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 to 100 SAG and a degree of esterification of from 30 to 100%. The present invention further relates to processes of producing said modified citrus fiber product. The present invention avoids using activation steps involving the use of chemicals (e.g., acid) to convert trapped, water-insoluble pectin into free, water-soluble pectin whilst still obtaining suitable amounts of free, water-soluble pectin to produce a citrus fiber product having a gelling strength (SAG) of between 30 and 100 SAG. The avoidance of such activation steps ensures that the intrinsic factors of the pectin contained in the modified citrus fiber product are equivalent to that of pectin found in the native source of citrus fibers.

Description

MODIFIED CITRUS FIBER PRODUCTCROSS REFERENCE TO RELAED APPLICATIONS

[0001] This application claims the benefit of European Application No. 23201623.8, filed October 4, 2023, the disclosure of which is incorporated by reference herein in its entirety.FIELD OF THE INVENTION

[0001] The present invention relates to a modified citrus fiber product, a process for producing a modified citrus fiber product, compositions and consumables comprising a modified citrus fiber product and uses of said modified citrus fiber product. In particular, the present invention relates to modified citrus fiber products, and methods for producing said modified citrus fibers products, whereby the modified citrus fiber products have a gelling strength (° SAG) that is greater than that of native citrus fibers found in the source of citrus fibers (e.g. citrus peel) and a degree of esterification that is essentially the same as that of native citrus fibers found in the source of citrus fibers.BACKGROUND OF THE INVENTION

[0002] Citrus fibers are a type of dietary fiber derived from citrus fruit, in particular from citrus peel. Citrus fibers, in various forms, are widely used, for example, in the food and consumer product industry for their viscosifying, water absorbing, bulking, emulsifying and texturizing properties.

[0003] Citrus fibers are mainly composed of water soluble and water insoluble fibers. Water insoluble fibers include cellulose and hemicellulose, and 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 pectin’s degree of esterification also positively contribute to the gelation of the solution. Thus, while important, the quantity of pectin is not the only factor that determines the gelling ability of a pectin-containing solution. Thus, a pectin-containing product needs to balance the amount of pectin obtained from a pectin source with the need for maintainingthe intrinsic properties of the pectin, such as degree of esterification, to ensure that said pectin- containing product has optimum gelling properties.

[0004] Native citrus fibers typically contain around 20-40% of pectin with the remaining contents being formed of insoluble citrus fibers (cellulose and hemicellulose) and other components. However, the majority of pectin found in citrus peel is trapped / intermingled with the other insoluble components (such as celluloses and hemicelluloses) of the cell wall of the citrus peel. This “trapped pectin” cannot escape the confines of the cellulose matrix of the cell wall and diffuse and dissolve in water. A small proportion of the total pectin content of the citrus peel is freely available (“free pectin”), i.e., not trapped / intermingled with other insoluble fibers, and so is ready soluble in water. The amount of free / soluble pectin and the intrinsic properties of this pectin, such as the degree of esterification, determines the gelling strength (° SAG) of a pectin-containing product and so efforts have been made to produce citrus fiber products with a high free / soluble pectin content while also maintaining the intrinsic properties, such as the degree of esterification of the free / soluble pectin.

[0005] To try to liberate trapped pectin, some citrus fiber products have been produced by placing citrus peel or pulp in water followed by subsequent drying and grinding of the citrus peel. Since no “activation” steps occur to convert “trapped pectin” into “free pectin”, the resulting ground citrus fibers have a water-soluble pectin content that is similar to that of native citrus peel. The majority of the pectin remains trapped in the cellulose / hemicellulose matrix meaning that citrus fiber products obtained by this method have a low free, water-soluble pectin content. As a result, the gelling strength of citrus fiber products obtained by this method is low.

[0006] Attempts have also been made to extract pectin from citrus peel, i.e., removing the pectin from the source of the citrus fibers. This involves using acid extraction methods, such as acid hydrolysis, to extract the majority of pectin from the citrus peel. The extracted pectin will be water soluble since it has been extracted from the environment of the citrus peel that traps the pectin and prevents solubility. The resulting citrus fiber product (i.e., the components of the citrus peel remaining post pectin extraction) is potentially processed, dried and ground. However, little to no water-soluble pectin is present in this citrus fiber product due to depletion of the pectin contained within the citrus peel prior to processing. As a result, even if the viscosity coming from theinsoluble fiber part can be boosted via process, the gelling ability of citrus fiber products obtained by this method is also low.

[0007] Further attempts to increase the amount of “free pectin” in the context of a citrus fiber product involve activation steps to liberate pectin trapped in the cellulose / hemicellulose matrix and to recover both free pectin and cellulose / hemicellulose together. Such activation steps include immersing citrus peels in an acidic environment with or without further chemicals, such as a solvent. The acid-treatment partially degrades the cellulose / hemicellulose and pectin in the cell wall of the citrus peel resulting in conversion of trapped, water-insoluble pectin to free, water- soluble pectin within the citrus peel. The activated citrus peel is subsequently dried and ground to produce the citrus fiber product. While this acid-activation may increase the amount of “free pectin” in the eventual citrus fiber product, the intrinsic properties, in particular the degree of esterification, of the free, soluble pectin is impacted by the effects of acid on the pectin structure. Thus, while acid-activation of citrus peels may increase the amount of “free pectin” in the eventual citrus fiber product, the internal properties (i.e., the degree of esterification) of this “free pectin” are compromised such that the gelling properties of the pectin are less than that of native free pectin. Moreover, the citrus fiber product cannot be deemed a “label-friendly” product since the intrinsic properties, such as the degree of esterification, of the pectin contained in the citrus fiber product have been altered to such a degree that they no longer resemble native pectin from the citrus peel but more like pectin extracted via traditional acidic extraction.

[0008] WO 2018 / 149893 Al discloses treating a pectin-containing biomass with an activating solution containing alcohol and an acid to convert trapped, water-insoluble pectin into free, soluble pectin. Due to the acidic treatment of native citrus peels, the resulting citrus fibers have a higher amount of freely available, water-soluble pectin. However, a problem with this method is that the intrinsic properties of the liberated pectin, such as the degree of esterification, are reduced when compared to the native pectin from the citrus peel. Therefore, the resulting citrus fiber product is not “label-friendly”.

[0009] US 5,567,462 discloses a method of obtaining a citrus fiber product that combines citrus peel with an acid or alkaline aqueous solution under conditions to at least partially solubilize pectin present in the peel. An alcohol is then used to precipitate the pectin and the resulting fibers are then dried. While this treatment may yield a larger amount of freely available, water-soluble fibers,again, due to the acidic treatment of native citrus peels, the intrinsic properties of the liberated pectin, such as the degree of esterification, are reduced when compared to the native pectin from the citrus peel. Therefore, the resulting citrus fiber product is not “label-friendly”.

[0010] WO 91 / 15517 Al discloses a method of obtaining citrus fibers by combining citrus peel with an acid thereby liberating the trapped, water-insoluble pectin. The resulting solution was then left to dry in a drying cupboard to obtain the dried citrus fibers. Again, due to the acidic treatment of native citrus peels a larger amount of freely available, water-soluble pectin was liberated, but the intrinsic properties of the liberated pectin, such as the degree of esterification, are reduced when compared to the native pectin from the citrus peel. Therefore, the resulting citrus fiber product is not “label-friendly”.

[0011] There is thus a need to provide a citrus fiber product that has a higher amount of free, soluble pectin compared to that found in native citrus peel whilst also maintaining the intrinsic properties, such as the degree of esterification, of the pectin so that they resemble that found in native citrus peel. Due to the higher amount of soluble pectin and retained degree of esterification, any such citrus fiber product will have improved gelling properties compared to citrus fiber products produced by merely grinding citrus peels. Retaining the intrinsic properties typical of those found in citrus peel, such as the degree of esterification, also ensures that the citrus fiber product is “label-friendly” unlike citrus fiber products that use acid-based activation steps. There is also a need to provide a process of obtaining said citrus fiber products from a source of citrus fibers. The present invention provides such an improved citrus fiber product and method for producing the same and thus addresses the problems associated with the prior art.SUMMARY OF THE INVENTION

[0012] In one embodiment, the present invention provides a modified citrus fiber product, wherein the citrus fiber has a gel strength of from 30 to 100 ° SAG and a degree of esterification (DE) of from 30 to 100%. The amount of freely available, water-soluble citrus fibers (pectin) in the modified citrus fiber product is increased compared to that seen in the source of citrus fibers meaning that the modified citrus fiber of the present invention has improved gelling properties. Additionally, the DE of modified citrus fiber is comparable to the DE of native citrus fibers found in the source of citrus fibers so the intrinsic properties of the pectin contained in the modifiedcitrus fiber product are substantially the same, if not identical, to the pectin found in the source of citrus fiber (e.g., citrus peel). The present invention thus provides an improved citrus fiber product by striking a balance between having an increased water-soluble pectin content compared to the source of citrus fibers but retaining the intrinsic properties, such as the DE, of the source of citrus fibers. The modified citrus fiber product is thus a lab el -friendly citrus fiber product with improved gelling properties.

