Composition comprising pectin and water

By adjusting the ratio of esterification to amidation of low-methoxyamidized pectin, a composition with specific gelation temperature and critical gelation concentration was prepared, solving the problem of limited gelation temperature and calcium sensitivity range of LM pectin in the food and beverage industry, and achieving wider application adaptability.

CN120897952APending Publication Date: 2025-11-04CARGILL INC
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Patent Information

Application Number
CN202480023001.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Priority Date
2023-04-06
Filing Date
2024-04-01
Publication Date
2025-11-04

AI Technical Summary

Technical Problem

Existing LM pectin has limitations in gelation temperature and calcium sensitivity range in the food and beverage industry, making it difficult to meet the needs of different products.

Method used

By preparing low-methoxyamidized pectin, adjusting the ratio of esterification to amidation of the pectin, and controlling the water concentration range, a composition with a specific gelation temperature and critical gelation concentration is formed.

Benefits of technology

The calcium sensitivity range of LM amidated pectin has been expanded, enabling it to gel at a wider range of calcium concentrations and maintain stability in both liquid and solid forms during heating and cooling, making it suitable for the needs of various food and beverage products.

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Abstract

The present invention relates to a composition comprising pectin and water and a method for preparing the composition. Specifically, the present invention relates to a composition comprising pectin and water wherein the gelation temperature (Tg) changes from 0.5 DEG C to 2.5 DEG C when the pectin concentration in the water increases from 0.8% by weight to 1.4% by weight relative to the total weight of the composition. The composition has properties useful for the food and / or beverage industry.
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Description

[0001] Cross-reference to related applications

[0002] This application claims the benefit of European Patent Application No. 23167025.8, filed on 6 April 2023, which is incorporated herein by reference in its entirety. Technical Field

[0003] This invention relates to a composition comprising pectin and water, and a method for preparing the composition. The composition has properties useful to the food and / or beverage industry. Background Technology

[0004] Pectin is naturally found in plant cell walls. While it can be extracted from a wide variety of plants and fruits, its main industrial or conventional sources include citrus peels and apple pomace. The primary uses of pectin are as a gelling agent, thickener, viscous agent, and / or stabilizer in food. Therefore, pectin is commonly used as a food additive in jams, jellies, acidic dairy beverages, and dessert bases. Pectin also serves as dietary fiber and an effective food emulsifier. Pectin has potential uses in other areas, such as in the pharmaceutical field as a controlled drug or bioactive release carrier, and also in many other non-food applications.

[0005] Pectin is a polysaccharide consisting of galacturonic acid unit chains linked by α-1,4 glycosidic bonds. The galacturonic acid chains can be partially esterified to methyl esters. Although the galacturonic acid chain is the main chain of pectin, other chemical groups such as acetyl and methyl ester groups can still be bound to it. These groups are important for distinguishing different types of pectin. For a review of the properties and characteristics of pectin, see the article "Structure-related gels of pectin and their linkages with other natural compounds: a review" by D. Gawkowska et al., *Polymers (Basel)*, July 2018, 10(7):762. The full text of this article is incorporated herein by reference.

[0006] Pectin can be classified into two categories based on its degree of methylation, which refers to the percentage of carboxyl groups that have undergone esterification with methanol. The degree of methylation is important for the use of pectin as a gelling agent, and based on the degree of methylation, pectin is classified as high-methoxyl pectin (HM pectin) or low-methoxyl pectin (LM pectin). If more than 50% of the carboxyl groups are methylated, the pectin is HM pectin; if the degree of methylation is lower than this percentage, the pectin is LM pectin.

[0007] HM pectin is the most commonly used pectin and can be divided into two categories: fast-setting HM pectin and slow-setting HM pectin. Fast-setting pectin has a faster setting speed and a higher setting temperature than slow-setting pectin. Therefore, fast-setting pectin is more suitable for the production of food and / or beverage products that generally require a specific mouthfeel or require the suspension of various particulate matter such as whole fruits, fruit pieces, nuts, etc. Slow-setting pectin is more suitable for food and / or beverage products that do not require the presence of suspended particulate matter. HM pectin can form a gel with sugar and acid, which is referred to in the art as a low-water-activity gel or a sugar-acid pectin gel. Slow-setting pectin can take 1 to 2 days to set into a gel. These gels have a three-dimensional network of pectin molecules in which solvent, typically water, is optionally immobilized with the cosmotropic solutes sugar and acid, forming a system that can resist deformation.

[0008] LM pectin differs from HM pectin in that LM pectin only requires the presence of divalent cations to initiate the reaction that causes the pectin to set into a gel. The most commonly used divalent cation is calcium ion. Generally, the gel-forming ability of LM pectin is enhanced as the degree of methylation is reduced.

[0009] In recent years, LM pectin has been amidated to form LM amidated pectin. LM amidated pectin is a modified form of LM pectin in which some of the galacturonic acid units are converted to carboxylic acid amides by ammonia. In the traditional method of producing LM amidated pectin, HM pectin is first extracted from its natural source. The HM pectin is converted to LM pectin, which is amidated to form LM amidated pectin. The conversion of HM pectin to LM amidated pectin follows the following reaction scheme:

[0010] RCOOCH3+ NH4OH => RCONH2+ CH3OH + H2O

[0011] Known methods of forming LM amidated pectin are set out in US2480710A, EP1517925 and WO98 / 58968A1, the disclosures of which are hereby incorporated by reference in their entirety.

[0012] LM amidated pectin has advantages over non-amidated LM pectin because it is able to expand the calcium sensitivity tolerance range of LM pectin, and thus, unlike non-amidated LM pectin, it can gel over a wider range of calcium concentrations. Further advantageously, amidated pectin is generally heat reversible: LM amidated pectin can be formed into a liquid by heating and solidifies again upon cooling, whereas conventional pectin-gels will remain in liquid form upon heating and cooling. Further advantageously, LM amidated pectin can promote the stabilization of junction zones of the pectin gel network structure by forming additional hydrogen bonds with the amide groups. Further advantageously, LM amidated pectin shows good gelling properties under low sugar conditions.

[0013] Due to the many advantages of LM amidated pectin, LM amidated pectin is commonly used in the food and / or beverage industry. Thus, there is a continuing need for improved pectins and compositions comprising the same that can be used in the food and / or beverage industry. In particular, there is a continuing need for improved LM amidated pectins and compositions comprising the same that can be used in the food and / or beverage industry. SUMMARY

[0014] The present invention relates to a composition comprising pectin and water and a method of making the composition. The composition has properties useful in the food and / or beverage industry.

[0015] Representative features of the present invention are set forth in the following clauses, which can exist individually or can be combined in any combination with one or more features disclosed in the text and / or drawings of the specification.

[0016] The present invention is as described in the following clauses:

[0017] 1. A composition having a gelation temperature (Tg), the composition comprising:

[0018] pectin; and

[0019] water;

[0020] wherein the gelation temperature (Tg) changes by 0.5 °C to 2.5 °C when the concentration of pectin in the water increases from 0.8 wt% to 1.4 wt% relative to the total weight of the composition.

[0021] 2. The composition of clause 1, wherein the gelation temperature (Tg) changes by 0.50 °C to 2.0 °C, or 0.75 °C to 1.5 °C, or 1.0 °C to 1.3 °C, or 1.03 °C to 1.27 °C when the concentration of the pectin in the water increases from 0.8 wt% to 1.4 wt% relative to the total weight of the composition.

[0022] 3. The composition of clause 1 or clause 2, wherein the pectin has a degree of esterification (DE) of 15% to 45%, or 18% to 40%, or 20% to 35%, or 23% to 31%, or 23.3% to 31.0%.

[0023] 4. The composition of any one of clauses 1 to 3, wherein the pectin has a degree of amidation (DA) of 5% to 30%, or 12% to 25%, or 15% to 23%, or 16.0% to 22.1%.

[0024] 5. The composition of any one of clauses 1-4, wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, or 0.85 to 2.5, or 0.95 to 2.0, or 1.05 to 1.94.

[0025] 6. The composition of any one of clauses 1-5, wherein the gelation temperature changes by 1.27 °C when the pectin concentration in the water increases from 0.8 wt% to 1.4 wt% relative to the total weight of the composition.

[0026] 7. The composition of clause 6, wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.94.

[0027] 8. The composition of any one of clauses 1-5, wherein the gelation temperature changes by 1.03 °C when the pectin concentration in the water increases from 0.8 wt% to 1.4 wt% relative to the total weight of the composition.

[0028] 9. The composition of clause 8, wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.05.

[0029] 10. The composition of any one of clauses 1-9, wherein the pectin is a low methoxyl (LM) amidated pectin; optionally, wherein the low methoxyl (LM) amidated pectin has a degree of methylation below 50%.

[0030] 11. The composition of any one of clauses 1-10, wherein the degree of esterification (DE) is measured by titration; and / or, wherein the degree of amidation (DA) is measured by titration; and / or, wherein the gelation temperature (Tg) is measured by dynamic oscillatory rheometry.

[0031] 12. A pectin, the pectin having:

[0032] a degree of esterification (DE) of 15% to 45%, or 18% to 40%, or 20% to 35%, or 23% to 31%, or 23.3% to 31%;

[0033] a degree of amidation (DA) of 5% to 30%, or 12% to 25%, or 15% to 23%, or 16% to 22.1%; and

[0034] a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, or 0.85 to 2.5, or 0.95 to 2.0, or 1.05 to 1.94.

[0035] 13. A composition having a critical gel concentration (Co), the composition comprising:

[0036] pectin; and

[0037] water; and

[0038] wherein the critical gel concentration (Co) is from 0.01 wt% to 0.2 wt%.

[0039] 14. The composition of clause 13, wherein the critical gel concentration (Co) is from 0.02 wt% to 0.17 wt%, or from 0.025 wt% to 0.15 wt%, or from 0.04 wt% to 0.13 wt%, or from 0.05 wt% to 0.12 wt%.

[0040] 15. The composition of clause 13 or clause 14, wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) from 0.75 to 3.0, or from 0.85 to 2.5, or from 0.95 to 2.0, or from 1.05 to 1.94.

[0041] 16. The composition of any one of clauses 13 to 15, wherein:

[0042] the critical gel concentration (Co) is 0.12 wt%; optionally,

[0043] wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.94.

[0044] 17. The composition of any one of clauses 13 to 15, wherein:

[0045] the critical gel concentration (Co) is 0.05 wt%; optionally,

[0046] wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.05.

[0047] 18. The composition of any one of clauses 13 to 17, wherein the pectin is a low methoxyl (LM) amidated pectin; optionally, wherein the low methoxyl (LM) amidated pectin has a degree of methylation below 50%.

[0048] 19. The composition of any one of clauses 13 to 18, wherein the degree of esterification (DE) is measured by titration; and / or, wherein the degree of amidation (DA) is measured by titration; and / or, wherein the critical gel concentration (Co) is measured by dynamic oscillatory rheometry.

[0049] 20. A composition having a gelation temperature (Tg) and a critical gel concentration (C0), the composition comprising:

[0050] pectin; and

[0051] water;

[0052] wherein the gelation temperature (Tg) changes by 0.5°C to 2.5°C when the pectin concentration in the water increases from 0.8% to 1.4% by weight relative to the total weight of the composition; and

[0053] wherein the critical gel concentration (C0) is 0.01% to 0.2% by weight.

