 5000g of dried citrus peel (coarse or ground).

[0126] • Mix at 120 to 140 rpm for 3 to 8 hours, using double-wall heating to maintain 80°C in the medium.

[0127] • Recycle the paste and grind it to obtain small pieces.

[0128] • Dry in a ventilated oven at 60°C for 16 hours.

[0129] • Grind and sieve the sample to 250μm.

[0130] The resulting modified citrus fiber product has a gel strength of approximately 70°SAG.

[0131] Example using a KS mixer (steam injection) from Karl Schnell :

[0132] • Add 2000g of cold, soft water to the mixing tank.

[0133] • Add 5000g of dried citrus peel (coarse or ground).

[0134] • Inject steam to heat it to 90°C while mixing at 25 rpm.

[0135] • When the DM content is 33% to 40%, mix at 120 to 140 rpm for 3 to 7 hours, using double-wall heating to maintain 80°C in the medium.

[0136] • Recycle the paste and grind it to obtain small pieces.

[0137] • Dry in a ventilated oven at 60°C for 16 hours.

[0138] • Grind and sieve the sample to 250μm.

[0139] The resulting modified citrus fiber product has a gel strength of 75°SAG to 85°SAG.

[0140] Example using a Thermomix mixer from Vorwerk :

[0141] • Weigh 75g of dried citrus peel

[0142] • Add 1425g of boiling permeate water

[0143] • Mix manually, then transfer to an 80°C mixer.

[0144] • Let stand for 30 minutes with gentle stirring.

[0145] • Stirring / grinding speed 10, for 3 minutes

[0146] • Recycle mixture

[0147] • Dry in a ventilated oven at 60°C for 16 hours.

[0148] • Grind and sieve the sample to 250μm.

[0149] The resulting modified citrus fiber products have a gel strength of 60°SAG to 80°SAG.

[0150] Example under static conditions (beaker) :

[0151] • Weigh 60g of dried citrus peel (coarse or ground) into a hot beaker.

[0152] • Add 240g of boiling water for infiltration

[0153] • Mix manually to homogenize (<1 minute), cover the beaker with a lid to prevent evaporation, and maintain at 80°C for 3 to 8 hours without stirring.

[0154] • Recycle wet fruit peels

[0155] • Dry in a ventilated oven at 60°C for 16 hours.

[0156] • Grind and sieve the sample to 250μm.

[0157] The resulting citrus fiber products have a gel strength of 50°SAG to 60°SAG.

[0158] Example using a Leistritz twin-screw extruder ZSE 12 HP-PH :

[0159] • Manage the continuous introduction of ground, dried citrus peel (zone 1) and permeation water (zone 2) to have an inlet DM between 50% and 80%.

[0160] • Heating in 8 zones, from 40°C (zone 1, peel inlet) to 150°C (nozzle head), 200 rpm to 400 rpm, total flow rate of 600 g / h, single-hole nozzle head of 1 mm to 2 mm.

[0161] • Recycle extruded products

[0162] • Dry in a ventilated oven at 60°C for 16 hours.

[0163] • Grind and sieve the sample to 250μm.

[0164] The resulting modified citrus fiber product has a gel strength of 70°SAG to 80°SAG.

[0165] Example 2 - Total pectin content, water-soluble pectin content, gel strength, and esterification of modified citrus fiber products Spend

[0166] The total pectin content (%), water-soluble pectin content (%), gel strength (°SAG), and degree of esterification (DE) of the modified citrus fiber product obtained by the method of the present invention were analyzed and compared with the total pectin content (%), water-soluble pectin content (%), gel strength (°SAG), and degree of esterification (DE) of citrus fiber products obtained by prior art methods. Specifically, the parameters were compared with citrus fiber products that do not employ an activation step to convert entrapped water-insoluble pectin into free soluble pectin (e.g., from ground peel) or use an acid-based activation step to do so.

[0167] Specifically, citrus fibers produced by the claimed method or prior art methods are obtained, and the pectin content, gel strength, and degree of esterification are evaluated using the following methods.