[0013] In another embodiment, the present invention provides a process for producing modified a citrus fiber product comprising:• combining a source of citrus fibers with water to form an aqueous mixture; and• heating the aqueous mixture to a temperature from 60 to 150 degrees Celsius; and• drying the aqueous mixture to obtain the modified citrus fiber product. wherein the modified citrus fiber has a gel strength of from 30 to 100 ° SAG and a degree of esterification of from 30 to 100%.

[0014] The present invention avoids the use of harsh activation steps (such as acid treatment) to produce a modified citrus fiber product from a source of citrus fibers, e.g., citrus peel. The process of the invention liberates pectin trapped in the cellulose matrix using only thermomechanical activation method steps meaning that a higher proportion of free, water-soluble pectin is freely available and can dissolve in water. The process of the invention thus produces a citrus fiber product that has improved gelling properties over citrus fiber products that do not utilise an activation step to convert trapped, water-insoluble pectin into free, soluble pectin. Therefore, the obtained modified citrus fiber product contains an amount of free, water-soluble citrus fibers (e.g., pectin) that has a gelling strength of from 30-100 ° SAG, which is above that of citrus fiber products that do not utilise an activation step to convert trapped, water-insoluble pectin into free, soluble pectin. As the method avoids using chemicals (e.g., acid) to convert trapped, waterinsoluble pectin into free, soluble pectin, the intrinsic factors (such as the DE) of the pectin in the obtained citrus fiber product are substantially the same, if not identical, to that of the pectin found in the source of citrus fibers. The present invention thus relates to an improved method for producing a label-friendly citrus fiber product with improved gelling properties.

[0015] In a preferred aspect, the pectin contained in the modified citrus fiber product has a DE of between 30-90%, 30-85%, 30-80%, 30-70%, 30-60%, 30-50%, 30-40% 40-100%, 50-100%, 60-100%, 70-100%, 80-100% or any value in between any of these ranges. In a particularly preferred aspect, the DE is 65% or more. In an equally preferred aspect, the DE is 70% or more.

[0016] In a preferred aspect, the modified citrus fiber product has a gel strength of 40 to 90 ° SAG, 40 to 80 ° SAG, 40 to 70 ° SAG, 40 to 60 ° SAG or 40 to 50 ° SAG. In a particularly preferred aspect, the gel strength of the modified citrus fiber product is between 60 and 90 ° SAG.

[0017] In a preferred aspect, the modified citrus fiber product comprises from 10 to 40% by weight of water-soluble pectin relative to the total weight of the modified citrus fiber product. In a 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 comprises between 30 and 40% by weight 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 typically found in native citrus fiber. Thus, the present invention will have an improved gelling strength compared to citrus fiber products produced by methods that do not utilise an activation step to convert trapped, waterinsoluble pectin into free, soluble pectin, such as methods that simple grind citrus peel after being placed in water and subsequently dried. Additionally, unlike citrus fiber products obtained using harsh, acid-based activation steps, the modified citrus fiber product of the invention represents a lab el -friendly product since the intrinsic properties of the pectin in the modified citrus fiber product are substantially the same, if not identical, to those found in the source of citrus fibers.

[0018] In a preferred aspect of the invention, the mixture is heated to a temperature between 65°C to 105°C. Most preferably the mixture is heated to 80°C. The mixture temperature improves conversion of trapped, water-insoluble pectin into free, water-soluble pectin without the need for harsh, chemical-based (e.g., acid treatment) activation steps to liberate trapped, water-insoluble pectin.

[0001] As described herein in any aspect, heating comprises heating via thermal conduction (double-jacket using hot water, steam, oil or electricity for instance), direct introduction of steam (e.g., steam injection), mechanical shearing / friction (e.g. extrusion) or combinations of two or more thereof. In a preferred aspect of the invention, the mixture is heated via steam injection.

[0019] In a preferred aspect, the heating step of the above process is carried out under shear. In a preferred aspect, the mixture is sheared at a speed of between 0 to 20,000 rpm. Most preferably, the mixture is sheared at a speed of between 80-250 rpm. In an alternatively preferred aspect, the mixture is sheared for a period of time ranging from 1 minute to 7 hours, most preferably for a period of time ranging from 3-5 hours. Shearing the mixture at any speed for any period of time further helps to convert trapped, water-insoluble pectin to free, water-soluble pectin to increase the amount of pectin in the modified citrus fiber product compared to that found in the source of citrus fibers.

[0020] In a preferred aspect, the pectin contained in the modified citrus fiber product has a degree of esterification (DE) that is within 10% of the degree of esterification of the source of citrus fiber. In an even more preferred aspect, the pectin contained in the modified citrus fiber product has a degree of esterification which is substantially identical to the degree of esterification of the source of citrus fiber. In the context of the DE of pectin contained in the modified citrus fiber product of the present invention, the term “substantially identical” refers to pectin molecules that have a degree of esterification that is within plus or minus 0.1-5% of the DE of the pectin found in the source of citrus fibers.

[0021] 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 to 150 degrees Celsius. In particular, only the addition of water to the source of citrus fibers is required in the context of the invention. Nothing else is added or removed to the mixture. Not adding / enriching compounds to the mixture ensures that there are no disruptions to the flow as only the addition and subsequent evaporation of water is required to produce the modified citrus fiber product. The evaporated water resulting from step c) of the process of the invention can be subsequently condensed and recycled and used in step (a) of the invention in a further application of the process. In alternative embodiment, the heated mixture can be pressed such that the solid and liquid components of the mixture are separated. The liquid components of the mixture can then be recycled and used in step (a) of the process in a further application of the process. Thus, an advantage of the present process is that water use is minimized whilst facilitating drying of the product.

[0022] In a preferred aspect, the process does not comprise a chemical modification step, particularly the process does not comprise acid hydrolysis. In particular, chemicals (e.g., acid) arenot used to convert trapped, water-insoluble pectin into free, soluble pectin. The lack of chemical activation, e.g., acid hydrolysis, ensures that the resulting water-soluble pectin in the modified citrus fiber product is of high quality because the intrinsic properties of the pectin in the citrus fiber product is not compromised due to acid-induced changes in the structure and function of the pectin. Therefore, advantageously, the present process results in the production of a high quality, lab el -friendly modified citrus fiber product.

[0023] In a preferred aspect of the invention, the process further comprises a step of comminuting the modified citrus fiber product. Comminution may be performed by any suitable means known in the art, for example by milling or grinding. This step reduces the particle size distribution to within acceptable limits for the end user. Following comminution, the modified citrus fiber product may be classified or fractionated as required, for example by sieving.

[0024] In a preferred aspect, the ratio water to source of fibers in step (a) of the process is from 95:5 to 20:80 (w / w). Alternatively, the ratio water to source of fibers in step (a) of the process is from 95:5 to 60:40 (w / w), preferably from 80:20 to 70:30 (w / w). In a particularly preferred aspect, the ratio water to source of fibers in step (a) of the process is 50:50 (w / w). In a particularly preferred aspect, the ratio water to source of fibers in step (a) of the process is 20:80 (w / w).