[0054] 21. The composition of clause 20, wherein the gelation temperature (Tg) changes by 0.50°C to 2.0°C, or 0.75°C to 1.5°C, or 1.0°C to 1.3°C, or 1.03°C to 1.27°C when the pectin concentration in the water increases from 0.8% to 1.4% by weight relative to the total weight of the composition.

[0055] 22. The composition of clause 20 or clause 21, wherein the critical gel concentration (C0) is 0.02% to 0.17% by weight, or 0.025% to 0.15% by weight, or 0.04% to 0.13% by weight, or 0.05% to 0.12% by weight.

[0056] 23. The composition of any one of clauses 20 to 22, wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, or 0.85 to 2.5, or 0.95 to 2.0, or 1.05 to 1.94.

[0057] 24. The composition of any one of clauses 20 to 23, wherein the pectin is a low methoxyl (LM) amidated pectin; optionally, wherein the low methoxyl (LM) amidated pectin has a degree of methylation below 50%.

[0058] 25. The composition of any one of clauses 20 to 24, wherein the degree of esterification (DE) is measured by titration; and / or, wherein the degree of amidation (DA) is measured by titration; and / or, wherein the gelation temperature (Tg) and / or the critical gel concentration (C0) is measured by dynamic oscillatory rheometry.

[0059] 26. The composition of any one of clauses 1 to 25, wherein the pectin is derived from apple pomace and / or citrus peel.

[0060] 27. The composition of any one of clauses 1-26, wherein the composition further comprises a sugar, optionally,

[0061] wherein the sugar is any one of sucrose, dextrose, lactose, maltose, glucose, and / or galactose; optionally,

[0062] wherein the sugar is present at 20-60%, or 30-50%, or 35-45%, or 40% by weight relative to the total weight of the composition.

[0063] 28. A method of making the composition of any one of clauses 1-27, the method comprising the steps of:

[0064] obtaining high methoxyl (HM) pectin in an aqueous form from a natural source;

[0065] drying the high methoxyl (HM) pectin in the aqueous form to form dried high methoxyl (HM) pectin, wherein the dried high methoxyl (HM) pectin has a moisture content of 10% by weight of the total weight of the dried high methoxyl (HM) pectin;

[0066] placing the dried high methoxyl (HM) pectin in a suspension comprising an alcohol and ammonia to form amidated low methoxyl (LM) pectin;

[0067] drying the amidated low methoxyl (LM) pectin to form dried amidated low methoxyl (LM) pectin, wherein the dried amidated low methoxyl (LM) pectin has a moisture content of 10% by weight of the total weight of the dried amidated low methoxyl (LM) pectin;

[0068] adding water to the amidated low methoxyl (LM) pectin to form a composition.

[0069] 29. The method of clause 28, wherein the natural source is any one of apple, apple pomace, citrus peel, lemon, Chinese citron, grapefruit, sweet orange, pomelo, Clementine, lime, kumquat, bitter orange, blood orange, seedless honey tangerine, yubari, tangelo, or any combination thereof.

[0070] 30. The method of clause 28 or clause 29, wherein the natural source is apple pomace or citrus peel.

[0071] 31. The method of any one of clauses 28-30, further comprising any one or more of the following steps:

[0072] clarifying the aqueous form of high methoxyl (HM) pectin; optionally, wherein the aqueous form of high methoxyl (HM) pectin is clarified by centrifugation and / or filtration;

[0073] concentrating the aqueous form of high methoxyl (HM) pectin;

[0074] washing the aqueous form of high methoxyl (HM) pectin with an alcohol;

[0075] subjecting the aqueous form of high methoxyl (HM) pectin to a separation process; optionally, wherein the separation process is mechanical separation;

[0076] filtering the amidated low methoxyl (LM) pectin;

[0077] washing the amidated low methoxyl (LM) pectin with an alcohol; and / or

[0078] adjusting the pH of the amidated low methoxyl (LM) pectin.

[0079] 32. Use of the composition according to any one of clauses 1 to 27 in a food and / or beverage product.

[0080] 33. A pectin having:

[0081] an esterification degree (DE) of 15% to 45%;

[0082] an amidation degree (DA) of 5% to 30%; and

[0083] a ratio of esterification degree (DE) to amidation degree (DA) of 0.5 to 9.0.

[0084] 34. The pectin according to clause 33 having a galacturonic acid content (GalA) of 85% or more, or 90% or more, or 85% to 95%, or 88% to 94%, or 93.0%.

[0085] 35. The pectin according to clause 33 having a galacturonic acid content (GalA) of 75% or less, or 70% or less, or 65% or less, or 60% or less, or 50% to 75%, or 55% to 65%, or 57% to 61%, or 59.0%.

[0086] 36. The pectin according to any one of clauses 33 to 35, wherein:

[0087] the esterification degree (DE) is 18% to 40%, or 20% to 35%, or 23% to 31%, or 23.3% to 31.0%;

[0088] the degree of amide formation (DA) is 12% to 25%, or 15% to 23%, or 16.0% to 22.1%; and / or

[0089] wherein the ratio of the degree of esterification (DE) to the degree of amide formation (DA) is 0.75 to 3.0, or 0.85 to 2.5, or 0.95 to 2.0, or 1.05 to 1.94.

[0090] 37. The pectin of clause 33, clause 34, or clause 36, wherein:

[0091] the degree of esterification (DE) is 15% to 28%, or 19% to 26%, or 21% to 25%, or 22% to 24%, or 23.3%;

[0092] the degree of amide formation (DA) is 5% to 30%, or 10% to 25%, or 20% to 23%, or 22.1%; and / or,

[0093] the ratio of the degree of esterification (DE) to the degree of amide formation (DA) is 0.5 to 1.5, or 0.75 to 1.25, or 0.9 to 1.1, or 1.05;

[0094] wherein the pectin has a galacturonic acid content (GalA) of 85% or more, or 90% or more, or 85% to 95%, or 88% to 94%, or 93.0%.

[0095] 38. The pectin of clause 37, wherein:

[0096] the degree of esterification (DE) is 23.3%,

[0097] the degree of amide formation (DA) is 22.1%, and

[0098] the ratio of the degree of esterification (DE) to the degree of amide formation (DA) is 1.05; and

[0099] the galacturonic acid content (GalA) is 93.0%.

[0100] 39. The pectin of clause 37 or clause 38, wherein the pectin is derived from citrus peel.

[0101] 40. The pectin of clause 33, clause 35, or clause 36, wherein:

[0102] the degree of esterification (DE) is 25% to 35%, or 30% to 32%, or 31.0%;

[0103] the degree of amide formation (DA) is 10% to 20%, or 12.5% to 17.5%, or 16.0%.

[0104] the ratio of the degree of esterification (DE) to the degree of amidation (DA) is 1.75 to 2.25, or 1.8 to 2.1, or 1.9 to 2.0, or 1.94; and / or,

[0105] wherein the pectin has a galacturonic acid content (GalA) of 75% or less, or 70% or less, or 65% or less, or 60% or less, or 50% to 75%, or 55% to 65%, or 57% to 61%, or 59.0%.

[0106] 41. The pectin according to Clause 40, wherein:

[0107] the degree of esterification (DE) is 31.0%,

[0108] the degree of amidation (DA) is 16.0%,

[0109] the ratio of the degree of esterification (DE) to the degree of amidation (DA) is 1.94; and

[0110] the galacturonic acid content (GalA) is 59.0%.

[0111] 42. The pectin according to Clause 40 or Clause 41, wherein the pectin is derived from apple pomace.

[0112] 43. The pectin according to any one of Clauses 33 to 42, wherein the degree of esterification (DE) is measured by titration; and / or, wherein the degree of amidation (DA) is measured by titration; and / or, wherein the galacturonic acid content (GalA) is measured by titration.

[0113] 44. The pectin according to any one of Clauses 33 to 43, wherein the pectin is a low methoxyl (LM) amidated pectin, optionally, wherein the low methoxyl amidated pectin has a degree of methylation of less than 50%.

[0114] 45. Use of the pectin according to any one of Clauses 33 to 44 in a food and / or beverage product;

[0115] optionally, wherein the food and / or beverage product is a dairy product, a confectionery product, a low sugar jam product, a fruit product, and an icing.

[0116] 46. A method of making the pectin according to any one of Clauses 33 to 44, the method comprising the steps of:

[0117] obtaining a high methoxyl (HM) pectin in an aqueous form from a natural source;

[0118] drying the high methoxyl (HM) pectin in the aqueous form to form dried high methoxyl (HM) pectin, wherein the dried high methoxyl (HM) pectin has a moisture content of 10% by weight of the total weight of the dried high methoxyl (HM) pectin;

[0119] placing the dried high methoxyl (HM) pectin in a suspension comprising an alcohol and ammonia to form amidated low methoxyl (LM) pectin; and

[0120] drying the amidated low methoxyl (LM) pectin to form pectin;

[0121] Optionally, the method further comprises any one or more of the following steps:

[0122] clarifying the high methoxyl (HM) pectin in the aqueous form; optionally, wherein the high methoxyl (HM) pectin in the aqueous form is clarified by centrifugation and / or filtration;

[0123] concentrating the high methoxyl (HM) pectin in the aqueous form;

[0124] washing the high methoxyl (HM) pectin in the aqueous form with an alcohol;

[0125] subjecting the high methoxyl (HM) pectin in the aqueous form to a separation process; optionally, wherein the separation process is a mechanical separation;

[0126] filtering the amidated low methoxyl (LM) pectin;

[0127] washing the amidated low methoxyl (LM) pectin with an alcohol; and / or

[0128] adjusting the pH of the amidated low methoxyl (LM) pectin.

[0129] 47. A composition comprising:

[0130] pectin; and

[0131] water;

[0132] wherein the pectin is the pectin of any one of clauses 33 to 44;

[0133] Optionally, the composition further comprises a sugar,

[0134] Optionally, the sugar is any one of sucrose, dextrose, lactose, maltose, glucose and / or galactose;

[0135] Optionally, wherein the sugar is present at 20% to 60% by weight, or 30% to 50% by weight, or 35% to 45% by weight, or 40% by weight of the total weight of the composition.

[0136] 48. Use of the composition according to Clause 47 in a food and / or beverage product;

[0137] Optionally, wherein the food and / or beverage product is a dairy product.

[0138] 49. A method of making the composition according to Clause 47, the method comprising:

[0139] providing pectin;

[0140] combining the pectin with water to form a composition;

[0141] wherein the pectin is the pectin according to any one of Clauses 33 to 44;

[0142] Optionally, wherein the composition comprises pectin at a concentration of 0.001% to 10% by weight relative to the total amount of pectin and water, or 0.01% to 7.5% by weight relative to the total amount of pectin and water, or 0.1% to 5% by weight relative to the total amount of pectin and water, or 0.2% to 3% by weight relative to the total amount of pectin and water, or 0.3% to 2.5% by weight relative to the total amount of pectin and water, or 0.4% to 2% by weight relative to the total amount of pectin and water. BRIEF DESCRIPTION OF DRAWINGS

[0143] Figure 1 Flow chart of the method for producing the pectin according to the application from dry HM pectin.