[0168] Water-soluble pectin. Extraction and recovery of pectin / soluble fiber under mild conditions. 75 g of fiber source was added to 2500 g of permeate water at room temperature with magnetic stirring. The medium was stirred at 450 rpm for 1 hour at room temperature. The medium was then centrifuged at 4500 rpm for 20 minutes at room temperature. The supernatant was then precipitated in isopropanol. The recovered solids were dried in a ventilated oven at 60 °C. The yield was defined as the sum of the amount of dry solids obtained from the supernatant and the assumed portion lost in the wet bottom, divided by the initial weight (75 g).

[0169] Total pectin content. Acid extraction of pectin. 100 g of fiber source was added to 4000 g of permeate water at 80 °C with mechanical stirring. The pH of the medium was adjusted to 1.6 using 30% HNO3. The medium was stirred at 80 °C for 4 hours. The medium was centrifuged at 4500 rpm for 20 minutes. The supernatant was adjusted to pH 3 using 10% Na2CO3 and then precipitated in IPA. The recovered solids were dried in a ventilated oven at 60 °C. The yield was defined as the amount of dry solids obtained from the supernatant divided by the initial weight (100 g).

[0170] Determination of cementitious strength (SAG)

[0171] This method comes from IFT Committee's method 5-54 on pectin standardization.

[0172] The device includes the following:

[0173] • Laboratory balance (accuracy 0.1g and 0.001g)

[0174] • Stainless steel pot, 15cm diameter

[0175] • Heating plate

[0176] • Hand whisk

[0177] • Beakers (1000ml and 150ml)

[0178] •scraper

[0179] Stopwatch

[0180] • Thermometer, 100℃

[0181] pH meter

[0182] •SAG glassware and tape

[0183] •Ridgelimeter

[0184] • Wire cheese slicer

[0185] • Refractometer

[0186] • Incubator

[0187] The chemicals used were sugar, tartaric acid (CAS 87-698-4) (488g, in 1L solution) and permeate.

[0188] The preparation of the gel is as follows:

[0189] Weigh [650 – (650 / x)] g of sugar into a 1000 mL beaker, where x = the assumed hardness of the sample.

[0190] • Add the sample to a dry 150 mL beaker. Sample weight (g) = [650 / x], where x = the assumed hardness of the sample.

[0191] • Add 20g of the weighed sugar to the sample.

[0192] • Mix the sample and sugar by stirring with a spatula.

[0193] • Divide the weighed sugar into two equal parts.

[0194] • Pour 410g of soaking water into a peeled stainless steel pot using a manual whisk.

[0195] • While manually stirring, pour the entire sample / sugar mixture into the water at once.

[0196] • Stir continuously for two minutes.

[0197] • After 2 minutes, place the pot on a hot plate and heat it while stirring manually continuously.

[0198] • When the medium reaches a complete rolling boil, add one part sugar. Stir continuously.

[0199] • When the medium begins to boil again, add the second portion of sugar. Stir continuously until the net weight of the jelly batch is 1015g. The hot plate should be set so that the entire heating time for the jelly is 5 to 8 minutes.

[0200] • After weighing 1015g of the batch on a laboratory balance, let it stand on the table for 1 minute.

[0201] • Quickly pour the batch into three previously prepared SAG glasses, each containing 2 mL of tartaric acid solution and equipped with adhesive tape, allowing filling to 26 pprox. Fill 1 cm above the rim.

[0202] • When the temperature reaches 30℃ to 35℃, place the glass in an incubator at 25℃±3℃ for 20 to 24 hours.

[0203] The properties of gel are measured as follows:

[0204] • After storing at 25℃±3℃ for 20 to 24 hours, remove the tape from the glass. Using a wire cheese slicer, cut off the top layer and discard it.

[0205] •Then carefully invert the jelly from the glass onto the inverted position on the square glass plate containing the Ridgelimer.

