Amidated pectin

Abstract

The present invention relates to pectin, a composition comprising pectin and water and a method for preparing the composition. In particular, the present invention relates to a pectin having: a degree of esterification (DE) of 15% to 45%; a degree of amidation (DA) of from 5% to 30%; and a ratio of the degree of esterification (DE) to the degree of amidation (DA) of 0.5 to 9.0. The composition has properties useful in the food and / or beverage industry.

Description

[0001] Cross-references to related applications

[0002] This application claims the benefit of European Patent Application No. 23167020.9, filed on 6 April 2023, which is incorporated herein by reference in its entirety. Technical Field

[0003] This invention relates to compositions comprising pectin and water, and methods for preparing the compositions. The compositions possess properties suitable for use in the food and / or beverage industries. Background Technology

[0004] Pectin is naturally found in plant cell walls. Although it can be extracted from a wide variety of plants and fruits, major 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 as a stabilizer in food. Therefore, pectin is commonly used as a food additive in jams, jellies, acidic dairy beverages, and dessert bases. Pectin can also be used as dietary fiber and as an effective food emulsifier. Pectin also has potential uses in other areas, such as in the pharmaceutical field as a carrier for the controlled release of drugs or bioactive substances, and in many other non-food applications.

[0005] Pectin is a polysaccharide consisting of chains of galacturonic acid units 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 backbone of pectin, other chemical groups such as acetyl and methyl ester groups can also be incorporated into the chain. These groups may be important for distinguishing different types of pectin. A review of the properties and characteristics of pectin can be found in D. Gawkowska et al. “Structure-Related Gelling of Pectins and Linking with Other Natural Compounds: A Review” Polymers (Basel), 2018 Jul;10(7): 762, the entire contents of which are incorporated herein by reference.

[0006] Methylation degree is the percentage of carboxyl groups that have been esterified with methanol, and pectin can be classified into two categories based on its methylation degree. Methylation degree is very important for the use of pectin as a gelling agent, and based on methylation degree, 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 methylation degree is lower than this, 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 sets faster and at a higher setting temperature than slow-setting pectin, and is therefore preferred in the production of food and / or beverage products that typically require a certain texture or suspension of various particles (e.g., whole or diced fruits, nuts, etc.). For food and / or beverage products where the presence of suspended particles is not required, slow-setting pectin is preferred. HM pectin can form gels with sugars and acids, thereby forming low-water-activity gels or sugar-acid pectin gels known in the art. Slow-setting pectin may take 1 to 2 days to solidify into a gel. These gels have a 3D network of pectin molecules, in which the solvent (typically water) is optionally fixed together with the cosolvents of sugars and acids, resulting in a system resistant to deformation.

[0008] The difference between LM pectin and HM pectin is that LM pectin only requires the presence of a divalent cation to initiate the reaction that causes the pectin to gel. The most commonly used divalent cation is the calcium ion. Generally speaking, the gel-forming ability of LM pectin increases as the degree of methylation decreases.

[0009] Recently, LM pectin has been amidated to form LM amidated pectin. LM amidated pectin is a modified form of LM pectin in which some of its galacturonic acid units are converted to carboxylic amides by ammonia. In the conventional method for producing LM amidated pectin, HM pectin needs to be extracted from its natural source first. HM pectin is converted to LM pectin and then undergoes amidation to form LM amidated pectin. The conversion of HM pectin to LM amidated pectin follows the reaction scheme below:

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

[0011] Known methods for forming LM amidated pectin can be found in US2480710A, EP1517925 and WO98 / 58968A1, the disclosures of which are incorporated herein by reference in their entirety.

[0012] LM-aminated pectin is more advantageous than non-aminated LM-aminated pectin because it enhances the calcium sensitivity tolerance of LM-aminated pectin, thus allowing gelation over a wider range of calcium concentrations, unlike non-aminated LM-aminated pectin. Further advantageously, aminated pectin is generally thermally reversible: LM-aminated pectin can be heated to form a liquid and solidify again upon cooling, while conventional pectin-gels remain in a liquid form after heating and cooling. Further advantageously, LM-aminated pectin can promote the stability of the bonding regions of the pectin gel network structure by forming additional hydrogen bonds with the amide groups. Further advantageously, LM-aminated pectin exhibits good gelling properties under low-sugar conditions.