[0144] Figure 2 Graph of the storage modulus (G’) and loss modulus (G”) of the composition comprising pectin and water according to the application (the analysed composition is Composition 1).

[0145] Figure 3 Graph of the storage modulus (G’) versus concentration (C) of the composition comprising pectin and water according to the application (the analysed composition is Composition 1). DETAILED DESCRIPTION

[0146] Embodiments of the present application are described below with reference to the accompanying drawings. The figures show various embodiments of systems, methods, and embodiments of various other aspects of the present disclosure. Those of ordinary skill in the art will appreciate that the boundaries between the elements of the figures are not meant to be absolute and that one element can be designed as multiple elements or that multiple elements can be designed as one element. In some examples, elements shown as internal components of one element can be implemented as external components of another element, or vice versa. Further, elements can not be drawn to scale. Non-limiting and non-exhaustive descriptions are described with reference to the following figures. Components in the figures are not necessarily drawn to scale, but emphasis is placed on illustrating principles.

[0147] Embodiments of the present disclosure will be described more fully hereinafter with reference to the accompanying drawings, in which like numerals refer to 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.

[0148] The words “comprise,” “has,” “contain” and “include,” and other forms thereof, are meant to be interpreted in an inclusive sense and are used inclusively, as opposed to an exclusive or exhaustive sense, since any one or more of the items listed after any form of these words are not meant to be an exhaustive listing of one or more items that the statement that the item precedes is including. Additionally, the phrase “consisting essentially of’ will be understood to include those elements specifically listed, and additional elements that do not materially affect the basic and novel characteristics of the application. The phrase “consisting of’ excludes any unspecified element. It must also be noted that, as used in the specification and the appended claims, the singular form “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.

[0149] As used herein, the terms “for example,” “e.g.,” “such as,” or “including” set off a list of one or more items, factors, or aspects that are explained in further detail below. None of these examples are intended to be limiting in any way, unless otherwise specified.

[0150] As used herein, “about” will be understood by those of ordinary skill in the art and will vary to some extent depending upon the context in which it is used. If the term “about” is used in reference to a particular value, it is meant to encompass minor fluctuations of that value as would be understood by one of ordinary skill in the art, considering the context in which the term is used. If the use of the term “about” in reference to a particular value is not clear to one of ordinary skill in the art, given the context of the term, “about” will mean up to positive or negative 10% of that particular value.

[0151] Also, it is to be understood that the phraseology or terminology employed herein, and not otherwise defined, is for the purpose of description only and is not of limitation on the scope of the present application. Any use of section headings is intended to aid reading the document and is not to be interpreted as limiting; information that is relevant to a section heading can occur within or outside of that particular section. If any document incorporated by reference contradicts any disclosure contained in the present document, the disclosure contained in the present document will control.

[0152] Some terms used to describe the present application are listed below:

[0153] "Amidation" refers to the modification of pectin to include at least one amide group (-NH2).

[0154] "Critical gelling concentration" refers to the lowest concentration of a substance in a solvent at which the substance is able to form a gel. A typical example is a composition comprising pectin (i.e. the substance) in water (i.e. the solvent), with or without additives (such as, but not limited to, sugars as defined herein below). The critical gelling concentration depends on the molecular properties (such as, but not limited to, the degree of esterification (DE) and / or the degree of amidation (DA)) and on the environmental conditions (such as, but not limited to, the nature of the solvent, the ionic strength, the type of salts present and the pH).

[0155] "Composition" refers to a mixture of at least two components. The mixture can be a solution, a suspension or a dispersion.

[0156] "Degree of amidation" (DA) refers to the percentage of carboxyl groups that have become amides. Theoretically, the degree of amide groups can range from 0% to 100%. Preferably, the degree of amidation of the pectin is between 5% and 30%. The degree of amidation can be measured by titration, an example of such a method being set forth in EP 1517925, the disclosure of which is hereby incorporated by reference in its entirety.

[0157] "Degree of esterification" (DE) refers to the percentage of carboxyl groups that have undergone an esterification reaction. Theoretically, the degree of esterification can range from 0% to 100%. The degree of esterification is also known in the art as the degree of methylesterification or methylation (DM). The degree of esterification can be measured by titration, an example of such a method being set forth in EP 1294920 and EP 1171473, the disclosures of which are hereby incorporated by reference in their entirety.

[0158] "Methylation degree" refers to the percentage of carboxyl groups that have been esterified with methanol. If more than 50% of the carboxyl groups have been methylated, the pectin is referred to as high methoxyl pectin (HM); if the degree of methylation is lower than this proportion, the pectin is referred to as low methoxyl pectin (LM).

[0159] "High methoxyl pectin" or "HM pectin" means a pectin extracted from citrus fruit peels, wherein a certain degree of the original carboxyl groups present in the pectin have been esterified with methanol. High methoxyl pectin has a degree of methylation higher than 50%.

[0160] "Low methoxyl pectin" or "LM pectin" means a pectin extracted from citrus fruit peels, wherein a certain degree of the original carboxyl groups present in the pectin have been esterified with methanol. Low methoxyl pectin has a degree of methylation lower than 50%.

[0161] "Homogeneous" means that a substance as a whole has a uniform composition. For example, a homogeneous substance does not present a gradient of a particular property (e.g. concentration) of more than 1% by weight of the calculated property. According to the present application, the composition can comprise a pectin, wherein the pectin is homogeneous (i.e. the composition comprises only one type of pectin). In this context, one type of pectin is understood as meaning that the pectin used according to the present application is obtained from a single pectin source and has a specific degree of amidation and a specific degree of esterification.

[0162] "Low methoxyl amidated pectin" or "LM amidated pectin" or "LMA pectin" means a modified form of LM pectin, wherein some or at least some of the methoxyl groups are converted to carboxyl amides with ammonia. Preferably, the LM amidated pectin has a degree of amidation of 5% to 30%.

[0163] "Blend" or "mixture" means a substance containing two or more different components, while the term "mixing" means the method step in which the blend or mixture is formed.

[0164] "Pectin" means an anionic, water-soluble plant cell wall polysaccharide comprising chains of galacturonic acid units, which are linked by a-1,4 glycosidic bonds. The galacturonic acid chains are partially esterified, i.e. the galacturonic acid chains contain methyl ester groups. Other chemical groups such as acetyl groups can be bound into the galacturonic acid chains and can be of importance for distinguishing different pectin types.

[0165] "Pectin gel" means a sample containing a three-dimensional (3-D) network of pectin molecules. Pectin gels are the result of long stretches of pectin polymer chains associating into conformationally ordered junction zones stabilized by an array of non-covalent interactions. Pectin gels possess both the viscous properties of a liquid and the elastic properties of a solid, i.e. they are viscoelastic materials. Pectin gels are known to the person skilled in the art for decades, e.g. see the document "Chapter 11 - Rheology of pectin dispersions and gels" ("Pectin Chemistry and Technology", "Food Science and Technology", 1991, pages 227-250, ISBN 978-0-08-092644-5) by M.A.V. Axelos, the disclosure of which is hereby incorporated by reference in its entirety.

[0166] "Gelation temperature" (Tg) refers to the temperature at which a material undergoes a reversible thermal gelation, i.e. below which the material is soluble in water and above which the material undergoes a phase transition resulting in an increase in viscosity or formation of a semi-solid gel. For example, for a gelling polysaccharide such as pectin, the gelation temperature (Tg) refers to the temperature at which a solution containing pectin changes from a liquid to a gel.

[0167] Composition

[0168] The compositions according to the presently described application have various desirable properties, such properties making these compositions useful in various food and beverage products.

[0169] Composition: gelation temperature

[0170] The composition comprises pectin and water.

[0171] The pectin is present in the composition in an amount of 0.001 wt% to 10 wt% relative to the total amount of pectin and water, preferably 0.01 wt% to 7.5 wt% relative to the total amount of pectin and water, more preferably 0.1 wt% to 5 wt% relative to the total amount of pectin and water, even more preferably 0.2 wt% to 3 wt% relative to the total amount of pectin and water, even more preferably 0.3 wt% to 2.5 wt% relative to the total amount of pectin and water, most preferably 0.4 wt% to 2 wt% relative to the total amount of pectin and water.

[0172] The composition has a gelation temperature (Tg) wherein the gelation temperature (Tg) changes between 0.5°C to 2.5°C, preferably 0.5°C to 2.0°C, more preferably 0.75°C to 1.5°C, even more preferably 1.0°C to 1.3°C, most preferably 1.03°C to 1.27°C when the pectin concentration in water is increased from 0.8 wt% to 1.4 wt% relative to the total amount of pectin and water. Preferably, the gelation temperature (Tg) changes between 1.03°C to 1.27°C when the pectin concentration in water is increased from 0.8 wt% to 1.4 wt% relative to the total amount of pectin and water.

[0173] The pectin in the composition preferably has a degree of esterification (DE) of 15% to 45%, more preferably 18% to 40%, even more preferably 20% to 35%, even more preferably 23% to 31%, most preferably 23.3% to 31.0%.

[0174] The pectin in the composition has a degree of amidation (DA) of 5% to 30%, more preferably 12% to 25%, even more preferably 15% to 23%, most preferably 16.0% to 22.1%.

[0175] The pectin in the composition can have a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, most preferably 1.05 to 1.94.

[0176] Preferably, the pectin in the composition has a degree of esterification (DE) of 15% to 45%, more preferably 18% to 40%, even more preferably 20% to 35%, even more preferably 23% to 31%, most preferably 23.3% to 31.0%; a degree of amidation (DA) of 5% to 30%, more preferably 12% to 25%, even more preferably 15% to 23%, most preferably 16.0% to 22.1%; and a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, most preferably 1.05 to 1.94. More preferably, the pectin in the composition has a degree of esterification (DE) of 23.3% to 31%, a degree of amidation (DA) of 16.0% to 22.1%, and a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.05 to 1.94.

[0177] The pectin can be derived from any one of: apple, apple pomace, citrus fruit, citrus peel, lemon, mandarin, grapefruit, sweet orange, pomelo, clementine, lime, kumquat, bitter orange, blood orange, seedless honey tangerine, yubari king mandarin, tangelo, or any combination thereof.

[0178] The composition can comprise apple pectin, for example pectin extracted from apple pomace. The composition can comprise apple pectin and water, and when the concentration of pectin in the water is increased from 0.8% by weight to 1.4% by weight relative to the total amount of pectin and water, the gelation temperature is 1.27°C. Preferably, the pectin also has a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.9 to 2.0, preferably 1.94. Preferably, all of the amount of pectin present in the composition is apple pectin.

[0179] The composition can comprise citrus pectin, for example pectin extracted from citrus fruit (e.g., citrus peel). The composition can comprise citrus pectin and water, and when the concentration of pectin in the water is increased from 0.8% by weight to 1.4% by weight relative to the total amount of pectin and water, the gelation temperature is 1.03°C. Preferably, the pectin also has a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.00 to 1.10, preferably 1.05. Preferably, all of the amount of pectin present in the composition is citrus pectin.

[0180] The degree of esterification and the degree of amidation can be measured by titration techniques.

[0181] The pectin in the composition can be homogenized.