[0206] • Start the stopwatch once it's glued to the glass plate.

[0207] • Carefully place the plate and gel on the base of the Ridgelimeter, with the gel centered below the micrometer screw, and then screw the micrometer screw down to near the surface of the gel.

[0208] • Two minutes after the stopwatch is started, bring the tip of the micrometer screw into contact with the gel surface and record the Ridgelimeter reading, accurate to 0.1.

[0209] • Measure the pH, which must be between 2.2 and 2.4. Otherwise, the sample must be retested. If the pH is too high, increase the amount of tartaric acid solution; if the pH is too low, decrease the amount of tartaric acid solution.

[0210] The gelation grade of the sample is calculated as follows:

[0211] • Use a Ridgelimeter calibration table to convert the Ridgelimeter readings to a factor of F. The Ridgelimeter readings should be between 19.5 and 27; otherwise, the sample hardness must be retested under another assumption.

[0212] • Use a soluble solids correction table to convert the measured soluble solids to a factor C. The soluble solids content must be between 64.5 and 65.5; otherwise, the sample must be retested.

[0213] • When multiplying the assumed rank of the test by a correction factor, the true rank is obtained using the following formula:

[0214] Hypothetical rank x factor F x factor C = True rank / SAG

[0215] Factors F and C can be determined using the following table:

[0216]

[0217]

[0218] Determination of degree of esterification (DE) and galacturonic acidity

[0219] Degree of esterification (DE) and degree of galacturonic acid (GalA) were measured using a modified method described in TRS 669-JECFA 25 / 28 INS No. 440.

[0220] Sample preparation:

[0221] • In a beaker, add 100 mL of acidic alcohol (250 mL of 50% to 60% isopropanol + 5 mL of 37% fuming HCl) to 2.00 g of the ground sample (W1) and stir with a magnetic stirrer for 10 minutes.

[0222] • Filter and pass the mixture through a Buchner funnel.

[0223] • Rinse the beaker and pour 6 × 15 mL of acidic alcohol through the Buchner funnel.

[0224] • Wash the solid residue in the Buchner funnel at least 8 times with 50 mL of 50% to 60% isopropanol, and then wash twice with 50 mL of 87% isopropanol.

[0225] • Dry the sample at 105°C for approximately 2.5 hours. Weigh the dried sample (W2).

[0226] • Weigh 0.5g of sample (W3)

[0227] • Wet the sample with approximately 2 mL of 87% isopropanol.

[0228] • While stirring with a magnetic stirrer, add approximately 100 mL of boiling ultrapure water. Cover the medium with plastic wrap and allow it to cool to room temperature.

[0229] The sample was then evaluated by titration using a pH meter / automatic burette, as follows:

[0230] • Titrate the sample with 0.1N NaOH (record Viq1).

[0231] • Add 20.0 mL of 0.5 N NaOH while stirring, and cover with foil for exactly 15 minutes.

[0232] • Add 20.0 mL of 0.5 N HCl while stirring.

[0233] • Titrate the sample with 0.1N NaOH (record Viq2).

[0234] • To compensate for potential inaccuracies in balancing 20 mL of 0.5 N NaOH and HCl separately, a so-called “blind measurement” was performed (i.e., 100 mL of deionized water was treated in the same manner as the sample solution, including titration). The titration of this blank test was recorded as Vc.

[0235] Use the following calculations to determine DE and GalA:

[0236]

[0237]

[0238] The results are summarized in Table 1:

[0239] Table 1

[0240]

[0241] [1] Same initial citrus fiber source (batch 1); [2] Same initial citrus fiber source (batch 2). Standard deviation is reported when extraction is repeated 3 times.