[0025] In another embodiment, a modified citrus fiber product obtained by the above process is provided. The concentration of free, water-soluble pectin contained in the modified citrus fiber product is greater than that found in the source of citrus fibers and so the modified citrus fiber product has superior gelling properties compared to citrus fiber products that do not utilise an activation step to liberate trapped, water-insoluble pectin (e.g., products that simply grind the source of citrus fibers). In particular, the modified citrus fiber product of the present invention has a gelling strength of between 30 to 100 ° SAG whereas products that do not utilise an activation step to liberate trapped, water-insoluble pectin have a gelling strength of less than 30 ° SAG. Moreover, as activation steps using chemicals (e.g., acid) are avoided, the intrinsic properties of the pectin in the modified citrus fiber product are substantially the same, if not identical, to that of pectin found in the source of citrus fibers. For example, the degree of esterification of the pectin found in the modified citrus fiber product of the invention is within 5-10% of the degree of esterification of the pectin found in the source of citrus fibers. Conversely, the degree of esterification of the pectin in citrus fiber products obtained using chemical-based (e.g., acid-based)activation steps to liberate free, soluble pectin is significantly reduced compared to the degree of esterification of the pectin found in the source of citrus fibers. For example, the degree of esterification of such pectin is at least 5% less, but more commonly at least 10% less than that found in the source of citrus fibers.

[0026] In another embodiment, 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 from 30 to 100 ° SAG and a degree of esterification of from 30 to 100% is provided.

[0027] In another embodiment, a consumable comprising the modified citrus fiber product, or the composition mentioned above is provided. In a preferred aspect, the consumable is a food product, a beverage or nutraceutical product. Incorporating the earlier-mentioned modified citrus fiber product / composition ensures that a lab el -friendly consumable can be produced since the intrinsic properties, such as the degree of esterification, of the pectin contained in the modified citrus fiber product is substantially the same, if not identical, to the pectin found in the source of citrus fibers.

[0028] In another embodiment, use of the modified citrus fiber product or composition mentioned earlier are envisaged. Preferably, the consumable is a food product, a beverage or nutraceutical product. Using said modified citrus fiber product / composition ensures that a lab el -friendly consumable can be produced since the intrinsic properties, such as the degree of esterification, of the pectin contained in the modified citrus fiber product is substantially the same, if not identical, to the pectin found in the source of citrus fibers.BRIEF DESCRIPTION OF THE FIGURES

[0029] In order that the present disclosure may be more readily understood, preferable embodiments thereof will now be described, by way of example only, with reference to the accompanying drawings, in which:FIGURE l is a schematic of a process forming part of the present invention.

[0030] The accompanying drawings illustrate various embodiments of systems, methods, and embodiments of various other aspects of the disclosure. Any person with ordinary skills in the art will appreciate that the illustrated element boundaries (e.g., boxes, groups of boxes, or othershapes) in the figures represent one example of the boundaries. It may be that in some examples one element may be designed as multiple elements or that 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 in another and vice versa. Furthermore, elements may not be drawn to scale. Non-limiting and non-exhaustive descriptions are described with reference to the following drawings. The components in the figures are not necessarily to scale, emphasis instead being placed upon illustrating principles.

[0031] Embodiments of the present disclosure will be described more fully hereinafter with reference to the accompanying drawings in which like numerals represent like elements throughout the several figures, and in which example embodiments are shown. Embodiments of the claims may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.DETAILED DESCRIPTION

[0032] 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. It must also be noted that as used herein and in the appended claims, the singular for “a,” “an,” and “the” include plural references unless the context clearly dictates otherwise. Although any systems and methods similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present disclosure, the preferred systems and methods are now described.

[0033] Some of the terms used to describe the present invention are set out below:

[0034] “Acid hydrolysis” refers to a technique used to liberate water-soluble pectin. Acid hydrolysis breaks down the cellulose matrix structure containing trapped pectin to release free, water-soluble pectin from the cellulose matrix. Acid hydrolysis also converts insoluble protopectin into water-soluble pectin and determining the total pectin content of a source of citrus fibers (e.g., citrus peel). Thus, acid hydrolysis is an effective method for increasing the amount of free pectin in solution. Acid hydrolysis also decreases the degree of esterification of the pectin by at least 5% versus the degree of esterification of the pectin found in the source of citrus fibers(e.g., citrus peels). Acid hydrolysis is an example of a harsh treatment used to liberate pectin from citrus fibers.

[0035] “Activation step” refers to any step in a proceeding of producing a citrus fiber product that attempts to convert trapped, water-insoluble pectin into free, water-soluble pectin. Examples of activation steps include incubating a source of citrus fibers (e.g., citrus peel) in an acidic environment, which results in conversion of water-insoluble pectin to soluble pectin by modifying the intrinsic properties of pectin, such as decreasing the degree of esterification the pectin and breaking down the cellulose matrix that traps pectin.

[0036] “Chemical modification” refers to any modification of the citrus fibers during the production method that is imparted by addition of a chemical substance. Examples include acid hydrolysis, contact with an acid, contact with an alkali, etc. Chemical modification of citrus fiber is an example of a harsh treatment used to liberate pectin from citrus fibers.

[0037] “Citrus fiber” refers broadly to the dietary fibers (including both insoluble and soluble fibers) contained within citrus fruit. Citrus fibers are fibers contained by and obtained from the fruits of the citrus family. The citrus family is a large and diverse family of flowering plants. The citrus fruit is considered to be a specialized type of berry, characterized by a leathery peel and a fleshy interior containing multiple sections filled with juice filled sacs. Common varieties of the citrus fruit include oranges, sweet oranges, Clementines, kumquats, tangerines, tangelos, satsumas, mandarins, grapefruits, citrons, pomelos, lemons, rough lemons, limes and leech limes. The citrus fruit may be early-season, mid-season or late-season citrus fruit. Citrus fruits also contain pectin, common in fruits, but found in particularly high concentrations in the citrus fruits. Pectin is a gel-forming polysaccharide with a complex structure. It is essentially made of methoxylated galacturonic acid, galacturonic acid, rhamnose with side chains containing arabinose and galactose, which are linked through a glycosidic linkage. The pectin content and the degree of esterification of the pectin of the citrus fruit may vary based on season, where ripe fruit may contain less pectin than unripe fruit.

[0038] Citrus fiber is to be distinguished from citrus pulp, which are whole juice sacs and are sometimes referred to as citrus vesicles, coarse pulp, floaters, citrus cells, floating pulp, juice sacs, or pulp. Citrus fiber is also to be distinguished from citrus rag, which is a material containing segment membrane and core of the citrus fruit. "Citrus peel", as used herein, refers to thepectinaceous and cellulosic material contained in the outer portion of citrus fruit. It can be a waste product from the juice industry.

[0039] The citrus fibers in citrus fiber products are typically obtained from a source of citrus fibers, e.g., citrus peel, citrus pulp, citrus rag or combinations thereof. Moreover, the citrus fiber products may contain the components of the primary cell walls of the citrus fruit such as cellulose, pectin and hemicelluloses and may also contain proteins. Preferably, the source of citrus fibers used to produce the modified citrus fiber product of the invention do not undergo any substantial chemical modification, i.e., said source of citrus fibers were not subjected to chemical modification processes, such as any of esterification, derivatisation or enzymatic modification and combinations thereof.

[0040] “Comminuting” refers to the process of reducing the absolute particle size and the particle size distribution of a substance. Example machinery that can be used to comminute the modified citrus fiber product of the claimed invention include without limitation: a cutter mill, a hammer mill, a pin mill, a jet mill and the like.

[0041] “Degree of esterification (DE)” refers to the amount of esterification of pectin expressed as a molar percentage. Pectins are rich in galacturonic acid. In nature, in citrus fruit, a large proportion of the carboxyl groups of galacturonic acid are esterified with methanol. The proportion of esterified carboxyl groups with methanol relates to the DE. The DE decreases as pectin is extracted, particularly if harsh activation techniques are used, such as acid hydrolysis 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 that of the native pectin.

[0042] “Free pectin” refers to pectin that is water-soluble. Free pectin is the proportion of the total pectin content that is not trapped in the cellulose matrix or in an insoluble form (e.g., protopectin) and so can readily dissolve in water at room temperature.

[0043] “Gelling strength” refers to the ability of a citrus fiber to promote gelling in acidic and sugar conditions. A reference test is the SAG test (developed by the American Pectin Committee) in order to determine the grade strength of pectin in well-defined condition 65% sugar at pH 3 (Baker, G.L. (1959) “Pectin Standardization - Final Report of the IFT Committee”, Food Technology, 13, 496-500), which is incorporated herein by reference. The amount and quality(molar mass and DE) of water-soluble pectin determines a citrus fiber product’s ability to gel in such conditions. Increased amounts of water-soluble pectin result in a citrus fiber with high gelling strength whereas citrus fibers with low levels of water-soluble pectin have a low gelling strength. Gelling strength is directly proportional to the amount of water-soluble pectin.