[0182] The composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source selected from the group consisting of: apple, apple pomace, citrus fruit, citrus peel, lemon, Chinese citron, grapefruit, sweet orange, grapefruit, Clementine, lime, kumquat, bitter orange, blood orange, seedless honey tangerine, Japanese grapefruit, tangelo, or any combination thereof.

[0183] Preferably, the composition consists of pectin and water, preferably wherein the pectin is uniformly distributed in the water.

[0184] The pectin in the composition can be amidated. Preferably, the pectin in the composition can be LM amidated pectin.

[0185] The composition can comprise sugar. The sugar can be, but is not necessarily limited to, sucrose, dextrose, lactose, maltose, glucose, and / or galactose. Preferably, the sugar is sucrose. Preferably, the composition comprises 20% to 60%, more preferably 30% to 50%, even more preferably 35% to 45%, most preferably 40% by weight of the total weight of the composition of sugar.

[0186] The composition can further comprise a gel promoting medium and / or a buffer.

[0187] Preferably, wherein the gel promoting medium comprises citric acid monohydrate, trisodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate, and water. Preferably, wherein the citric acid monohydrate is present in 300g to 350g, more preferably in 320g to 330g, most preferably in 325.598g. Preferably, wherein the trisodium citrate dihydrate is present in 150g to 200g, more preferably in 160g to 170g, most preferably in 167.493g. Preferably, wherein the sodium benzoate is present in 0.5g to 10g, more preferably in 3g to 7g, most preferably in 5g. Preferably, wherein the calcium chloride dihydrate is present in 0.5g to 10g, more preferably in 4g to 8g, most preferably in 6.2g. Preferably, wherein the distilled water is present in 4000g to 5000g, more preferably in 4400g to 4600g, most preferably in 4495.709g. Preferably, wherein the citric acid monohydrate is present in 325.598g, the trisodium citrate dihydrate is present in 167.493g, the sodium benzoate is present in 5g, the calcium chloride dihydrate is present in 6.2g, and the distilled water is present in 4495.709g.

[0188] Preferably, wherein the buffer comprises sodium citrate and water. Preferably, the buffer contains sodium citrate such that the pH of the buffer is 3 to 4, more preferably 3.2 to 3.6, most preferably 3.4.

[0189] Preferably, the composition has a gelation temperature (Tg) wherein the gelation temperature (Tg) changes from 0.5°C to 2.5°C when the pectin concentration increases from 0.8% to 1.4% by weight relative to the total amount of pectin and water; and wherein the composition further comprises a gel promoting medium and a buffer; wherein the gel promoting medium comprises citric acid monohydrate, citric acid trisodium dihydrate, sodium benzoate, calcium chloride dihydrate, and water; and wherein the buffer comprises sodium citrate and water.

[0190] Composition: critical gel concentration

[0191] The composition comprises pectin and water.

[0192] The pectin is present in the composition in an amount of 0.001% to 10% by weight relative to the total amount of pectin and water, preferably 0.01% to 7.5% by weight relative to the total amount of pectin and water, more preferably 0.1% to 5% by weight relative to the total amount of pectin and water, even more preferably 0.2% to 3% by weight relative to the total amount of pectin and water, even more preferably 0.3% to 2.5% by weight relative to the total amount of pectin and water, most preferably 0.4% to 2% by weight relative to the total amount of pectin and water.

[0193] The composition has a critical gel concentration (C0) of 0.01% to 0.2% by weight, preferably 0.02% to 0.17% by weight, more preferably 0.025% to 0.15% by weight, even more preferably 0.04% to 0.13% by weight, most preferably 0.05% to 0.12% by weight.

[0194] The pectin in the composition preferably has a degree of esterification (DE) of 15% to 45%, more preferably 18% to 40%, even more preferably 20% to 35%, even more preferably 23% to 31%, most preferably 23.3% to 31.0%.

[0195] The pectin in the composition has a degree of amidation (DA) of 5% to 30%, more preferably 12% to 25%, even more preferably 15% to 23%, most preferably 16.0% to 22.1%.

[0196] The pectin in the composition can have a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, even most preferably 1.05 to 1.94.

[0197] Preferably, the pectin in the composition has a degree of esterification (DE) of 15% to 45%, more preferably 18% to 40%, even more preferably 20% to 35%, even more preferably 23% to 31%, most preferably 23.3% to 31.0%; a degree of amidation (DA) of 5% to 30%, more preferably 12% to 25%, even more preferably 15% to 23%, most preferably 22.1% to 16.0%; and a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, most preferably 1.05 to 1.94. More preferably, the pectin in the composition has a degree of esterification (DE) of 23.3% to 31%, a degree of amidation (DA) of 16.0% to 22.1%, and a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.05 to 1.94.

[0198] Preferably, the composition can comprise pectin and water, wherein the critical gel concentration (C0) is 0.05% to 0.12% by weight, and preferably wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.05 to 1.94.

[0199] The pectin can be derived from any one of: apples, apple pomace, citrus fruits, citrus peels, lemons, mandarins, grapefruits, sweet oranges, pummelos, Clementines, limes, kumquats, bitter oranges, blood oranges, seedless tangerines, Japanese pummelos, tangelos, or any combination thereof.

[0200] The composition can comprise apple pectin, such as pectin extracted from apple pomace. The composition can comprise apple pectin and water, wherein the critical gel concentration (C0) is 0.12% by weight, and preferably wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.94. Preferably, all of the amount of pectin present in the composition is apple pectin.

[0201] The composition can comprise citrus pectin, such as pectin extracted from citrus fruits (e.g., citrus peels). The composition can comprise citrus pectin and water, wherein the critical gel concentration (C0) is 0.05% by weight, and preferably wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.05. Preferably, all of the amount of pectin present in the composition is citrus pectin.

[0202] The degree of esterification and the degree of amidation can be measured by titration techniques.

[0203] The pectin in the composition can be homogenized.

[0204] The composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source selected from the group consisting of: apple, apple pomace, citrus fruit, citrus peel, lemon, mandarin, grapefruit, sweet orange, pomelo, clementine, lime, kumquat, bitter orange, blood orange, seedless honey tangerine, shaddock, tangelo, or any combination thereof.

[0205] Preferably, the composition consists of pectin and water, preferably wherein the pectin is uniformly distributed in the water.

[0206] The pectin in the composition can be amidated. Preferably, the pectin in the composition can be LM amidated pectin.

[0207] The composition can comprise sugar. The sugar can be, but is not necessarily limited to, sucrose, dextrose, lactose, maltose, glucose, and / or galactose. Preferably, the sugar is sucrose. Preferably, the composition comprises 20% to 60%, preferably 30% to 50%, more preferably 35% to 45%, most preferably 40% by weight of the total weight of the composition.

[0208] The composition can further comprise a gel promoting medium and / or a buffer.

[0209] Preferably, wherein the gel promoting medium comprises citric acid monohydrate, trisodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate, and water. Preferably, wherein the citric acid monohydrate is present in 300g to 350g, more preferably in 320g to 330g, most preferably in 325.598g. Preferably, wherein the trisodium citrate dihydrate is present in 150g to 200g, more preferably in 160g to 170g, most preferably in 167.493g. Preferably, wherein the sodium benzoate is present in 0.5g to 10g, more preferably in 3g to 7g, most preferably in 5g. Preferably, wherein the calcium chloride dihydrate is present in 0.5g to 10g, more preferably in 4g to 8g, most preferably in 6.2g. Preferably, wherein the distilled water is present in 4000g to 5000g, more preferably in 4400g to 4600g, most preferably in 4495.709g. Preferably, wherein the citric acid monohydrate is present in 325.598g, the trisodium citrate dihydrate is present in 167.493g, the sodium benzoate is present in 5g, the calcium chloride dihydrate is present in 6.2g, and the distilled water is present in 4495.709g.

[0210] Preferably, wherein the buffer comprises sodium citrate and water. Preferably, the buffer contains sufficient sodium citrate such that the pH of the buffer is 3 to 4, more preferably 3.2 to 3.6, most preferably 3.4.

[0211] Preferably, the composition has a critical gelling concentration (C0), wherein the critical gelling concentration (C0) changes by 0.01 wt% to 0.2 wt%, wherein the composition further comprises a gelling promoting medium and a buffer; wherein the gelling promoting medium comprises citric acid monohydrate, citric acid trisodium dihydrate, sodium benzoate, calcium chloride dihydrate, and water; and wherein the buffer comprises sodium citrate and water.

[0212] Composition: gelation temperature and critical gel concentration

[0213] The composition comprises pectin and water.

[0214] The pectin is present in the composition in an amount of 0.001 wt% to 10 wt% relative to the total amount of pectin and water, preferably 0.01 wt% to 7.5 wt% relative to the total amount of pectin and water, more preferably 0.1 wt% to 5 wt% relative to the total amount of pectin and water, even more preferably 0.2 wt% to 3 wt% relative to the total amount of pectin and water, even more preferably 0.3 wt% to 2.5 wt% relative to the total amount of pectin and water, most preferably 0.4 wt% to 2 wt% relative to the total amount of pectin and water.

[0215] The composition has a gelling temperature (Tg) and a critical gelling concentration (C0), wherein the gelling temperature (Tg) changes by 0.5°C to 2.5°C, preferably 0.5°C to 2.0°C, more preferably 0.75°C to 1.5°C, even more preferably 1.0°C to 1.3°C, most preferably 1.03°C to 1.27°C, when the pectin concentration increases from 0.8 wt% to 1.4 wt% relative to the total amount of pectin and water; and wherein the critical gelling concentration (C0) is 0.01 wt% to 0.2 wt%, preferably 0.02 wt% to 0.17 wt%, more preferably 0.025 wt% to 0.15 wt%, even more preferably 0.04 wt% to 0.13 wt%, most preferably 0.05 wt% to 0.12 wt%.

[0216] Preferably, the composition can have a gelling temperature (Tg) and a critical gelling concentration (C0), wherein the gelling temperature (Tg) changes by 1.03°C to 1.27°C when the pectin concentration increases from 0.8 wt% to 1.4 wt% relative to the total amount of pectin and water, and wherein the critical gelling concentration (C0) is 0.05 wt% to 0.12 wt%.

[0217] The pectin in the composition preferably has a degree of esterification (DE) of 15% to 45%, more preferably 18% to 40%, even more preferably 20% to 35%, even more preferably 23% to 31%, most preferably 23.3% to 31.0%.

[0218] The pectin in the composition has a degree of amidation (DA) of 5% to 30%, more preferably 12% to 25%, even more preferably 15% to 23%, most preferably 16.0% to 22.1%.

[0219] The pectin in the composition can have a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, even most preferably 1.05 to 1.94.

[0220] Preferably, the pectin in the composition has a degree of esterification (DE) of 15% to 45%, more preferably 18% to 40%, even more preferably 20% to 35%, even more preferably 23% to 31%, most preferably 23.3% to 31.0%; a degree of amidation (DA) of 5% to 30%, more preferably 12% to 25%, even more preferably 15% to 23%, most preferably 16.0% to 22.1%; and, a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, most preferably 1.05 to 1.94. More preferably, the pectin in the composition has a degree of esterification (DE) of 23.3% to 31%, a degree of amidation (DA) of 16.0% to 22.1%, and a ratio of degree of esterification (DE) to degree of amidation (DA) of 1.05 to 1.94.