[0242] As shown in Table 1, the citrus fiber product obtained using the method of the present invention (row 3) contains a higher amount of water-soluble pectin compared to other citrus fiber products produced by methods that do not involve an activation step (rows 1 and 2). The water-soluble pectin content of the citrus fiber product produced using a method involving acid-based activation (row 4) is greater than that of the claimed citrus fiber product because the acid-based method used to produce these citrus fibers releases water-insoluble pectin trapped in the cellulose matrix of the citrus peel. However, when compared to the citrus fiber product of the present invention, the degree of esterification of the water-soluble pectin contained in the citrus fiber product produced by the method employing an acid-based activation step is reduced by approximately 8%. Therefore, the pectin contained in these citrus fiber products has been substantially altered compared to the pectin contained in natural citrus peel. In contrast, the degree of esterification of pectin in the modified citrus fiber product of the present invention (row 3) is comparable to that seen in natural citrus peel, as indicated by a degree of esterification similar to that seen in milled citrus peel (rows 1 and 2 of the table above). Therefore, the method of the present invention produces a modified citrus fiber product with a higher pectin content compared to citrus fiber products produced without an activation step, while ensuring that the degree of esterification of pectin in the modified citrus fiber product is substantially the same (if not different) as the degree of esterification found in the citrus fiber source, because the internal pectin structure has not been damaged by acid treatment.

[0243] In summary, the modified citrus fiber products separated using the method of the present invention may not contain as much water-soluble pectin as other citrus fibers (such as those produced using methods involving an acid activation step), but the method produces products containing a greater amount of soluble pectin than products produced by methods that do not use an activation step at all. Crucially, the degree of esterification of the water-soluble pectin in the modified citrus fiber products of the present invention is closer to (if not identical to) the degree of esterification seen in the citrus fiber source than in products produced using acid-based activation steps, because the internal pectin structure has not been damaged by the gentle thermomechanical methods used to separate the pectin. Therefore, the modified citrus fiber products of the present invention represent label-friendly citrus fiber products (as evidenced by similar DE percentages of the modified citrus fiber products of the present invention and citrus fiber products produced using methods without an activation step), which are modified to increase the amount of free water-soluble available pectin (as evidenced by the increased percentage of water-soluble pectin in the modified citrus fiber products of the present invention and citrus fiber products produced using methods without an activation step).

[0244] Example 3 - Comparative Properties of Modified Citrus Fiber Products

[0245] Evaluation through Example 1 and Figure 1 The properties of the modified citrus fiber products obtained by the methods outlined in Table 2 are described and compared with known citrus fiber products obtained using methods that do not employ an activation step to convert truncated water-insoluble pectin into free water-soluble pectin, or use acid-based methods to do so, or have already extracted the pectin and the remaining citrus peel has subsequently been dried and milled. The results are summarized in Table 2.

[0246] The values ​​described in Table 2 represent a range of values; that is, the results do not indicate the values ​​recorded on a single sample. Therefore, the results represent a typical range that can be obtained for a particular type of product.

[0247] Table 2

[0248]

[0249] Commercial products

[0250] As shown in Table 2, the gelling capacity of the modified citrus fiber product (Sample 4) obtained by the method of the claimed invention is greater than that of citrus fiber (Sample 3) with similar pectin content or pectin-depleted citrus fiber (Sample 1) obtained not by the claimed invention. This increase in gelling capacity is due to the thermomechanical activation step used in the method of the invention, which promotes pectin availability by converting entrapped water-insoluble pectin into free water-soluble pectin. The pectin present in the modified citrus fiber product (Sample 4) of the present invention will have a similar degree of esterification to that of natural pectin (i.e., pectin present in the citrus fiber source (citrus peel)) because the structural integrity of natural pectin will be maintained due to the lack of acid treatment. As can be seen with respect to Sample 2, the pectin level increases due to large-scale acid treatment, which is due to the release of pectin from the cellulose matrix and insoluble stores (protopectin). The increased amount of pectin leads to an increase in gelling capacity. However, the structural integrity of the pectin in Sample 2 and the resulting degree of esterification will be significantly lower than that of Sample 4, as shown in Table 1.

[0251] Example 4 - The isolated citrus fibers exhibited improved gel strength.