[0044] “Insoluble fiber” refers to the proportion of citrus fibers that are insoluble in water at room temperature. Typically, citrus fibers are composed of around 60% insoluble fibers. Examples of insoluble fibers include cellulose and hemicellulose.

[0045] “Mixture” refers to any mixture or medium of ingredients. The term covers mixtures / mediums that can flow or are so viscous that they cannot easily flow e.g., pastes. In the context of the present invention, the ratio water to source of fibers are in the range of 95:5 to 20:80 (w / w), preferably in the range of from 80:20 to 70:30 (w / w). A particularly preferred aspect includes a ratio water to source of fibers are in the range of 50:50. A particularly preferred aspect includes a ratio water to source of fibers are in the range of 20:80.

[0046] “Native citrus fiber” refers to citrus fibers found in sources of citrus fibers (e.g., citrus peel, citrus pulp, citrus rag or combinations thereof). Native citrus fibers have not been processed nor exposed to methods associated with increasing free, water-soluble pectin content.

[0047] “Nutraceutical” refers to any substance that is a food or part of a food and provides medical or health benefits, including the prevention and treatment of disease.

[0048] “Pectin” refers to a form of water-soluble fiber found in citrus fibers. By water soluble pectin, a pectin that is soluble in water at room temperature is envisaged. Pectin can be trapped in a cellulose matrix or present in an insoluble form (protopectin). Acid hydrolysis breaks down the cellulose matrix structure to release free, water-soluble pectin from the cellulose matrix and also converts water-insoluble protopectin to water-soluble pectin. Thus, acid hydrolysis is an effective activation step for increasing the amount of free pectin in solution.

[0049] Sugar- Acid Gel (SAG) test refers to the test used to determine the grade strength of pectins in specific conditions (65% sugar at pH 3.0). The unit of value obtained is ° SAG.

[0050] “Shear” refers generally to mixing ingredients. All speeds and timings are included by the term shear. A non-limiting example of an apparatus that can be used to generate the necessaryshear is a magnetic stirrer, blender, mixer, stirrer, stretcher, extruder. Other suitable means known in the art can also be used.

[0051] “Soluble fiber” refers to the portion of citrus fibers that are soluble in water at room temperature. Typically, citrus fibers are composed of around 40% soluble fibers. An example of a soluble fiber is pectin.

[0052] “Source of citrus fibers” refers to any product from which citrus fibers can be obtained. An example of a source of citrus fibers includes citrus peel, citrus pulp, citrus rag or combinations thereof. Citrus peel, citrus pulp, citrus rag can relate to the peel, pulp or rag of any citrus fruit, including but not limited to orange, lemon, lime, mandarin, clementine, grapefruit, etc.

[0053] “Trapped pectin” refers to the proportion of total pectin that cannot freely dissolve in water. This pectin is usually trapped within the cellulose matric of the source of citrus fibers and so cannot readily diffuse out and subsequently dissolve in water. Insoluble forms of pectin (e.g., protopectin) are also encompassed by this term.

[0054] 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.

[0055] As used herein, the singular forms “a”, “an” and “the" and similar referents in the context of describing the elements (especially in the context of the following claims) include plural referents unless the context clearly dictates otherwise. For example, reference to "a substituent" encompasses a single substituent as well as two or more substituents, and the like. It is understood that any term in the singular may include its plural counterpart and vice versa, unless otherwise indicated herein or clearly contradicted by context.

[0056] Additionally, the phrase “consisting essentially of’ will be understood to include those elements specifically recited and those additionally elements that do not materially affect the basic and novel characteristics of the invention. The phrase “consisting of’ excludes any element not specified.

[0057] In addition, where features or aspects of the disclosure are described in terms of Markush groups, those skilled in the art will recognize that the disclosure is also thereby described in terms of any individual member or subgroup of members of the Markush group. Each of the narrower species and subgeneric groupings falling within the generic disclosure also form part of the invention. This includes the generic description of the invention with a proviso or negative limitation removing any subject matter form the genus, regardless of whether or not the excised material is specifically.

[0058] Throughout this document, particularly in terms of providing a written description, all values expressed in a range format should be interpreted in a flexible manner to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. Any listed range can be easily recognized as sufficiently describing and enabling the same range being broken down into at least equal halves, thirds, quarters, fifths, tenths, etc. For example, a range of “about 0.1% to about 5%” or “about 0.1% to 5%” should be interpreted to include not just about 0.1% to about 5%, but also the individual values (e.g., 1%, 2%, 3%, and 4%) and the sub-ranges (e.g., 0.1% to 0.5%, 1.1% to 2.2%, 3.3% to 4.4%) within the indicated range. As will also be understood by one skilled in the art all language such as “up to,” “at least,” “greater than,” “less than,” and the like, include the number recited and refer to ranges which can be subsequently broken down into subranges as discussed above. Finally, as will be understood by one skilled in the art, a range includes each individual member.

[0059] As used herein, the terms “for example,” “for instance,” “such as,” or “including” are meant to introduce examples that further clarify more general subject matter. Unless otherwise specified, these examples are provided only as an aid for understanding the applications illustrated in the present disclosure and are not meant to be limiting in any fashion.

[0060] As used herein, “about” will be understood by persons of ordinary skill in the art and will vary to some extent depending upon the context in which it is used. If there are uses of the term which are not clear to persons of ordinary skill in the art, given the context in which it is used, “about” will mean up to plus or minus 10% of the particular term.

[0061] Modified citrus fiber product.

[0062] An aspect of the present invention relates to an improved modified citrus fiber product.

[0063] The modified citrus fiber product of the present invention has a fiber content and degree of esterification (DE) that is similar (i.e., within 10%) to that of the citrus fibers contained within the source of citrus fibers. The DE of pectin contained in citrus fiber products that utilise chemicalbased (e.g., acid-based) method steps to increase the amount of free, water-soluble pectin is significantly lower than the DE of pectin found in the source of citrus fibers due to negative impacts of the chemicals / acid on the intrinsic factors and structural integrity of the pectin. Moreover, the modified citrus fiber product of the invention has a free, water-soluble pectin content that is greater than that seen in citrus fiber products that do not utilise an activation step. Therefore, the modified citrus fiber product of the present invention represents a label friendly citrus fiber product modified to increase the amount of freely, water soluble available pectin.

[0064] The modified citrus fiber product of the present invention thus represents an improvement over known citrus fiber products.

[0065] In some examples, the modified citrus fiber product contains from 10 to 40% water soluble pectin. Preferably, the modified citrus fiber product contains between 10 to 30%, 20 to 40% or 30 to 40% water soluble pectin. The amount of free, water-soluble pectin comprised in the modified citrus fiber product is greater than that present in citrus peel, but the intrinsic properties, such as the degree of esterification, of the free, water-soluble pectin comprised in the modified citrus fiber product is substantially the same, if not identical, to the pectin found in citrus peel. Surprisingly, the modified citrus fiber product exhibits improved properties (e.g., gel strength) compared to the source of citrus fibers (e.g., citrus peel). For example, the modified citrus fiber product has a gel strength of from 30 to 100 SAG, preferably a gel strength of from 45 to 100 SAG, more preferably 45 to 95 SAG, even more preferably 50 to 80 SAG. Thus, the modified citrus fiber product of the present invention represents a lab el -friendly citrus fiber product modified to increase the amount of freely available, water-soluble pectin.

[0066] Process for producing a modified citrus fiber product.

[0067] An aspect of the present invention relates to an improved process for producing modified citrus fiber products.

[0068] The process comprises a) combining a source of citrus fibers with water to form an aqueous mixture; and b) heating the aqueous mixture to a temperature between 60 to 150 degrees Celsius; and c) drying the aqueous mixture to obtain the modified citrus fiber product. The resulting modified citrus fiber product has a gel strength of from 30 to 100 SAG and a degree of esterification of from 30 to 100%.

[0069] The process of the present invention avoids the use of harsh activation methods that require treatment with a chemical, such as an acid, to convert trapped, water-insoluble pectin to free, water-soluble pectin. In contrast, the present invention modifies the native citrus fibers found in the source of citrus fibers (e.g., citrus peel) using water and energy i.e., thermomechanical activation steps only. The use of acid (or any other chemical) is avoided. The use of water, heat and energy (thermomechanical activation steps only) converts trapped, water-insoluble pectin to free, water-soluble pectin without the need to use chemical-activation steps in the method meaning that the intrinsic factors, such as the degree of esterification, of the pectin found in the source of citrus fibers is thus maintained in the modified citrus fiber product. The modified citrus fiber product of the present invention this represents an improved, lab el -friendly citrus fiber product.