[0013] Due to the numerous advantages offered by LM-aminated pectin, it is commonly used in the food and / or beverage industry. Therefore, there will be a long-term need for improved pectins and pectin-containing compositions suitable for use in the food and / or beverage industry. Specifically, there will be a long-term need for improved LM-aminated pectins and compositions containing LM-aminated pectin suitable for use in the food and / or beverage industry. Summary of the Invention

[0014] This invention relates to compositions comprising pectin and water, and methods for preparing the compositions. The compositions possess properties suitable for use in the food and / or beverage industries.

[0015] Representative features of the present invention are listed in the following clauses. These representative features may exist alone or may be combined in any combination with one or more features disclosed in the text and / or drawings of this specification.

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

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

[0018] Pectin; and,

[0019] water;

[0020] When the concentration of pectin 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.

[0021] 2. The composition according to Clause 1, wherein when the concentration of pectin in 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.

[0022] 3. The composition according to 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 according to 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 according to any one of clauses 1 to 4, wherein the pectin has a ratio of the degree of esterification (DE) to the 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 according to any one of clauses 1 to 5, wherein the gelation temperature changes by 1.27°C when the concentration of pectin in water increases relative to the total weight of the composition from 0.8% by weight to 1.4% by weight.

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

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

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

[0029] 10. The composition according to any one of clauses 1 to 9, 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%.

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

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

[0032] 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] Acidity of amidation (DA) of 5% to 30%, or 12% to 25%, or 15% to 23%, or 16% to 22.1%; and

[0034] The ratio of 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.

[0035] 13. A composition having a critical gel concentration (C0), said composition comprising:

[0036] Pectin; and,

[0037] Water; and

[0038] The critical gel concentration (C0) is 0.01% to 0.2% by weight.

[0039] 14. The composition according to Clause 13, 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.

[0040] 15. The composition according to Clause 13 or Clause 14, wherein the pectin has a ratio of the degree of esterification (DE) to the 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.

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

[0042] The critical gel concentration (C0) is 0.12% by weight; optionally,

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

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

[0045] The critical gel concentration (C0) is 0.05% by weight; optionally,

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

[0047] 18. The composition according to 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 methylation degree of less than 50%.

[0048] 19. The composition according to 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; wherein the critical gel concentration (CO) is measured by dynamic oscillatory rheology.

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

[0050] Pectin; and,

[0051] water;

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

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

[0054] 21. The composition according to Clause 20, wherein when the concentration of pectin in water increases relative to the total weight of the composition from 0.8% by weight to 1.4% by weight, the gelation temperature (Tg) varies 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.

[0055] 22. The composition according to Clause 20 or Clause 21, 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.

[0056] 23. The composition according to any one of clauses 20 to 22, wherein the pectin has a ratio of the degree of esterification (DE) to the 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 according to 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 methylation degree of less than 50%.

[0058] 25. The composition according to 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; wherein the gelation temperature (Tg) and / or the critical gelation concentration (C0) are measured by dynamic oscillatory rheology.

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

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

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

[0062] The sugar is present in 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.

[0063] 28. A method for preparing a composition according to any one of clauses 1 to 27, the method comprising the steps of:

[0064] Obtain water-based high-methoxyl (HM) pectin from natural sources;

[0065] 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.

[0066] The dried high-methoxyl (HM) pectin was placed in a suspension containing alcohol and ammonia to form amidated low-methoxyl (LM) pectin.

[0067] 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.

[0068] Water is added to the amidated low-methoxyl (LM) pectin to form a composition.

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

[0070] 30. The method described in accordance with Clause 28 or Clause 29, wherein the natural source is apple pomace or citrus peel.