[0252] The gel strength (°SAG) of the modified citrus fiber products produced according to the method of the present invention and the citrus fiber products prepared without using an activation step to convert the entrapped water-insoluble pectin into free soluble pectin was evaluated using the method outlined in Example 2.

[0253] Citrus fiber products are produced by subjecting citrus fiber sources (indicated in the first column of Table 3) to a method that converts trapped water-insoluble pectin into free water-soluble pectin without an activation step (column 2) or by employing the thermomechanical activation method steps of the present invention (column 3).

[0254] The results are shown in Table 3:

[0255] Table 3

[0256]

[0257] Repetition means starting from the same initial fiber source and applying the method of the present invention several times. Standard deviation is reported for three or more repetitions.

[0258] As shown in Table 3, exposing the citrus fiber sources indicated in the first column of Table 3 to the method of the present invention increases the gelling ability of the resulting citrus fiber products (column 3) compared to simply drying and grinding the citrus fiber source without exposing it to the activation step of the method of the present invention (column 2). This is because the method of the present invention increases the amount of freely available water-soluble pectin contained in the citrus fiber product while ensuring that the pectin retains the inherent properties of natural pectin found in the original citrus fiber source, such as the degree of esterification.

[0259] The invention may also broadly include any and all combinations of parts, elements, steps, examples, and / or features mentioned or indicated individually or collectively in the specification as two or more of the stated parts, elements, steps, examples, and / or features. Specifically, one or more features of any of the embodiments described herein may be combined with one or more features from any other embodiment described herein.

[0260] Protection may be sought for any feature disclosed in any one or more published documents cited herein in connection with this disclosure.

[0261] Although certain exemplary embodiments of the invention have been described, the scope of the appended claims is not intended to be limited to these embodiments. The claims should be interpreted literally, intentionally, and / or covering equivalents.

[0262] The words “comprising,” “having,” “containing,” and “including,” and their other forms, are intended to be equivalent in meaning and are open-ended, as one or more items following any of these words are not meant to be an exhaustive list of such items or to be limited to only the listed items. Additionally, the phrase “consistently composed of” will be understood to include those specifically listed elements and those additional elements that do not substantially affect the essential and novel characteristics of the invention. The phrase “consisting of” excludes any unspecified elements. It must also be noted that, unless the context explicitly indicates otherwise, the singular forms “a” and “the” as used herein and in the appended claims include plural references. Although any systems and methods similar to or equivalent to those described herein may be used in practicing or testing embodiments of this disclosure, preferred systems and methods are now described.

[0263] As used herein, the terms “for example,” “to illustrate,” “such as,” or “including” are intended to provide examples that further illustrate a more general subject. Unless otherwise stated, these examples are provided merely to aid in understanding the application of the descriptions in this disclosure and are not intended to be limiting in any way.

[0264] As used herein, “about” will be understood by one of ordinary skill in the art and will vary to some extent depending on the context in which it is used. If the use of the term is unclear to one of ordinary skill in the art, “about” will mean at most positive or negative 10% of that particular term, taking into account the context in which it is used.

[0265] Furthermore, it should be understood that the wording or terminology used herein, unless otherwise defined, is for descriptive purposes only and not for limitation. Any use of chapter headings is intended to aid reading the document and should not be construed as restrictive; information relating to chapter headings may appear within or outside that particular chapter. In the event of any inconsistency between the usage in this document and that of documents so incorporated by reference, the usage in the incorporated references shall be considered supplementary to the usage in this document; in the case of irreconcilable inconsistencies, the usage in this document shall prevail.

[0266] Representative characteristics

[0267] Representative features are set forth in the following clauses, which are independent or may be combined in any combination with one or more features disclosed in the text and / or drawings of this specification.

[0268] 1. A modified citrus fiber product, wherein the citrus fiber product has a gel strength of 30°SAG to 100°SAG and a degree of esterification of 30% to 100%.

[0269] 2. The citrus fiber product according to Clause 1, wherein the citrus fiber product contains 10% to 40% water-soluble pectin.