[0070] While the use of harsh, chemical -heavy activation methods may result in higher quantities of water-soluble fibers (i.e., pectin), the intrinsic properties (i.e., the degree of esterification) of these water-soluble fibers is significantly reduced compared to that of pectin found in the source of citrus fibers since the chemicals used to increase pectin yield alter the structure of the cellulose matrix and of the natural pectin. As the degree of esterification of pectin found in products that utilise acid-based activation methods is significantly reduced compared to pectin found in the source of citrus fibers, these citrus fiber products are not lab el -friendly.

[0071] In contrast, the present invention avoids the use of harsh activation methods meaning that the liberated pectin, albeit present in smaller amounts, has substantially the same degree of esterification to that of the pectin found in citrus peel. Due to the higher pectin levels, the gelling strength of the modified citrus fiber product obtained by the process of the invention is between 30 and 100 ° SAG whereas citrus fiber products obtained using methods that do not employ anactivation step to liberate trapped, water-insoluble pectin is 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 peel shows that the present invention relates to a lab el -friendly citrus fiber product. The present invention thus provides a process for producing a modified citrus fiber product that has a strong gelling strength, as indicated by the high SAG value. The fact that the degree of esterification of the pectin comprised in the citrus fiber product is substantially the same, if not identical, to the pectin found in the source of citrus fibers (e.g., citrus peels) demonstrates that the citrus fiber product is lab el -friendly.

[0072] Thus, the process of the present invention relates to an improved process for producing a modified, label-friendly, citrus fiber product by ensuring that the intrinsic factors of the water soluble citrus fibers (pectin) present in the modified citrus fiber product remains substantially the same, if not identical, as those found in pectin of native citrus peel but increases the amount of freely available, water soluble pectin by virtue of the thermomechanical activation method steps that convert trapped, water-insoluble pectin to free, water soluble pectin.

[0073] In an example, the heating step is performed under shear. The shear can be provided using any device that permits mixing of the water and source of citrus fiber. An example includes magnetic stirring or extrusion or use of a mixer. Shearing has the advantage of mixing the source of citrus fibers and water, which increases the quantity of soluble citrus fibers and to increase the functionality. In a preferred example, the shear occurs at a speed of up to 20,000 rpm, most preferably between 80 and 250 rpm. In a further preferred example, the heating with or without shearing occurs for up to 7 hours, most preferably between 3 and 5 hours. In some aspects, shearing is carried out using extrusion for up to five minutes. In some aspect, shearing is carried out using extrusion for less than five minutes. This ensures that there is sufficient time to permit conversion of trapped, water-insoluble pectin to be converted into free, water soluble that can diffuse into the water. The skilled person would readily appreciate that the intensity of shearing, the shearing time and the ratio water to source of fibers are inter-related and adjust the conditions accordingly. For example, if the mixture is being mixed at a high shear then a shorter shearing time would be needed and vice versa.

[0074] In a preferred example, the mixture is heated to a temperature between 60 and 150°C. The temperature should not exceed 150°C as this could result in degradation of the source of citrus fibers.

[0075] In a preferred example, the ratio of water to source of fibers is in the range of between 95:5 and 20:80 (w / w). In a further preferred example, the ratio of water to source of fibers is in the rage of between 80:20 to 70:30 (w / w). In an even more preferred example, the ratio of water to source of fibers is in the rage of between 50:50 (w / w). In an even more preferred example, the ratio water to source of fibers is in the rage of between 20:80 (w / w). This has the advantage that there is sufficient water for the liberated soluble citrus fibers that are converted from trapped, insoluble sources within the source of citrus fibers to dissolve in whilst not having too much water present in the mixture that could negatively affect the drying step. The skilled person would be able to adjust the amounts of water and source of citrus fibers accordingly. The skilled person would also be able to select the most appropriate method of shearing to account for the volume of water present in the mixture.

[0076] In a preferred example, the pectin contained in the modified citrus fiber product produced using the process of the claimed invention has a degree of esterification (DE) that is within 5% of the degree of esterification of the source or citrus fibers. In a further preferred example, the DE of the pectin is substantially identical to the DE of the pectin found in the source of citrus fibers. Since the claimed invention avoids harsh activation techniques (e.g., using acid), the pectin structure and the associated cellulose matrix is maintained meaning that there are little to no differences in the degree of esterification of the pectin found in the modified citrus fiber product of the invention compared to the pectin found in citrus peel. The proportion of the carboxyl groups of galacturonic acid that are esterified with methanol in the pectin comprised within the modified citrus fiber product is largely unchanged when compared to the native citrus fiber found in the source of citrus fibers since the use of harsh chemicals in an activation step is avoided. While any acid technique is expected to result in a decrease (at least 5%) in the DE of the resulting citrus fiber product, the DE of the pectin comprised in the modified citrus fiber product obtained using the process of the present invention will be far greater than the DE of pectin comprised in citrus fiber products obtained using harsh, acid-based, conditions due to the negative effects that these conditions have on the pectin structure. Since only thermomechanical activation method steps are used in the process of the invention, the DE of the pectin comprised in the citrus fiber productobtained using the process is comparable to that of pectin found in native citrus fibers unlike citrus fibers obtained using acid activation method steps, such as the prior art processes.

[0077] In a preferred example, the process of the present invention does not comprise a chemical modification step. These chemical modifications can include, but are not limited to treatment with acid, treatment with alkali, acid hydrolysis, enzyme treatment (e.g., pectinase). These chemical modifications can also include esterification, derivatisation or enzymatic modification and combinations thereof. Chemical modifications are intended to include crosslinking, acetylation, organic esterification, organic etherification, hydroxyalkylation (including hydroxypropylation and hydroxyethylation), phosphorylation, inorganic esterification, ionic (cationic, anionic, nonionic, and zwitterionic) modification, succination and substituted succination of polysaccharides. Also included are oxidation and bleaching.

[0078] In a preferred example, the modified citrus fiber product is comminuted before thermomechanical treatment and / or after drying. Comminuting can be performed by any suitable apparatus. For example, the citrus fiber product can be ground using a grinder and subsequently sieved to obtain powdered form of the modified citrus fiber product. The modified citrus fiber product can then be packaged, stored and shipped for end use. Examples of suitable means to comminute the modified citrus fiber product include without limitation a cutter mill, a hammer mill, a pin mill, a jet mill, centrifugal mill and the like.

[0079] Citrus fibers obtained by the process of the present invention represent an improved modified citrus fiber product. Since the use of harsh activation techniques (such as the use of chemicals, such as acid) are avoided, the pectin contained in the modified citrus fiber product is not chemically degraded when compared to the pectin found in the native source of citrus fiber (i.e. pectin found in citrus peel) and thus the modified citrus fiber product obtained by the claimed method represent a simple, lab el -friendly citrus fiber as the intrinsic properties, such as the degree of esterification, of the pectin comprised in the modified citrus fiber product is substantially the same, if not identical, to the degree of esterification of the pectin found in the source of citrus fibers.

[0080] The modified citrus fiber product of the present invention can be packed into a composition (containing additives of excipients) or a consumable. Preferably, the consumable is a food product, beverage, cosmetic product, or a nutraceutical product.

[0081] Uses of the modified citrus fiber product

[0082] A further aspect of the invention relates to uses of the modified citrus fiber product.

[0083] The uses envisaged by the isolated citrus fibers of the present invention include uses in the food, consumer and health industries. Specifically, the isolated citrus fibers will be used for their viscosifying, water absorbing, bulking, emulsifying, texturizing and gelling properties.

[0084] Examples

[0085] The invention will now be defined by reference to the following, non-limiting, examples.

[0086] Example 1 - process for preparing a modified citrus fiber product

[0087] Eight methods for producing the modified citrus fiber products in accordance with the claimed invention are outlined below.

[0088] Example using Sigma blade mixer MRL 5 from RMC Guittard:• Weigh 300 g of dry citrus peels.• Add 1200 g of boiling osmosis water.• Mix manually, transfer to the mixer tank at 85°C.• Mix at 80 rpm for 5 h.• Recover the paste after 5 h, grind to obtain small pieces.• Dry in a ventilated oven at 60°C for 16h.• Grind and sieve the sample at 250 pm.