[0221] The pectin can be derived from any one of: apple, apple pomace, citrus fruit, citrus peel, lemon, mandarin, grapefruit, sweet orange, pomelo, clementine, lime, kumquat, bitter orange, blood orange, seedless honey tangerine, Japanese pomelo, tangelo, or any combination thereof.

[0222] The degree of esterification and the degree of amidation can be measured by titration techniques.

[0223] The pectin in the composition can be homogenized.

[0224] The composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source selected from the group consisting of: apple, apple pomace, citrus fruit, citrus peel, lemon, mandarin, grapefruit, sweet orange, pomelo, clementine, lime, kumquat, bitter orange, blood orange, seedless honey tangerine, Japanese pomelo, tangelo, or any combination thereof.

[0225] Preferably, the composition consists of pectin and water, preferably wherein the pectin is uniformly distributed in the water.

[0226] The pectin in the composition can be amidated. Preferably, the pectin in the composition can be LM amidated pectin.

[0227] The composition can comprise a sugar. The sugar can be, but is not necessarily limited to, sucrose, dextrose, lactose, maltose, glucose and / or galactose. Preferably, the sugar is sucrose. Preferably, the composition comprises 20 to 60 wt%, preferably 30 to 50 wt%, more preferably 35 to 45 wt%, most preferably 40 wt% of the total weight of the composition.

[0228] The composition can further comprise a gel promoting medium and / or a buffer.

[0229] Preferably, wherein the gel promoting medium comprises citric acid monohydrate, trisodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water. Preferably, wherein the citric acid monohydrate is present in an amount of 300 to 350 g, more preferably in an amount of 320 to 330 g, most preferably in an amount of 325.598 g. Preferably, wherein the trisodium citrate dihydrate is present in an amount of 150 to 200 g, more preferably in an amount of 160 to 170 g, most preferably in an amount of 167.493 g. Preferably, wherein the sodium benzoate is present in an amount of 0.5 to 10 g, more preferably in an amount of 3 to 7 g, most preferably in an amount of 5 g. Preferably, wherein the calcium chloride dihydrate is present in an amount of 0.5 to 10 g, more preferably in an amount of 4 to 8 g, most preferably in an amount of 6.2 g. Preferably, wherein the distilled water is present in an amount of 4000 to 5000 g, more preferably in an amount of 4400 to 4600 g, most preferably in an amount of 4495.709 g. Preferably, wherein the citric acid monohydrate is present in an amount of 325.598 g, the trisodium citrate dihydrate is present in an amount of 167.493 g, the sodium benzoate is present in an amount of 5 g, the calcium chloride dihydrate is present in an amount of 6.2 g, and the distilled water is present in an amount of 4495.709 g.

[0230] Preferably, wherein the buffer comprises sodium citrate and water. Preferably, the buffer contains sufficient sodium citrate such that the pH of the buffer is 3 to 4, more preferably 3.2 to 3.6, most preferably 3.4.

[0231] Preferably, the composition has a gelation temperature (Tg) and a critical gel concentration (C0), wherein the gelation temperature (Tg) changes by 0.5 to 2.5 °C when the pectin concentration increases from 0.8 to 1.4 wt% relative to the total amount of pectin and water; wherein the critical gel concentration (C0) is 0.01 to 0.2 wt%; wherein the composition further comprises a gel promoting medium and a buffer; wherein the gel promoting medium comprises citric acid monohydrate, trisodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate and water; and wherein the buffer comprises sodium citrate and water.

[0232] Composition as a pectin gel

[0233] The composition listed under the heading "Composition" can be in the form of a pectin gel. The pectin gels according to the presently described application have various desirable properties, such properties making these pectin gels useful in various food and beverage products.

[0234] The pectin gel comprises a composition as listed under the heading "Composition", i.e. the pectin gel comprises water and pectin.

[0235] The pectin is present in the pectin gel in an amount of 0.001 wt% to 10 wt% relative to the total amount of the pectin gel, preferably 0.01 wt% to 7.5 wt% relative to the total amount of the pectin gel, more preferably 0.1 wt% to 5 wt% relative to the total amount of the pectin gel, even more preferably 0.2 wt% to 3 wt% relative to the total amount of the pectin gel, even more preferably 0.3 wt% to 2.5 wt% relative to the total amount of the pectin gel, most preferably 0.4 wt% to 2 wt% relative to the total amount of the pectin gel.

[0236] The pectin gel can further comprise an additional material, which is but not limited to sucrose, glucose, fructose, ribose, glyceraldehyde, lactose, maltose, glycerol, erythritol, sorbitol, xylitol, mannitol, lactitol, maltitol, or any combination thereof. Preferably, the pectin gel comprises 20 wt% to 60 wt%, preferably 30 wt% to 50 wt%, more preferably 35 wt% to 45 wt%, most preferably 40 wt% of the additional material relative to the total weight of the pectin gel.

[0237] The pectin gel can further comprise a flavorant, a colorant, a preservative, etc. The pectin gel can comprise a gel promoting medium, such as but not limited to calcium.

[0238] The pectin gel can comprise one or more water immiscible materials dispersed throughout the pectin gel. Preferably, the water immiscible material is dispersed in the gel in the form of an emulsion. Preferably, the water immiscible material is a volatile organic component, such as an oil, or a water immiscible organic oil, or an aqueous base. Preferably, the water immiscible material is but not limited to a fragrance, a flavorant, a pheromone, a fungicide, an insect attractant, an insect repellent, a veterinary attractant, a veterinary repellent, an insecticide, a fungicide, a pharmaceutical, a veterinary drug, other volatile oils or organic materials, or any combination thereof.

[0239] Process for preparing pectin

[0240] Another aspect of the application relates to a method of preparing a pectin. In particular, this aspect of the application relates to a method of preparing an LM amidated pectin.

[0241] In this method of preparing pectin, HM pectin is first extracted from citrus peel or apple pomace. Then, the extracted HM pectin is amidated to form LM amidated pectin.

[0242] Figure 1 A flowchart of Method 1 is depicted.

[0243] Step 1 : extraction of HM pectin from natural pectin source

[0244] First, a natural pectin source is mixed with acidic hot water, and HM pectin is extracted from the natural pectin source in aqueous form according to the methods described in other literature, such as Endreb, H.-U. and Christensen, S. H. 2020. Pectin. In: G. O. Philips and P. A. Williams (eds.), Handbook of hydrocolloids, 3rd edition, pp. 274-297. Cambridge: Woodhead Publishing, the disclosure of which is hereby incorporated by reference in its entirety. Typically, the natural pectin source is a raw material extracted from fruit.

[0245] In this method, the natural pectin source can be fruit, such as apple, apple pomace, pear, plum, guava, aronia, currant, and citrus fruit, such as citrus peel, lemon, mandarin, grapefruit, sweet orange, pomelo, Clementine, lime, kumquat, bitter orange, blood orange, seedless honey tangerine, yubari, tangelo, or any combination thereof. Preferably, the fruit extract is derived from apple pomace and / or citrus peel.

[0246] Preferably, the temperature of the acidic hot water is 60 °C to 80 °C, or 65 °C to 75 °C, or 68 °C to 72 °C.

[0247] Preferably, the pH of the acidic hot water is pH 1 to 2, or pH 1.25 to 1.95, or pH 1.4 to 1.8, or pH 1.45 to 1.75, or pH 1.50 to 1.70.

[0248] Preferably, the residence time of the fruit extract in the acidic hot water is 1 hour to 20 hours, or 6 hours to 14 hours, or 7 hours to 13 hours, or 8 hours to 12 hours.

[0249] Preferably, the temperature of the acidic hot water is 68 °C to 72 °C, the pH of the acidic hot water is pH 1.50 to 1.70, and the residence time of the fruit extract in the acidic hot water is 8 hours to 12 hours.

[0250] Then, the aqueous form of HM pectin can be clarified using centrifugation, filtration, or other conventional separation techniques known in the art to obtain the clarified aqueous form of HM pectin.

[0251] The clarified aqueous form of HM pectin can then be concentrated to form a concentrated aqueous form of HM pectin using any technique known in the art.

[0252] An alcohol can be added to the concentrated aqueous form of HM pectin to precipitate the HM extract in the form of a HM pectin-containing precipitate. The amount of alcohol added depends on the amount of alcohol required to precipitate the clarified HM extract from its aqueous form in the form of a HM pectin-containing precipitate.

[0253] Preferably, the alcohol used is one or more of isopropyl alcohol, tertiary amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, t-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutyl alcohol, isopropyl alcohol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanediol, propan-1-ol, propylene glycol, propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropyl alcohol.

[0254] The HM pectin-containing precipitate can be separated from the alcohol / water mixture. Preferably, the HM pectin-containing precipitate is separated from the alcohol / water mixture by mechanical separation, wherein any mechanical separation known in the art can be used.

[0255] The HM pectin-containing precipitate obtained from the separation is washed with an alcohol to form a washed HM pectin-containing precipitate.

[0256] Preferably, the alcohol used is one or more of isopropyl alcohol, tertiary amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, t-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutyl alcohol, isopropyl alcohol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanediol, propan-1-ol, propylene glycol, propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropyl alcohol.

[0257] Preferably, the HM amidated pectin-containing precipitate obtained from the separation is washed with an alcohol one, two, three, four, five, six, seven, eight, nine, ten, or more than ten times. Preferably, the HM amidated pectin is washed with an alcohol three times.

[0258] Preferably, the precipitate containing HM amidated pectin obtained from the separation is washed with an alcohol in an amount of 50% to 70% by weight, or 55% to 65% by weight, or 60% by weight of the total weight of the alcohol to form a washed HM pectin.

[0259] Preferably, the alcohol used is one or more of the following: isopropyl alcohol, t-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butantriol, butanol, 1-butanol, 2-butanol, t-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutyl alcohol, isopropyl alcohol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanediol, propan-1-ol, propylene glycol, propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropyl alcohol.

[0260] The washed HM pectin can then undergo a drying step to form a dried HM pectin. The drying step dries the washed HM pectin until the washed HM pectin has a moisture content of 5% to 15% by weight, or 7.5% to 12.5% by weight, or 10% by weight of the total weight of the dried HM pectin. Preferably, the drying step is performed by hot air drying. The product of the drying step is a dried HM pectin.

[0261] The dried HM pectin can be milled until a uniform particle size distribution is obtained. The dried HM pectin can be blended with sugar to form a standardized HM pectin.

[0262] To make the product of the first step a pectin of the present invention, the parameters of the above process need to be strictly controlled.

[0263] Step 2: amidation of dried HM pectin

[0264] The dried HM pectin can be placed in a suspension comprising an alcohol and ammonia to form an amidated LM pectin.

[0265] Preferably, the alcohol used is one or more of the following: isopropyl alcohol, t-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butantriol, butanol, 1-butanol, 2-butanol, t-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutyl alcohol, isopropyl alcohol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanediol, propan-1-ol, propylene glycol, propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropyl alcohol.

[0266] Preferably, the alcohol is present at 50% to 80% by weight, or 55% to 75% by weight, or 60% to 70% by weight, of the total weight of the suspension. Preferably, the alcohol is present at 60% to 70% by weight of the total weight of the suspension.