[0270] 3. The citrus fiber product according to Clause 2, wherein the citrus fiber product contains 20% to 30% water-soluble pectin.

[0271] 4. The modified citrus fiber product according to any one of the preceding clauses, wherein the gel strength is between 50°SAG and 80°SAG.

[0272] 5. The modified citrus fiber product according to Clause 4, wherein the gel strength is 70°SAG.

[0273] 6. The modified citrus fiber product according to any one of the preceding clauses, wherein the degree of esterification is between 50% and 80%.

[0274] 7. The modified citrus fiber product according to any one of the preceding clauses, wherein the degree of esterification is 70%.

[0275] 8. A method for producing modified citrus fiber products, the method comprising:

[0276] a) Combining citrus fiber sources with water to form an aqueous mixture; and

[0277] b) Heating the aqueous mixture to a temperature of 60°C to 150°C; and

[0278] c) Dry the aqueous mixture to obtain the modified citrus fiber product;

[0279] The modified citrus fiber product described herein has a gel strength of 30 SAG to 100 SAG and an esterification degree of 30% to 100%.

[0280] 9. The method according to Clause 8, wherein the heating comprises heating via thermal conduction, direct introduction of steam, mechanical shearing / friction, or a combination of two or more of these.

[0281] 10. The method according to clause 8 or 9, wherein step (b) is performed under cutting.

[0282] 11. The method according to any one of clauses 8 to 10, wherein the modified citrus fiber product has an esterification degree within + / -10% of the esterification degree of the citrus fiber source.

[0283] 12. The method according to any one of clauses 8 to 11, wherein the modified citrus fiber product has a degree of esterification substantially the same as that of the citrus fiber source.

[0284] 13. The method according to any one of clauses 8 to 12, wherein the citrus fiber product contains between 10% and 40% water-soluble pectin.

[0285] 14. The method according to Clause 13, wherein the citrus fiber product comprises 20% to 30% water-soluble pectin.

[0286] 15. The method according to any one of clauses 8 to 14, wherein the gel strength of the citrus fiber product is between 50°SAG and 80°SAG.

[0287] 16. The method according to Clause 15, wherein the gel strength of the citrus fiber product is 70°SAG.

[0288] 17. The method according to any one of clauses 8 to 16, wherein the degree of esterification of the citrus fiber product is between 50% and 80%.

[0289] 18. The method according to Clause 17, wherein the degree of esterification of the citrus fiber product is 70%.

[0290] 19. The method according to any one of clauses 8 to 18, wherein no compound is added and / or enriched prior to step (b).

[0291] 20. The method according to any one of clauses 8 to 19, wherein no compound is extracted and / or depleted prior to step (b).

[0292] 21. The method according to any one of Clauses 8 to 20, wherein the method does not include a chemical modification or chemical activation step.

[0293] 22. The method according to Clause 21, wherein the chemical modification or activation step is alkaline hydrolysis or acid hydrolysis.

[0294] 23. The method according to any one of clauses 8 to 22, the method further comprising the step of pulverizing the modified citrus fiber product before step a) and / or after step c).

[0295] 24. The method according to any one of clauses 8 to 23, wherein the ratio of water to fiber source in step (a) is from 95:5 (w / w) to 20:80 (w / w).

[0296] 25. The method according to Clause 24, wherein the ratio of water to fiber source in step a) is 50:50 (w / w), preferably wherein the ratio of water to fiber source in step a) is 20:80 (w / w).

[0297] 26. A modified citrus fiber product, said modified citrus fiber product being obtainable by any one of the methods according to clauses 8 to 25.

[0298] 27. A composition comprising a modified citrus fiber product and one or more additives or excipients, wherein the modified citrus fiber product has a gel strength of 30 SAG to 100 SAG and a degree of esterification of 30% to 100%.

[0299] 28. A consumer product comprising a modified citrus fiber product according to any one of clauses 1 to 7 or 26, or a composition according to clause 27.