[0089] The resulting modified citrus fiber product had a gelling strength of 70-80 °SAG.

[0090] Example using lab cheese stretcher from Blentech:• Weight 400 g of dry citrus peels• Add 600 g of boiling osmosis water• Mix manually, transfer to the stretcher tank at 80°C (double jacket regulation)• Mix at approx. 250 rpm for 3-5 h• Recover the paste, grind to obtain small pieces• Dry in a ventilated oven at 60°C for 16h• Grind and sieve the sample at 250 pm

[0091] The resulting modified citrus fiber product has a gelling strength of 80-90 °SAG.

[0092] Example using lab cheese stretcher from Blentech (steam injection):• Weight 750 g of dry citrus peels• Add 320 g of boiling osmosis water• Mix manually, transfer to the stretcher tank at 80°C• Mix at approx. 50 rpm for 1 h, inject steam to maintain the temperature and decrease the dry matter• After 1 h, increase to approx. 250 rpm for 2-4 h, maintain the temperature with the double jacket• Recover the paste, grind to obtain small pieces• Dry in a ventilated oven at 60°C for 16h• Grind and sieve the sample at 250 pm

[0093] The resulting modified citrus fiber product has a gelling strength of 80-95 °SAG.

[0094] Example using KS Mixer from Karl Schnell:• Add 10000 g of soft water in the mixer tank, heat it up to 85°C• Add 5000 g of dry citrus peels (coarse or ground)• Mix at 120-140 rpm for 3-8 h used double wall heating to maintain 80°C in the medium• Recover the paste, grind to obtain small pieces• Dry in a ventilated oven at 60°C for 16hGrind and sieve the sample at 250 pm

[0095] The resulting modified citrus fiber product had a gelling strength of approximately 70° SAG.

[0096] Example using KS Mixer from Karl Schnell (steam injection):• Add 2000 g of cold soft water in the mixer tank• Add 5000 g of dry citrus peels (coarse or ground)• Inject steam to heat it up 90°C while mixing 25 rpm• When DM is 33-40%, mix at 120-140 rpm till 3-7 h time used double wall heating to maintain 80°C in the medium• Recover the paste, grind to obtain small pieces• Dry in a ventilated oven at 60°C for 16h• Grind and sieve the sample at 250 pm

[0097] The resulting modified citrus fiber product had a gelling strength of 75-85 °SAG.

[0098] Example using Thermomix blender from Vorwerk:• Weight 75 g of dry citrus peels• Add 1425 g of boiling osmosis water• Mix manually, transfer to blender at 80°C• Let 30 min under gentle stirring• Stir / grind speed 10 for 3 min• Recover the mixture• Dry in a ventilated oven at 60°C for 16h• Grind and sieve the sample at 250 pm

[0099] The resulting modified citrus fiber product had a gelling strength of 60-80 °SAG.

[0100] Example in static condition (beaker):• Weight 60 g of dry citrus peels (coarse or ground) in hot beaker• Add 240 g of boiling osmosis water• Mix manually to homogenize (<1 min), cover the beaker with a lid to avoid evaporation, maintain at 80°C without stirring for 3-8 h• Recover the wet peels• Dry in a ventilated oven at 60°C for 16h• Grind and sieve the sample at 250 pm

[0101] The resulting citrus fiber product had a gelling strength of 50-60 °SAG.

[0102] Example using twin-screw extruder ZSE 12 HP -PH from Leistritz:• Manage the continuous introduction of ground dry citrus peels (zone 1) and osmosis water (zone 2) in order to have inlet DM between 50 and 80%• Heat 8 zones from 40°C (zone 1, peels entrance) to 150°C (nozzle head), 200-400 rpm, 600 g / h total flow, single hole nozzle head of 1-2 mm• Recover the extruded product• Dry in a ventilated oven at 60°C for 16h• Grind and sieve the sample at 250 pm

[0103] The resulting modified citrus fiber product had a gelling strength of 70-80 °SAG.

[0104] Example 2 - total pectin content, water soluble pectin content, gelling strength and degree of esterification of the modified citrus fiber product

[0105] The total pectin content (%), water soluble pectin content (%), gelling strength (° SAG) and degree of esterification (DE) of the modified citrus fiber product obtained from the method of the present invention was analysed and compared to that of citrus fiber products obtained from methods of the prior art. Specifically, the parameters were compared to citrus fiber products that either do not employ an activation step to convert trapped, water-insoluble pectin to free, soluble pectin (e.g. ground peels) or that use acid-based activation steps to do so.

[0106] Specifically, citrus fibers produced from either the claimed method or methods of the prior art were obtained and the pectin content, gelling strength and degree of esterification assessed using the following methods.

[0107] Water soluble pectin. Pectin / soluble fiber extraction and recovery in mild conditions. 75 g of source of fibers are added to 2500 g of osmosis water at room temperature under magnetic stirring. The medium is stirred at 450 rpm for 1 h at room temperature. The medium is centrifuged at room temperature 20 min at 4500 rpm. The supernatant is then precipitated in isopropanol. The solid recovered is dried in a ventilated oven at 60°C. The yield is defined as the sum of the quantity of dry solid obtained from the supernatant and the assumed part lost in the wet bottom divided by the initial weight (75 g).

[0108] Total pectin content, acid extraction of Pectin. 100 g of source of fibers are added to 4000 g of osmosis water at 80°C under mechanical stirring. pH of the medium is adjusted to 1.6 using 30% HNO3. The medium is stirred for 4 h at 80°C. The medium is centrifuged 20 min at 4500 rpm. The supernatant is adjusted at pH 3 using 10% Na2COs and then precipitated in IPA. The solid recovered is dried in a ventilated oven at 60°C. The yield is defined as the quantity of dry solid obtained from the supernatant divided by the initial weight (100 g).

[0109] Determination of gelling strength (SAG)

[0110] The method comes from method 5 - 54 of the IFT committee on pectin standardization.

[0111] The apparatus included the following:• Laboratory scale (accuracy 0.1 and 0.001 g)• Stainless steel saucepan, 15 cm diameter• Electric hotplate• Hand whisk• Beakers (1000 ml and 150 ml)• Spatula• Stop watch• Thermometer, 100 °C• pH-meter• SAG-glasses and tape• Ridgelimeter• Wire cheese slicer• Refractometer• Incubator

[0112] The chemicals used were sugar, tartaric acid (CAS 87-698-4) (488 g in 1 L solution), and osmosis water.

[0113] The preparation of jelly was as follows:• Weigh into 1000 mL beaker [650 - (650 / x)] g sugar, where x = assumed firmness of sample.• In a dry 150 mL beaker, add sample. Sample weight (g) = [650 / x], where x = assumed firmness of sample.• Add 20 g of the weighed sugar into the sample.• Mix the sample and sugar by stirring with spatula.• Split the weighed sugar in two equal fractions.• Pour 410 g osmosis water in the tared stainless steel saucepan with hand whisk.• Pour the sample / sugar mixture into water - all at once - while stirring manually.• Stir continuously for two minutes.• After 2 minutes, place the saucepan on the electric hotplate, and heat while continuously stirring manually.• When the medium reaches a full rolling boil, add one part of the sugar. Stir continuously.• When the medium starts to boil again, add the second part of the sugar. Stir continuously until net weight of the jelly batch is 1015 g. The electric hotplate should be set so that the entire heating time for the jelly is 5 - 8 minutes.• After weighing the 1015 g batch on the laboratory scale, leave it undisturbed on the table for one minute.• 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 26pprox.. 1 cm above the brims.• When the temperature reaches 30 - 35 °C, place the glasses in an incubator at 25 ± 3 °C for 20 - 24 hours.

[0114] The properties of the jelly were measured as follows:• After 20 - 24 hours storage at 25 ± 3 °C, remove the tape from glasses. Using a wire cheese slicer, cut off the top layer and discard it.• Then carefully turn the jelly out of the glass to an inverted position on a square glass plate furnished with Ridgelimeter.• Start stop watch once the jelly is on the glass plate.• Place plate and jelly carefully on the base of the Ridgelimeter so that the jelly is centered under the micrometer screw, which should then be screwed down near to the surface of the jelly.• Two minutes after the stop watch was started, bring the point of the micrometer screw into contact with the jelly surface and record the Ridgelimeter reading to the nearest 0.1.• Measure pH, which must be between 2.2 and 2.4. Otherwise, the sample must be retested. Increase the amount of tartaric acid solution if the pH is too high, decrease the amount if the pH is too low.