[0267] Preferably, the ammonia is present at 2% to 4% by weight, or 2.5% to 3.75% by weight, or 2.8% to 3.5% by weight, of the total weight of the suspension. Preferably, the ammonia is present at 2.8% to 3.5% by weight of the total weight of the suspension.

[0268] Preferably, the temperature of the suspension is maintained at 5°C to 20°C, or 8°C to 16°C, or 9°C to 15°C, or 10°C to 14°C. Preferably, the temperature of the suspension is maintained at 10°C to 14°C.

[0269] Preferably, the dry HM pectin is maintained in the suspension for 3 hours to 10 hours, or 4 hours to 9 hours, or 5 hours to 8 hours. Preferably, the dry HM pectin is maintained in the suspension for 5 hours to 8 hours.

[0270] Preferably, the alcohol is present at 60% to 70% by weight of the total weight of the suspension, the ammonia is present at 2.8% to 3.5% by weight of the total weight of the suspension, the temperature of the suspension is maintained at 10°C to 14°C, the dry HM pectin is maintained in the suspension for 5 hours to 8 hours, and the alcohol used is isopropanol.

[0271] The LM amidated pectin can be filtered from the suspension to produce a filtrate comprising the alcohol and a residue comprising the LM amidated pectin. The LM amidated pectin can be filtered from the suspension by any filtration technique known in the art.

[0272] Preferably, the filtrate comprising the alcohol and the ammonia is passed to a recovery step.

[0273] Preferably, the residue comprising the LM amidated pectin is washed with an alcohol to form washed LM amidated pectin. Preferably, the residue comprising the LM amidated pectin is washed with an alcohol. Preferably, the residue comprising the LM amidated pectin is washed with an alcohol that is 50% to 70%, or 55% to 65%, or 60% by weight of the total weight of the alcohol. Preferably, the alcohol used is isopropyl alcohol. Preferably, the alcohol used is one or more of: isopropyl alcohol, t-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, t-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutyl alcohol, isopropyl alcohol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanediol, propan-1-ol, propylene glycol, propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropyl alcohol.

[0274] Preferably, the pH of the washed LM amidated pectin is adjusted until the pH is 3.0 to 5.5, or 3.5 to 4.0, or 4.0 to 4.5.

[0275] Preferably, the pH of the washed LM amidated pectin is adjusted with an acid to form pH-adjusted LM amidated pectin. Preferably, the acid is nitric acid.

[0276] The pH-adjusted LM amidated pectin can be washed with an alcohol to form twice-washed LM amidated pectin.

[0277] Preferably, the alcohol is one or more of: t-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, t-butyl alcohol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutyl alcohol, isopropyl alcohol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentyl alcohol, 2-pentanol, 1,3-propanediol, propan-1-ol, propylene glycol, propylene glycol methyl ether, isopropyl alcohol, or any combination thereof. Preferably, the alcohol is isopropyl alcohol.

[0278] Preferably, the neutralized LM amidated pectin is washed with an alcohol one, two, three, four, five, six, seven, eight, nine, ten, or more than ten times. Preferably, the neutralized LM amidated pectin is washed with an alcohol three times.

[0279] Preferably, the pH-adjusted LM amidated pectin is washed with an alcohol that is 50% to 70%, or 55% to 65%, or 60% by weight of the total weight of the alcohol.

[0280] The second washed LM amidated pectin can be subjected to a drying step to form a dried LM amidated pectin.

[0281] Preferably, the drying step is performed by hot air drying.

[0282] Preferably, the second washed LM amidated pectin can be dried until the dried LM amidated pectin has a moisture content of 1% to 30%, or 2% to 20%, or 7.5% to 15.0%, or 9% to 11%, or 10% by weight of the total weight of the dried LM amidated pectin.

[0283] The dried LM amidated pectin is the LM amidated pectin ready for use in the composition according to the present application. The dried LM amidated pectin can be blended with sugar to form a standardised LM amidated pectin.

[0284] In order for the product of the second step to be a pectin according to the present application, some key parameters of the above process need to be controlled in the amidation reaction. The parameters include the % by weight of alcohol and ammonia in the suspension, the residence time of the HM pectin in the suspension and the temperature of the suspension. By controlling these parameters, the desired degree of esterification and degree of amidation can be obtained.

[0285] Preferably, the % by weight of ammonia in the suspension is 2.8% to 3.5% by weight of the total weight of the suspension. Preferably, the % by weight of alcohol in the suspension is 60% to 70% by weight of the total weight of the suspension. Preferably, the residence time is kept at 5 hours to 8 hours. Preferably, the reaction temperature is kept at 10°C to 14°C. Preferably, the % by weight of ammonia in the suspension is 2.8% to 3.5% by weight of the total weight of the suspension, the % by weight of alcohol in the suspension is 60% to 70% by weight of the total weight of the suspension, the residence time is kept at 5 hours to 8 hours and the reaction temperature is kept at 10°C to 14°C.

[0286] Process for preparing a composition comprising pectin

[0287] Another aspect of the present application relates to a method of preparing a composition, wherein the composition comprises pectin and water. The method of preparing the composition comprises the steps of:

[0288] (a) providing pectin;

[0289] (b) combining the pectin with water to form the composition.

[0290] The composition can comprise pectin in a concentration of 0.001 wt% to 10 wt% relative to the total amount of pectin and water, preferably 0.01 wt% to 7.5 wt% relative to the total amount of pectin and water, more preferably 0.1 wt% to 5 wt% relative to the total amount of pectin and water, even more preferably 0.2 wt% to 3 wt% relative to the total amount of pectin and water, even more preferably 0.3 wt% to 2.5 wt% relative to the total amount of pectin and water, most preferably 0.4 wt% to 2 wt% relative to the total amount of pectin and water.

[0291] The composition can further comprise a gel promoting medium in a concentration of 0.001 mM to 10 mM, preferably 0.005 mM to, most preferably 0.01 mM to 8 mM. Preferably, the gel promoting medium is calcium.

[0292] Preferably, the composition comprises pectin in a concentration of 0.4 wt% to 2 wt% relative to the total weight of the composition and calcium (as gel promoting medium) in a concentration of 0.01 mM to 8 mM.

[0293] The composition can further comprise a sugar. The composition can comprise a sugar in a concentration of 20 wt% to 60 wt%, or 30 wt% to 50 wt%, or 35 wt% to 45 wt%, or 40 wt% relative to the total weight of the composition. Preferably, the sugar is, but is not limited to, sucrose, dextrose, lactose, maltose, glucose and / or galactose.

[0294] Process for preparing a composition as a pectin gel

[0295] Another aspect of the present application relates to a method of preparing a pectin gel, wherein the pectin gel comprises a composition as listed under the heading "Composition", i.e. wherein the pectin gel comprises pectin and water. The method of preparing the pectin gel comprises the following steps:

[0296] (a) combining pectin, a gel promoting medium and water to form a solution;

[0297] (b) heating the solution until the pectin and the gel promoting medium are dissolved;

[0298] (c) cooling the pectin solution to form a gel.

[0299] Preferably, the concentration of pectin is 0.001 wt% to 10 wt% of the total weight of the pectin gel, preferably 0.01 wt% to 7.5 wt% of the total weight of the pectin gel, more preferably 0.1 wt% to 5 wt% of the total weight of the pectin gel, even more preferably 0.2 wt% to 3 wt% of the total weight of the pectin gel, even more preferably 0.3 wt% to 2.5 wt% of the total weight of the pectin gel, most preferably 0.4 wt% to 2 wt% of the total weight of the pectin gel. Preferably, the concentration of the gel promoting medium is 0.001 mM to 10 mM, preferably 0.005 mM to 9 mM, most preferably 0.01 mM to 8 mM. Preferably, the gel promoting medium is calcium. Preferably, the concentration of pectin is 0.4 wt% to 2 wt% of the total weight of the pectin gel and the concentration of the gel medium cation is 0.01 mM to 8 mM.

[0300] Preferably, the solution is heated to 70°C to 110°C, preferably 75°C to 105°C, most preferably 80°C to 95°C. Preferably, the solution is heated for 1 minute to 60 minutes, preferably 5 minutes to 45 minutes, most preferably 10 minutes to 30 minutes. Preferably, the solution is heated to 80°C to 95°C for 10 minutes to 30 minutes.

[0301] Preferably, the solution is cooled to a temperature of 1°C to 30°C, preferably 5°C to 25°C, most preferably 10°C to 20°C.

[0302] Composition in a food or beverage product

[0303] Another aspect of the present application relates to a composition in a food or beverage product, wherein the composition is as listed under the heading "Composition".

[0304] The composition can be incorporated into a dairy product including, but not limited to, milk, condensed milk, dry milk powder, milk beverage, cheese, butter, yogurt, cottage cheese, egg nog, farmer's cheese, cream cheese, curd, frozen dairy products such as frozen egg nog, frozen yogurt, and ice cream, gelato, milk powder, sweetened condensed milk, sour cream, yogurt, whey, whey protein, or crème fraiche.

[0305] The composition can be incorporated into a sweetened product including, but not limited to, confectionery products, low sugar jams, fruit preparations, jellies, icings, and glazes.

[0306] Preferably, the composition is incorporated into a meat product, a poultry product, a fish product, a dairy product (such as milk, ice cream, yogurt, cheese, pudding, and flavored dairy drinks), a baked good (such as bread, cake, cookie, cracker, biscuit, pie, donut, pretzel, and potato chip), a non-dairy spread, mayonnaise, soup, sauce, dressing, condiment, frozen confection, fruit preparation, jam and jelly, beverage, hydrogel, gummy candy, or low-fat spread.

[0307] Composition in a non-food or non-beverage product

[0308] Another aspect of the present application relates to a composition in a non-food or non-beverage product, wherein the composition is as listed under the heading "Composition".

[0309] The composition can be incorporated into other products related to nutraceuticals, bioactives, cosmetics, and pharmaceuticals.

[0310] Process for producing a composition in a food or beverage product

[0311] Another aspect of the present application relates to a method of making a food or beverage product comprising a composition, wherein the composition is as listed under the heading "Composition". The method of making a food or beverage product comprises the steps of:

[0312] (a) providing a composition; and

[0313] (b) combining the composition with at least one food or beverage product.

[0314] Process for producing a composition in a non-food or non-beverage product

[0315] Another aspect of the present application relates to a method of making a non-food or non-beverage product comprising a composition, wherein the composition is as listed under the heading "Composition". The method of making a non-food or non-beverage product comprises the steps of:

[0316] (a) providing a composition; and

[0317] (b) combining the composition with at least one non-food or non-beverage product.

[0318] Example

[0319] The following are non-limiting examples of the advantages of the present application discussed with reference to the tables and figures. The examples set forth herein are merely examples of many possible examples.

[0320] Materials used in the example

[0321] A novel pectin was prepared according to the method listed in Example 1.

[0322] The novel pectin was compared to commercially available pectins provided by Cargill, Incorporated.

[0323] The pectin samples are listed in Table 1.

[0324] Table 1 : Pectin samples used for the evaluation of the present invention .

[0325]

[0326] The composition of the commercially available pectins is listed in Table 2.

[0327] Table 2: Composition of commercial pectins .

[0328]

[0329]

[0330] wherein GalA is the galacturonic acid (GalA) content of each pectin.