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

[0072] 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;

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

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

[0075] The aqueous form of high-methoxyl (HM) pectin is subjected to a separation process; optionally, the separation process is mechanical separation.

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

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

[0078] Adjust 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 food and / or beverage products.

[0080] 33. A pectin, said pectin having:

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

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

[0083] The ratio of the degree of esterification (DE) to the degree of amidation (DA) is between 0.5 and 9.0.

[0084] 34. The pectin according to Clause 33, wherein the pectin has a galacturonic acid (GalA) content of 85% or higher, or 90% or higher, or 85% to 95%, or 88% to 94%, or 93.0%.

[0085] 35. The pectin according to Clause 33, wherein the pectin has a galacturonic acid (GalA) content 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. Pectin according to any one of clauses 33 to 35, wherein:

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

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

[0089] The ratio of 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.

[0090] 37. Pectin as described in 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 amidation (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 amidation (DA) is 0.5 to 1.5, or 0.75 to 1.25, or 0.9 to 1.1, or 1.05;

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

[0095] 38. The pectin as described in Clause 37, wherein:

[0096] The degree of esterification (DE) is 23.3%;

[0097] The degree of amidation (DA) is 22.1%; and

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

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

[0100] 39. The pectin as described in Clause 37 or Clause 38, wherein the pectin is derived from citrus peel.

[0101] 40. Pectin as described in 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 amidation (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] The pectin therein has a galacturonic acid (GalA) content 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 as described in 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;

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

[0111] 42. The pectin as described in 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 methoxy (LM) amidated pectin, and optionally wherein the low methoxy (LM) amidated pectin has a methylation degree of less than 50%.

[0114] 45. Use of pectin in food and / or beverage products as described in any one of clauses 33 to 44,

[0115] Optionally, the food and / or beverage products mentioned are dairy products, confectionery products, reduced-sugar jam products, fruit products, and coatings.

[0116] 46. ​​A method for preparing pectin according to any one of clauses 33 to 44, the method comprising the following steps:

[0117] Obtain water-based high-methoxyl (HM) pectin from natural sources;

[0118] 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.

[0119] The dried high-methoxyl (HM) pectin was placed in a suspension containing alcohol and ammonia to form amidated low-methoxyl (LM) pectin; and,

[0120] The amidated low-methoxyl (LM) pectin is dried to form pectin;

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

[0122] 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;

[0123] Concentrate the aqueous form of high-methoxyl (HM) pectin;

[0124] Wash the aqueous form of high-methoxyl (HM) pectin with alcohol;

[0125] The aqueous form of high-methoxyl (HM) pectin is subjected to a separation process; optionally, the separation process is mechanical separation.

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

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

[0128] Adjust 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 described in any one of clauses 33 to 44;

[0133] Optionally, the composition further comprises sugar.

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

[0135] Optionally, the sugar is present in 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 described in Clause 47 in food and / or beverage products,

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

[0138] 49. A method for preparing the composition according to clause 47, the method comprising:

[0139] Provides pectin; and

[0140] The pectin is combined with water to form a composition;

[0141] Wherein, the pectin is the pectin described in any one of clauses 33 to 44;

[0142] Optionally, the composition comprises the pectin at the following concentrations: 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. Attached Figure Description

[0143] Figure 1 This is a flowchart of a method for producing pectin according to the present invention from dried HM pectin.

[0144] Figure 2 This is a graph of the storage modulus (G') and loss modulus (G") of a composition comprising pectin and water according to the present invention (the composition analyzed is composition 1).

[0145] Figure 3 This is a graph of the storage modulus (G') versus concentration (C) of the composition comprising pectin and water according to the present invention (the composition analyzed is composition 1). Detailed Implementation

[0146] Embodiments of the invention are described below with reference to the accompanying drawings. The drawings illustrate various embodiments of the system, method, and other aspects of this disclosure. Those skilled in the art will understand that the element boundaries (e.g., boxes, groups of boxes, or other shapes) shown in the drawings represent one example of a boundary. In some examples, one element may be designed as multiple elements, or multiple elements may be designed as one element. In some examples, an element shown as an internal component of one element may be implemented as an external component of another element, and vice versa. Furthermore, elements may not be drawn to scale. The following description is non-limiting and non-exhaustive, with reference to the accompanying drawings. Components in the drawings are not necessarily drawn to scale, but rather to illustrate principles.