[0115] The jelly grade of the sample is calculated as follows:• Using the Ridgelimeter calibration table, convert the Ridgelimeter reading to a Factor F. The Ridgelimeter reading needs to be between 19.5 and 27; otherwise the sample must be retested with another assumption for the sample firmness.• Using the soluble solids correcting table, the soluble solids measured is converted into a Factor C. The soluble solid content needs to be between 64.5 and 65.5; otherwise the sample must be retested.• When multiplying the assumed grade of the test by the correction factors, the true grade is obtained using the following formula:Assumed grade x factor F x factor C = True grade / SAG

[0116] Factors F and C can be determined using the below tables:

[0117] Determination of Degree of Esterification (DE) and Degree of Galacturonic Acid

[0118] The degree of esterification (DE) and degree of galacturonic acid (Gal A) are measured using a modification of the method set forth in TRS 669-JECFA 25 / 28 INS No. 440.

[0119] Sample preparation:• In a beaker, add 100 mL of the acid alcohol (250 mL 50-60% isopropanol + 5 mL HC1 fuming 37%) to 2.00 g of ground sample (Wl) while stirring with a magnetic stirrer for 10 min.• Filter and pass the mixture through a Buchner funnel.• Rinse the beaker and pour 6 x 15 mL acid alcohol through the Buchner funnel.• Wash the solid residue in the Buchner funnel at least 8 times with 50 mL 50-60% isopropanol and then 2 times with 50 mL 87% isopropanol.• Dry the sample for approximately 2.5 hours at 105°C. Weight the dry sample (W2).• Weight 0.5 g of samples (W3)• Moisten the sample with approximately 2 mL 87% isopropanol.• Add approximately 100 mL of boiling ultrapure water while stirring with a magnetic stirrer. Cover the medium with plastic wrap and let it cool down to room temperature.

[0120] The sample is then evaluated by titration by using a pH meter / autoburette, as follows:• Titrate the sample with 0.1 N NaOH (record Veql).• Add 20.0 mL 0.5 N NaOH while stirring and cover with foil for exactly 15 min.• Add 20.0 mL 0.5 N HC1 while stirring.• Titrate the sample with 0.1 N NaOH (record Veq2).• In order to compensate for possible inaccuracies of balancing the two portions of 20 mL of 0.5 N NaOH and HC1 respectively, a so-called “blind measurement” was performed (i.e., 100 mL of deionized water was treated in the same way as the sample solution, including the titrations). The titration of this blank test is recorded as Vc.

[0121] The DE and Gal A are determined using the following calculations:

[0122] The results are outlined in Table 1 :Table 1[1] same initial source of citrus fiber (batch 1); [2] same initial source of citrus fiber (batch 2). Standard deviation is reported when extraction was repeated 3 times.

[0123] As shown in Table 1, the citrus fiber product obtained using the method of the 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 that involves acid-based activation (row 4) is greater than that of the claimed citrus fiber product as the acid-based methods used to produce these citrus fibers liberate water-insoluble pectin that is trapped in the cellulose matrix of the citrus peel. However, when compared to the citrus fiber product of the invention, the degree of esterification of the water-soluble pectin comprised in a citrus fiber product produced by methods that employ an acid-based activation step is reduced by approximately 8%. Therefore, the pectin comprised in these citrus fiber products has changed substantially compared to pectin comprised in the native citrus peel. In contrast, the degree of esterification of the pectin comprised in the modified citrus fiber product of the present invention (row 3) is comparable to that seen in native citrus peels, as shown by the similar degrees of esterification to that seen in ground citrus peels (rows 1 and 2 of the above table). Thus, the method of the present invention produces a modified citrus fiber product with a higher pectin content compared to citrus fiber products that do not employ an activation step in the production methods whilst ensuring that the degree of esterification of the pectin comprised in the modified citrus fiber product is substantially the same, if not identical, to that found in the source of citrus fibers since the internal pectin structure has not been compromised due to acid treatment.

[0124] In summary, the modified citrus fiber product isolated using the process of the invention may not comprise as much water-soluble pectin as other citrus fibers, such as those produced using methods that involve an acid-activation step, but the process produces a product containing amounts of soluble pectin that is greater than products produced by methods that do not use anactivation step at all. Crucially, the degree of esterification of the water-soluble pectin comprised in the modified citrus fiber product of the invention compared to that of products produced using acid-based activation method steps is far closer to, if not the same as, that seen in the source of citrus fibers as the internal pectin structure has not been compromised due to the mild, thermomechanical methods used to isolate the pectin. Therefore, the modified citrus fiber product of the claimed invention represents a label-friendly citrus fiber product (as demonstrated by the similar DE percentage of the modified citrus fiber product of the invention and citrus fiber products produced using methods that do not employ an activation step) modified to increase the amount of freely, water-soluble available pectin (as demonstrated by the increased percentage of water-soluble pectin of the modified citrus fiber product of the invention and citrus fiber products produced using methods that do not employ an activation step).

[0125] Example 3 - comparative properties of modified citrus fiber product

[0126] Properties of the modified citrus fiber product obtained by the process outlined in Example 1 and Figure 1 were assessed and compared with known citrus fiber products obtained using methods that either employ no activation step to convert trapped, water-insoluble pectin into free, water soluble pectin or that use acid-based methods to do so or that have had pectin extracted and the remaining citrus peels have been subsequently dried and ground. The results are outlined in Table 2.

[0127] The values stated in Table 2 represent a range of values, i.e., the results are not indicative of values recorded on a single sample. The results thus represent the typical range that can be obtained for the specific type of product.Table 2* Commercial products

[0128] As demonstrated in Table 2, the gelling ability of a modified citrus fiber product obtained by the process of the claimed invention (sample 4) is greater than a citrus fiber with a similar pectin content that is not obtained by the claimed invention (sample 3) or pectin-depleted citrus fibers (sample 1). This increase in gelling ability is due to the thermomechanical activation steps used in the process of the invention, which promotes pectin availability by converting trapped, water-insoluble pectin into free, water-soluble pectin. The pectin present within the modified citrus fiber product of the invention (sample 4) will have a similar degree of esterification as native pectin (i.e., pectin present in the source of citrus fiber (citrus peel)) since the structural integrity of the native pectin will have been maintained due to the lack of acid treatment. As can be seen for sample 2, pectin levels increase due to large-scale acid treatment due to liberation of pectin from the cellulose matrix and insoluble stores (protopectin). The increased amount of pectin causes an increase in gelling ability. However, the structural integrity and resulting degree of esterification of the pectin in sample 2 will be significantly less than the DE of sample 4, as shown in Table 1.

[0129] Example 4 -isolated citrus fibers exhibit improved gelling strength

[0130] The gelling strength (° SAG) of the modified citrus fiber product produced according to the method of the invention and citrus fiber products that are prepared without using an activationstep to convert trapped, water-insoluble pectin into free, soluble pectin were assessed using the method outlined in example 2.

[0131] A citrus fiber product was produced by subjecting a source of citrus fiber (indicated in the first column of Table 3) to methods that either do not employ an activation step to convert trapped, water-insoluble pectin into free, water-soluble pectin (column 2) or that employ the thermomechanical activation method steps of the present invention (column 3).

[0132] The results are shown in Table 3:Table 3Repetition means that the method of the present invention was applied several times starting from the same initial source of fiber. Standard deviation is reported for 3 and more repetitions.

[0133] As demonstrated in Table 3, exposing the source of citrus fibers indicated in the first column of Table 3 to the process of the invention increases the gelling ability of the resulting citrus fiber product (column 3) when compared to simply drying and grinding the source of citrus fibers without exposing them to the activation steps of the process of the invention (column 2). This is because the process of the invention increases the amount of freely available, water-soluble pectin comprised within the citrus fiber product whilst also ensuring that this pectin retains the intrinsic properties, such as the degree of esterification, of the native pectin found in the original source of citrus fibers.

[0134] The invention may also broadly consist in the parts, elements, steps, examples and / or features referred to or indicated in the specification individually or collectively in any and all combinations of two or more said parts, elements, steps, examples and / or features. In particular, one or more features in any of the embodiments described herein may be combined with one or more features from any other embodiment(s) described herein.