[0331] Example 1 : Extraction of LM amidated pectin

[0332] Step 1 : extraction of HM pectin

[0333] First, the citrus peels or apple pomace were mixed in acidic hot water to extract the HM pectin from the citrus peels or apple pomace as an aqueous form of HM pectin. The acidic hot water had a temperature of 68°C to 72°C, a pH of pH 1.50 to 1.70, and a residence time of 8 hours to 12 hours.

[0334] Centrifugation was used to clarify the aqueous form of HM pectin and it was filtered to form a clarified aqueous form of HM pectin.

[0335] The clarified aqueous form of HM pectin was then concentrated to form a concentrated aqueous form of HM pectin.

[0336] Isopropyl alcohol was added to the concentrated aqueous form of HM pectin to precipitate the HM extract as a precipitate containing HM pectin. The precipitate containing HM pectin was present in an alcohol (isopropyl alcohol) / water mixture.

[0337] The precipitate containing HM pectin was separated from the alcohol / water mixture by mechanical separation.

[0338] The precipitate containing HM pectin obtained from the separation was then washed three times with 60 wt% isopropyl alcohol based on the total weight of the alcohol to form a washed HM pectin.

[0339] The washed HM pectin then undergoes a drying step to form dried HM pectin. The drying step dries the washed HM pectin-containing precipitate until the washed HM pectin-containing precipitate has a moisture content of 10% by weight of the total weight of the dried HM pectin.

[0340] Step 2: amidation of dried HM pectin

[0341] The dried HM pectin is placed in a suspension comprising alcohol (isopropyl alcohol) and ammonia. The alcohol is present in 60% to 70% by weight of the total weight of the suspension and the ammonia is present in 2.8% to 3.5% by weight of the total weight of the suspension. The temperature of the suspension is maintained at 10°C to 14°C. The dried HM pectin is maintained in the suspension for 5 hours to 8 hours. Once 5 hours to 8 hours have elapsed, the dried HM pectin has undergone amidation to form LM amidated pectin.

[0342] To prevent further reactions from occurring in the suspension, the LM amidated pectin is filtered from the alcohol and ammonia. The alcohol and ammonia are passed to a recovery step. The LM amidated pectin is washed with 60% by weight of isopropyl alcohol of the total weight of the alcohol to form washed LM amidated pectin.

[0343] The pH of the washed LM amidated pectin is adjusted to form pH-adjusted LM amidated pectin. The pH of the washed LM amidated pectin is adjusted until the pH is between 4.0 to 4.5. The pH is adjusted with nitric acid.

[0344] The pH-adjusted LM amidated pectin is washed with isopropyl alcohol three times to form twice-washed LM amidated pectin.

[0345] The twice-washed LM amidated pectin undergoes a drying step to form dried twice-washed LM amidated pectin. The drying step dries the twice-washed LM amidated pectin until the twice-washed LM amidated pectin has a moisture content of 10% by weight of the total weight of the dried twice-washed LM amidated pectin.

[0346] Example 2: structural characterization of LM amidated pectin

[0347] In this non-limiting embodiment of the application, the degree of esterification (DE), degree of amidation (DA), and galacturonic acid content (GalA) of the pectin is determined using a titration method (such as the method set forth in National Research Council, 1981, Yu et al., 2021, the disclosures of which are hereby incorporated by reference in their entireties). The method of measuring the degree of esterification (DE), degree of amidation (DA), and galacturonic acid content (GalA) includes washing the pectin sample with acidified aqueous isopropanol to remove any cations, salts, and standardizing sugars. The purified pectin is then titrated with 0.1 M sodium hydroxide. The ester groups are saponified with an excess of 0.5 M sodium hydroxide, which is then neutralized with an exact equivalent amount of 0.5 M hydrochloric acid, such that the released acid groups can be titrated by 0.1 M sodium hydroxide. The solution can then be distilled with a strong base to release ammonia from the amide groups of the amidated pectin. The ammonia is determined by a back-titration procedure with the same 0.1 M sodium hydroxide. After titration, the degree of amidation, degree of esterification, and galacturonic acid content are calculated according to the methods described in National Research Council, 1981, Yu et al., 2021, the disclosures of which are hereby incorporated by reference in their entireties.

[0348] The degree of amidation, degree of esterification, and galacturonic acid content of the LM amidated pectin is shown in Table 3.

[0349] Table 3: Chemical composition of pectin .

[0350]

[0351] Example 3: measurement of intrinsic viscosity of LM amidated pectin

[0352] In this non-limiting embodiment of the application, the intrinsic viscosity of the pectin is determined by size exclusion chromatography - multi-angle laser light scattering (SEC-MALLS) as described in Hellin, P., Ralet, M. C., Bonnin, E., and Thibault, J.F. (2005). Homogalacturonans extracted from acid orange pectin show a homogeneous charge density and molar mass distribution. Carbohydrate Polymers, 60(3), 307-317, particularly page 309 (which discloses a method of determining the intrinsic viscosity of pectin), the disclosures of which are hereby incorporated by reference in their entireties.

[0353] A 5 mg / mL aqueous pectin solution was prepared in 50 mM sodium nitrate containing 0.02 wt% sodium azide as a preservative. Intrinsic viscosity was calculated using Astra software (Wyatt, Santa Barbara, CA, the disclosure of which is hereby incorporated by reference in its entirety) and TriSec software (version 3.0, Voscotek, Houston, TX, the disclosure of which is hereby incorporated by reference in its entirety). All analyses were repeated in triplicate, and the average was taken.

[0354] The average intrinsic viscosity of the pectins is shown in Table 4.

[0355] Table 4: Intrinsic viscosity of pectin .

[0356]

[0357] Example 4: preparation of a composition comprising LM amidated pectin and water

[0358] In this non-limiting example, individual compositions were prepared containing each of the pectins as shown in Table 1. The compositions contained pectin and water: each composition contained one of Pectin 1 through Pectin 5. The compositions were prepared so that the resulting pectin concentration was 0.4 wt% to 2.0 wt% of the total weight of the composition, with sucrose being 40 wt%.

[0359] To prepare each composition, a pectin pre-solution was first prepared by dissolving each pectin separately in distilled water at 90 °C with mechanical stirring for 10 minutes.

[0360] After the pectin was dissolved in distilled water, 190 g to 320 g of hot buffer and gelation promoting media was added to the distilled water and pectin solution.

[0361] The buffer contained sodium citrate at a sufficient concentration so that the pH of the buffer was 3.4. The sodium citrate was dissolved in distilled water. The buffer was heated to the same temperature as the distilled water and pectin solution (90 °C) before it was added to the distilled water and pectin solution. The buffer also contained CaCl2 (8.4 mM) and sucrose.

[0362] The gelation promoting media was added to the solution containing distilled water and pectin at a concentration of 8.4 mM of pectin in water. The composition of the gelation promoting media is listed in Table 5.

[0363] Table 5: gel promoting media .

[0364]

[0365] Corresponds to 5 liters of pH 3.4 buffer stock solution.

[0366] Advantageously, the ionic strength of the gel-promoting medium plays an important role on the gelation temperature and on the critical gel concentration. The higher the ionic strength of the gel-promoting medium, the higher the gelation temperature and the lower the critical gel concentration.

[0367] The resulting compositions, having a final calcium chloride (CaCl2) concentration of 3 mM, were kept under stirring (90°C) for 5 minutes. The final pH of each composition prepared was 3.4.

[0368] Table 6 shows which composition contains which pectin.

[0369] Table 6: pectin used for the preparation of each composition .

[0370]

[0371] Example 5: measurement of gelation temperature (Tg)

[0372] In this non-limiting example, the gelation temperature (Tg) of each composition was measured. For each composition, the gelation temperature (Tg) was measured over a pectin concentration range from 0.8% to 1.4% by weight (of the total weight of the composition).

[0373] The compositions analyzed were the ones prepared in Example 4.

[0374] To measure the gelation temperature (Tg) of each composition, dynamic oscillation (or small deformation) measurements were performed on each composition using an ARES-G2 strain controlled rheometer (TA Instruments) or an MCR 92 stress controlled rheometer (Anton Paar Physica), respectively. Both rheometers were equipped with a Couette device.

[0375] For these measurements, each composition (as described above in Example 4) was covered with a thin layer of paraffin oil to avoid evaporation during the measurements.

[0376] Before performing the measurements, each composition was poured (respectively) into the Couette device (pre-heated at 80°C) and a pre-shear (at 10 s -1 The viscoelastic experiments performed using the ARES-G2 strain controlled rheometer and the MCR 92 stress controlled rheometer were performed at a frequency of 0.8 Hz at a strain of 0.4% and 10%, respectively. It was verified that both strain amplitudes were within the LVE domain.

[0377] In all these small deformation experiments, each measurement was repeated three times using a new preparation of the composition (same composition). The average value was taken from the three repeated measurements.

[0378] After the end of the measurement, the gelation temperature (Tg) representing the cross-over point between the storage modulus (G') and the loss modulus (G") was collected from the gelation kinetics data obtained after the completion of the temperature sweep test (as described above). The automatic data export program of the Rheocompass software (from Anton Paar) was used to collect the storage modulus G' values and the loss modulus (G") values from the mechanical spectra. The cross-over point between the storage modulus (G') and the loss modulus (G") was determined as shown in Figure 2 Figure 2 The data points for composition 1 at a pectin concentration of 1.4% in water are shown. Then, the Tg average value and the corresponding standard deviation of the data obtained from the triplicate measurements were calculated.

[0379] The measurements were then repeated for each composition (separately).

[0380] The average values of the gelation temperature (Tg) measurements are shown in Table 7.

[0381] Table 7: average value of the gelation temperature (Tg) for each composition .

[0382]

[0383] Example 6: measurement of critical gel concentration (C0)

[0384] In this non-limiting example, the critical gel concentration of each composition was measured.

[0385] The compositions analyzed were those prepared in Example 4.

[0386] To measure the critical gel concentration, dynamic oscillation (or small deformation) measurements were performed using an ARES-G2 strain controlled rheometer (TA Instruments) or an MCR92 stress controlled rheometer (Anton Paar Physica). Both rheometers were equipped with a Couette device.

[0387] For these measurements, each composition prepared as described above was covered with a thin layer of paraffin oil to avoid evaporation during the measurements.

[0388] Before the measurements, each composition was (separately) poured into the Couette device (pre-heated at 80°C) and a pre-shear (at 10 s -1 ​The device was then subjected to a temperature sweep test (2°C / min) from 80°C to 10°C to clear the history of the load of the device. Each composition was then exposed to a temperature sweep test (2°C / min) from 80°C to 10°C, followed by a time sweep experiment at a frequency of 0.8 Hz for 30 minutes to ensure that the resulting gel was in an equilibrium state due to reorganization (structural rearrangement). To ensure that the viscoelastic measurements were performed in the LVE regime, a strain sweep experiment from 0.01% to 40% at 0.8 Hz was performed. The viscoelastic experiments performed using the ARES-G2 strain controlled rheometer and the MCR 92 stress controlled rheometer were performed at a strain of 0.4% and 10%, respectively. Both strain amplitudes were verified to be within the LVE regime.