[0300] 29. The consumer products described in Clause 28, wherein the consumer products are food, beverages, cosmetics or nutritional products.

[0301] 30. Use in a consumer product of a modified citrus fiber product according to any one of Clauses 1 to 7 or 26, or of a composition according to Clause 27.

[0302] 31. The use described in Clause 30, wherein the consumer product is food, beverage, cosmetic or nutritional product.

[0303] 32. Modified citrus fiber products according to clauses 1 to 7 or 26, compositions according to clause 27, or consumer products according to the clauses, used in medicine.

[0304] 33. Modified citrus fiber products according to Clauses 1 to 7 or 26, compositions according to Clause 27, or consumer products according to Clause 28, for the purpose of lowering blood cholesterol, reducing weight, stabilizing blood sugar, and / or diabetes.

[0305] 34. The method according to any one of clauses 8 to 25, wherein step (b) of the method is performed under shear at a speed of up to 20,000 rpm, preferably between 80 rpm and 250 rpm.

[0306] 35. The method according to any one of clauses 8 to 25 or 34, wherein the aqueous mixture is heated to 80 degrees Celsius.

[0307] 36. The method according to any one of clauses 8 to 25, 34 or 35, wherein the aqueous mixture is heated for a period of time between 1 minute and 7 hours, preferably between 3 hours and 5 hours, and even more preferably 4 hours.

[0308] 37. The method according to any one of clauses 8 to 25 or 34 to 36, wherein the ratio of water to fiber source in step (a) is from 95:5 (w / w) to 20:80 (w / w).

[0309] 38. The method according to Clause 37, wherein the ratio of water to fiber source in step (a) is from 80:20 (w / w) to 70:30 (w / w).

[0310] 39. The method according to Clause 38, wherein the ratio of water to fiber source in step (a) is 50:50 (w / w).

Claims

1. A modified citrus fiber product, wherein the citrus fiber product has a gel strength of 30°SAG to 100°SAG and a degree of esterification of 30% to 100%.

2. The modified citrus fiber product according to claim 1, wherein the modified citrus fiber product comprises 10% to 40% water-soluble pectin.

3. A method for producing modified citrus fiber products, the method comprising: a) Combining citrus fiber sources with water to form an aqueous mixture; as well as b) Heat the aqueous mixture to a temperature of 60°C to 150°C; as well as c) Dry the aqueous mixture to obtain the modified citrus fiber product; The modified citrus fiber product described herein has a gel strength of 30°SAG to 100°SAG and a degree of esterification of 30% to 100%.

4. The method of claim 3, wherein step (b) is performed under shearing.

5. The method according to claim 3 or 4, wherein the modified citrus fiber product has an esterification degree within + / - 10% of the esterification degree of the citrus fiber source.

6. The method according to any one of claims 3 to 5, wherein the modified citrus fiber product has a degree of esterification substantially the same as that of the citrus fiber source.

7. The method according to any one of claims 3 to 6, wherein no compound is added and / or enriched prior to step (b).

8. The method according to any one of claims 3 to 7, wherein no compound is extracted and / or depleted prior to step (b).

9. The method according to any one of claims 3 to 8, wherein the method does not include a chemical modification step.

10. The method according to any one of claims 3 to 9, the method further comprising the step of pulverizing the modified citrus fibers.

11. The method according to any one of claims 3 to 10, wherein the ratio of water to fiber source in step (a) is from 95:5 (w / w) to 20:80 (w / w).

12. A modified citrus fiber product, said modified citrus fiber product being obtainable by the method according to any one of claims 3 to 11.

13. A composition comprising a modified citrus fiber product and one or more additives or excipients, wherein the modified citrus fiber product has a gel strength of 30 SAG to 100 SAG and a degree of esterification of 30% to 100%.

14. A consumer product comprising a modified citrus fiber product according to any one of claims 1, 2 or 12, or a composition according to claim 13.

15. Use in a consumer product of the modified citrus fiber product according to any one of claims 1, 2 or 12, or of the composition according to claim 13.

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