[0135] Protection may be sought for any features disclosed in any one or more published documents referenced herein in combination with the present disclosure.

[0136] Although certain example embodiments of the invention have been described, the scope of the appended claims is not intended to be limited solely to these embodiments. The claims are to be construed literally, purposively, and / or to encompass equivalents.

[0137] 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. Additionally, the phrase “consisting essentially of’ will be understood to include those elements specifically recited and those additionally elements that do not materially affect the basic and novel characteristics of the invention. The phrase “consisting of’ excludes any element not specified. It must also be noted that as used herein and in the appended claims, the singular forms "a," "an," and "the" include plural references unless the context clearly dictates otherwise. Although any systems and methods similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present disclosure, the preferred systems and methods are now described.

[0138] As used herein, the terms “for example,” “for instance,” “such as,” or “including” are meant to introduce examples that further clarify more general subject matter. Unless otherwise specified, these examples are provided only as an aid for understanding the applications illustrated in the present disclosure and are not meant to be limiting in any fashion.

[0139] As used herein, “about” will be understood by persons of ordinary skill in the art and will vary to some extent depending upon the context in which it is used. If there are uses of the term which are not clear to persons of ordinary skill in the art, given the context in which it is used, “about” will mean up to plus or minus 10% of the particular term.

[0140] In addition, it is to be understood that the phraseology or terminology employed herein, and not otherwise defined, is for the purpose of description only and not of limitation. Any use of section headings is intended to aid reading of the document and is not to be interpreted as limiting; information that is relevant to a section heading may occur within or outside of that particular section. In the event of inconsistent usages between this document and those documents so incorporated by reference, the usage in the incorporated reference should be considered supplementary to that of this document; for irreconcilable inconsistencies, the usage in this document controls.REPRESENTATIVE FEATURESRepresentative features 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 and / or drawings of the specification.1. A modified citrus fiber product wherein the citrus fiber product has a gelling strength of from 30 to 100 °SAG and a degree of esterification of from 30 to 100%.2. The citrus fiber product of clause 1 comprising from 10 to 40% water-soluble pectin.3. The citrus fiber product of clause 2 comprising 20-30% water-soluble pectin.4. The modified citrus fiber product of any one of the preceding clauses, wherein the gelling strength is between 50 and 80 °SAG,5. The modified citrus fiber product of clause 4, wherein the gelling strength is 70 ° SAG.6. The modified citrus fiber product of any one of the preceding clauses, wherein the degree of esterification is between 50 and 80%.7. The modified citrus fiber product of any one of the preceding clauses, wherein the degree of esterification is 70%.8. A process for producing a modified citrus fiber product comprising: a) Combining a source of citrus fibers with water to form an aqueous mixture; and b) Heating the aqueous mixture to a temperature from 60 to 150 degrees Celsius; and c) Drying the aqueous mixture to obtain the modified citrus fiber product; wherein the modified citrus fiber product has a gel strength of from 30 to 100 SAG and a degree of esterification of from 30 to 100%.9. The process of clause 8, wherein the heating comprises heating via thermal conduction, direct introduction of steam, mechanical shearing / friction or combinations of two or more thereof.10. The process of clauses 8 or 9, wherein step (b) is carried out under shear.11. The process of any one of clauses 8-10, wherein the modified citrus fiber product has a degree of esterification within + / - 10% of the degree of esterification of the source of citrus fiber.12. The process of any one of clauses 8 to 11, wherein the modified citrus fiber product has a degree of esterification which is substantially identical to the degree of esterification of the source of citrus fiber.13. The process of any one of clauses 8-12, wherein the citrus fiber product comprises between 10 to 40% water-soluble pectin.14. The process of clause 13, wherein the citrus fiber product comprises 20-30% water-soluble pectin.15. The process of any one of clauses 8-14, wherein the gelling strength of the citrus fiber product is between 50 and 80 ° SAG,16. The process of clause 15, wherein the gelling strength of the citrus fiber product is 70 ° SAG.17. The process of any one of clauses 8-16, wherein the degree of esterification of the citrus fiber product is between 50 and 80%.18. The process of clause 17, wherein the degree of esterification of the citrus fiber product is 70%.19. The process of any one of clauses 8-18, wherein no compounds are added and / or enriched prior to step (b).20. The process of any one of clauses 8-19, wherein no compounds are extracted and / or exhausted prior to step (b).21. The process of any one of clauses 8-20, wherein the process does not comprise a chemical modification or chemical activation step.22. The process of clause 21, wherein the chemical modification or activation step is basic or acid hydrolysis.23. The process of any one of clauses 8-22, further comprising a step of comminuting the modified citrus fiber product before step a) and / or after step c).24. The process of any one of clauses 8-23, wherein the ratio of water to source of fibers in step (a) is from 95:5 to 20:80 (w / w),25. The process of clause 24, wherein the ratio of water to source of fibers in step a) is 50:50 (w / w), preferably wherein the ratio of water to source of fibers in step a) is 20:80 (w / w).26. Modified citrus fiber product obtainable by the process of any one of clauses 8-25.27. 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 from 30 to 100 SAG and a degree of esterification of from 30 to 100%.28. A consumable comprising the modified citrus fiber product of any one of clauses 1-7 or 26 or the composition of clause 27.29. A consumable according to clause 28, wherein the consumable is a food product, a beverage, cosmetic product or a nutraceutical product.30. Use of the modified citrus fiber product according to any one of clauses 1-7 or 26 or the composition of clause 27 in a consumable.31. The use of clause 30, wherein the consumable is a food product, a beverage, cosmetic product, or a nutraceutical product.32. The modified citrus fiber product of clauses 1-7 or 26, the composition of clause 27 or the consumable of clause for use in medicine.33. The modified citrus fiber product of clauses 1-7 or 26, the composition of clause 27 or the consumable of clause 28 for use in lowering blood cholesterol, reducing weight, stabilising blood glucose and / or diabetes.34. The process of any one of clauses 8-25, wherein step (b) of the process is carried out under shear at a speed of up to 20,000 rpm, preferably between 80-250 rpm.35. The process of any one of clauses 8-25 or 34, wherein the aqueous mixture is heated to 80 degrees Celsius.36. The process of any one of clauses 8-25, 34 or 35, wherein the aqueous mixture is heated for between 1 minute and 7 hours, preferably between 3-5 hours, even more preferably 4 hours.37. The process of any one of clauses 8-25 or 34-36, wherein the ratio water to source of fibers in step (a) is from 95:5 to 20:80 (w / w).38. The process of clause 37, wherein the ratio water to source of fibers in step (a) is from 80:20 to 70:30 (w / w).39. The process of clause 38, wherein the ratio water to source of fibers in step (a) is 50:50 (w / w).

Claims

CLAIMS1. A modified citrus fiber product wherein the citrus fiber product has a gelling strength of from 30 to 100 °SAG and a degree of esterification of from 30 to 100%.

2. The modified citrus fiber product of claim 1 comprising from 10 to 40% water soluble pectin.3 A process for producing a modified citrus fiber product comprising: a) combining a source of citrus fibers with water to form an aqueous mixture; and b) heating the aqueous mixture to a temperature from 60 to 150 degrees Celsius; and c) drying the aqueous mixture to obtain the modified citrus fiber product; wherein the modified citrus fiber product has a gelling strength of from 30 to 100 °SAG and a degree of esterification of from 30 to 100%.4 The process of claim 3, wherein step (b) is carried out under shear.5 The process of claim 3 or 4, wherein the modified citrus fiber product has a degree of esterification within + / - 10% of the degree of esterification of the source of citrus fiber.6 The process of any one of claims 3 to 5, wherein the modified citrus fiber product has a degree of esterification which is substantially identical to the degree of esterification of the source of citrus fibers.7 The process of any one of claims 3 to 6, wherein no compounds are added and / or enriched prior to step (b).8 The process of any one of claims 3 to 7, wherein no compounds are extracted and / or exhausted prior to step (b).9 The process of any one of claims 3 to 8, wherein the process does not comprise a chemical modification step.

10. The process of any one of claims 3 to 9, further comprising a step of comminuting the modified citrus fiber.

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

12. A modified citrus fiber product obtainable by the process of 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 from 30 to 100 SAG and a degree of esterification of from 30 to 100%.

14. A consumable comprising the modified citrus fiber product of any one of claims 1, 2 or 12 or the composition of claim 13.

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

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