[0389] In all these small deformation experiments, each measurement was repeated three times using a fresh preparation of the composition (same composition). The average was taken.

[0390] Then, the following steps were performed to determine C0:

[0391] (i) The storage modulus (G’) and loss modulus (G”) values were collected from the mechanical spectra using the automatic data export program of the Rheocompass software (from Anton Paar) and plotted as a function of the pectin concentration C (%) on a logarithmic scale, an example of such a plot is shown in Figure 3 , which shows the experimental data and the calculated data (the calculated data was obtained by using the equation G’ = 1700 (C - C0) 2.19 , as shown in Figure 3 ; Figure 3 The second equation (G’ = 1733.2 C 2.19 , R 2 = 0.9974) shown is a fitted model to the experimental data, where the exponential value reflects the structural level of the gel and R 2 is a statistical measure of fit, which indicates the proportion of the variation in the dependent variable that is explained by the independent values in the regression model: when R 2 is close to 1 (as it is in this case), the fitted model is robust);

[0392] (ii) The data was fitted using a power law relationship to obtain the equation G’ = kC n , where G’ is the storage modulus, k is a scaling factor, C (%) is the pectin concentration, and n is the exponential value (equations for the calculated data and experimental data are shown in step (i) above); and

[0393] (iii) the equation G' = kCn is fitted to the data by linear regression, as described in the literature (e.g. de Gennes, P.-G. (1979), Scaling Concepts in Polymer Physics, Cornell University Press: Ithaca, New York and London; Jones, J. L. and Marques, C. M. (1990), Model of a rigid polymer network, Physica A, 51, 1113-1127; Ross-Murphy, S. B. (1987) and Physical gelation of biological polymers, Food Hydrocolloids, 1, 485-495) the disclosures of which are hereby incorporated by reference in their entirety) and the critical gel concentration (C0) is determined as the intercept of the linear regression with the G' axis. n The mathematical transformation is G' = k'(C - C0) n Form. In this second equation, k' represents the scaling factor and C0represents the concentration below which no gel-like behaviour can be achieved.

[0394] Linear regression is performed on all the products studied, provided that G' = kCn n = k'(C - C0) n with the same value of the two exponents (n) and C > C0.

[0395] The validity of the critical gel concentration (C0) determined using the fitting model described above is then verified by evaluating the rheological behaviour of compositions 1, 2, 3, 4 and 5 under the same conditions.

[0396] The measurement is then repeated for each composition (separately). For each composition formulation, each measurement is repeated three times and the average is taken.

[0397] The average of the critical gel concentration (C0) measurements is shown in Table 8.

[0398] Table 8: average value of the critical gel concentration (C0) for each composition .

[0399]

[0400] Advantageously, a low critical gel concentration (C0) leads to a high functional product. The lower the critical gel concentration (C0) of a composition, the less of that composition is required to obtain a gel in a food and / or beverage product. The compositions of the present application have a low critical gel concentration (C0) and therefore less of the composition is required to obtain a gel in a food and / or beverage product. This property advantageously leads to a reduction in the cost of production of the food and / or beverage product as less of the composition is required in the food and / or beverage product.

[0401] Further advantageously, the lower the ratio of the degree of esterification (DE) to the degree of amidation (DA), the lower the critical gel concentration (C0).

[0402] Further advantageously, the above-mentioned advantages of the end-use product formulation contribute to new ways of identifying reasonable product formulations (thus reducing the cost of use) and to the continuous optimization of pectin processing conditions.

Claims

1. A composition having a gelation temperature (Tg), said composition comprising: Pectin; and water; When the pectin concentration in the water increases from 0.8% by weight to 1.4% by weight relative to the total weight of the composition, the gelation temperature (Tg) changes from 0.5°C to 2.5°C.

2. The composition according to claim 1, wherein when the pectin concentration in the water increases relative to the total weight of the composition from 0.8% by weight to 1.4% by weight, the gelation temperature (Tg) changes by 0.50°C to 2.0°C, or 0.75°C to 1.5°C, or 1.0°C to 1.3°C, or 1.03°C to 1.27°C; and / or The pectin described herein has a degree of esterification (DE) of 15% to 45%, or 18% to 40%, or 20% to 35%, or 23% to 31%, or 23.3% to 31.0%; and / or, The pectin described herein has a degree of amidation (DA) of 5% to 30%, or 12% to 25%, or 15% to 23%, or 16.0% to 22.1%; and / or, The pectin wherein the pectin has a ratio of degree of esterification (DE) to degree of amidation (DA) of 0.75 to 3.0, or 0.85 to 2.5, or 0.95 to 2.0, or 1.05 to 1.

94.

3. The composition according to claim 1 or claim 2, wherein the gelation temperature changes by 1.27°C when the pectin concentration in the water increases relative to the total weight of the composition from 0.8% by weight to 1.4% by weight; optionally, The pectin described therein has a ratio of esterification degree (DE) to amidation degree (DA) of 1.

94.

4. The composition according to claim 1 or claim 2, wherein the gelation temperature (Tg) changes by 1.03°C when the pectin concentration in the water increases relative to the total weight of the composition from 0.8% by weight to 1.4% by weight; optionally, The pectin described therein has a ratio of esterification degree (DE) to amidation degree (DA) of 1.

05.

5. The composition according to any one of claims 1 to 4, wherein the pectin is a low-methoxyl (LM) amidated pectin; optionally, wherein the low-methoxyl (LM) amidated pectin has a methylation degree of less than 50%; and / or, The degree of esterification (DE) is measured by titration; and / or the degree of amidation (DA) is measured by titration; and / or the gelation temperature (Tg) is measured by dynamic oscillatory rheology.

6. A pectin, said pectin having: Degree of esterification (DE) of 15% to 45%, or 18% to 40%, or 20% to 35%, or 23% to 31%, or 23.3% to 31%. Acidity of amidation (DA) of 5% to 30%, or 12% to 25%, or 15% to 23%, or 16% to 22.1%; and The ratio of degree of esterification (DE) to degree of amidation (DA) is 0.75 to 3.0, or 0.85 to 2.5, or 0.95 to 2.0, or 1.05 to 1.

94.

7. A composition having a critical gel concentration (C0), said composition comprising: Pectin; and Water; and The critical gel concentration (C0) is 0.01% to 0.2% by weight.

8. The composition according to claim 7, wherein the critical gel concentration (CO) is 0.02% to 0.17% by weight, or 0.025% to 0.15% by weight, or 0.04% to 0.13% by weight, or 0.05% to 0.12% by weight; and / or, The pectin wherein the degree of esterification (DE) to the degree of amidation (DA) is 0.75 to 3.0, or 0.85 to 2.5, or 0.95 to 2.0, or 1.05 to 1.94; and / or, in: The critical gel concentration (C0) is 0.12% by weight; optionally, The pectin described therein has a ratio of esterification degree (DE) to amidation degree (DA) of 1.94; or, in: The critical gel concentration (C0) is 0.05% by weight; optionally, The pectin described therein has a ratio of esterification degree (DE) to amidation degree (DA) of 1.

05.

9. The composition according to claim 7 or claim 8, wherein the pectin is a low-methoxyl (LM) amidated pectin; optionally, wherein the low-methoxyl (LM) amidated pectin has a methylation degree of less than 50%; and / or, The degree of esterification (DE) is measured by titration; and / or the degree of amidation (DA) is measured by titration; and / or the critical gel concentration (C0) is measured by dynamic oscillatory rheology.

10. A composition having a gelation temperature (Tg) and a critical gel concentration (C0), said composition comprising: Pectin; and water; When the pectin concentration in the water increases from 0.8% by weight to 1.4% by weight relative to the total weight of the composition, the gelation temperature (Tg) changes from 0.5°C to 2.5°C; and The critical gel concentration (C0) is 0.01% to 0.2% by weight.

11. The composition of claim 10, wherein when the pectin concentration in the water increases relative to the total weight of the composition from 0.8 wt% to 1.4 wt%, the gelation temperature (Tg) changes by 0.50°C to 2.0°C, or 0.75°C to 1.5°C, or 1.0°C to 1.3°C, or 1.03°C to 1.27°C; and / or, The critical gel concentration (C0) is 0.02 wt% to 0.17 wt%, or 0.025 wt% to 0.15 wt%, or 0.04 wt% to 0.13 wt%, or 0.05 wt% to 0.12 wt%; and / or, The pectin wherein the degree of esterification (DE) to the degree of amidation (DA) is 0.75 to 3.0, or 0.85 to 2.5, or 0.95 to 2.0, or 1.05 to 1.94; and / or, The pectin is a low-methoxyl (LM) amidated pectin; optionally, the low-methoxyl (LM) amidated pectin has a methylation degree of less than 50%; and / or, The degree of esterification (DE) is measured by titration; and / or the degree of amidation (DA) is measured by titration; and / or the gelation temperature (Tg) and / or the critical gel concentration (C0) are measured by dynamic oscillatory rheology.

12. The composition according to any one of claims 1 to 11, wherein the pectin is derived from apple pomace and / or citrus peel; and / or, The composition further comprises sugar, optionally, The sugar is any one of sucrose, dextrose, lactose, maltose, glucose, and / or galactose; optionally, The sugar is present in the composition at a weight of 20% to 60% by weight, or 30% to 50% by weight, or 35% to 45% by weight, or 40% by weight relative to the total weight of the composition.

13. A method for preparing a composition according to any one of claims 1 to 12, the method comprising the following steps: Obtain water-based high-methoxyl (HM) pectin from natural sources; The aqueous form of high methoxyl (HM) pectin is dried to form dried high methoxyl (HM) pectin, wherein the dried high methoxyl (HM) pectin has a water content of 10% by weight of the total weight of the dried high methoxyl (HM) pectin. The dried high-methoxyl (HM) pectin was placed in a suspension containing alcohol and ammonia to form amidated low-methoxyl (LM) pectin. The amidated low-methoxyl (LM) pectin is dried to form dried amidated low-methoxyl (LM) pectin, wherein the dried amidated pectin has a water content of 10% by weight of the total weight of the dried amidated low-methoxyl (LM) pectin. Water is added to the amidated low-methoxyl (LM) pectin to form a composition.

14. The method according to claim 13, wherein the natural source is any one of the following: apple, apple pomace, citrus peel, lemon, Chinese tangerine, grapefruit, sweet orange, pomelo, Clementine, lime, kumquat, bitter orange, blood orange, seedless mandarin orange, Japanese yuzu, citrus, or any combination thereof; and / or, The natural source mentioned above is apple pomace or citrus peel; and / or, The method further includes any one or more of the following steps: Clarify the aqueous form of high methoxyl (HM) pectin; optionally, wherein the aqueous form of high methoxyl (HM) pectin is clarified by centrifugation and / or filtration; Concentrate the aqueous form of high-methoxyl (HM) pectin; Wash the aqueous form of high-methoxyl (HM) pectin with alcohol; The aqueous form of high-methoxyl (HM) pectin is subjected to a separation process; optionally, the separation process is mechanical separation. Filter the amidated low-methoxyl (LM) pectin; Wash the amidated low-methoxyl (LM) pectin with alcohol; and / or Adjust the pH of the amidated low-methoxyl (LM) pectin.

15. Use of the composition according to any one of claims 1 to 12 in food and / or beverage products.

Citation Information

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