[0147] The embodiments of this disclosure will be described more fully below with reference to the accompanying drawings, in which the same numerals represent the same elements and exemplary embodiments are illustrated. However, the embodiments of the claims may be embodied in many different forms and should not be construed as limited to the embodiments described herein.

[0148] The words “comprising,” “having,” “containing,” and “including,” and their other forms, are intended to be equivalent in meaning and are open-ended, as one or more items following any of these words are not meant to be an exhaustive list of such items or to be limited to only the listed items. Additionally, the phrase “consistently composed of” will be understood to include those specifically listed elements and those additional elements that do not substantially affect the essential and novel characteristics of the invention. The phrase “consisting of” excludes any unspecified elements. It must also be noted that, unless the context explicitly indicates otherwise, the singular forms “a” and “the” as used herein and in the appended claims include plural references. Although any systems and methods similar to or equivalent to those described herein may be used in practicing or testing embodiments of this disclosure, preferred systems and methods are now described.

[0149] As used herein, the terms “for example,” “to illustrate,” “such as,” or “including” are intended to provide examples that further illustrate a more general subject. Unless otherwise stated, these examples are provided merely to aid in understanding the application of the descriptions in this disclosure and are not intended to be limiting in any way.

[0150] As used herein, “about” will be understood by one of ordinary skill in the art and will vary to some extent depending on the context in which it is used. If the use of the term is unclear to one of ordinary skill in the art, “about” will mean at most positive or negative 10% of that particular term, taking into account the context in which it is used.

[0151] Furthermore, it should be understood that the wording or terminology used herein, unless otherwise defined, is for descriptive purposes only and not for limitation. Any use of chapter headings is intended to aid reading the document and should not be construed as restrictive; information relating to chapter headings may appear within or outside that particular chapter. In the event of any inconsistency between the usage in this document and that of documents so incorporated by reference, the usage in the incorporated references shall be considered supplementary to the usage in this document; in the case of irreconcilable inconsistencies, the usage in this document shall prevail.

[0152] The following is a list of some terms used to describe the present invention:

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

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

[0155] A “composition” means a mixture of at least two components. The mixture may be a solution, suspension or dispersion.

[0156] The degree of amidation (DA) refers to the percentage of carboxyl groups that form an amide. Theoretically, the degree of amidation can be from 0% to 100%. Preferably, the degree of amidation of pectin is from 5% to 30%. The degree of amidation can be measured by titration, an example of which is found in EP1517925, the disclosure of which is incorporated herein by reference in its entirety.

[0157] "Degree of esterification" (DE) refers to the percentage of esterified carboxyl groups. Theoretically, the degree of esterification can range from 0% to 100%. The degree of esterification is also referred to in the art as the degree of methyl esterification or the degree of methylation (DM). The degree of esterification can be measured by titration, examples of which can be found in EP1294920 and EP1171473, the disclosures of which are incorporated herein by reference in their entirety.

[0158] "Methylation degree" refers to the percentage of carboxyl groups esterified by methanol. If more than 50% of the carboxyl groups are methylated, the pectin is called high-methoxyl pectin (HM), and if the degree of methylation is lower than this, the pectin is called low-methoxyl pectin (LM).

[0159] "High-methoxyl pectin" or "HM pectin" refers to pectin extracted from the peel of citrus fruits, in which a certain degree of the original carboxyl groups present in the pectin have undergone esterification with methanol. High-methoxyl pectin has a methylation degree of over 50%.

[0160] "Low-methoxyl pectin" or "LM pectin" refers to pectin extracted from the peel of citrus fruits, in which a certain degree of the original carboxyl groups present in the pectin have undergone esterification with methanol. Low-methoxyl pectin has a methylation degree of less than 50%.

[0161] "Homogeneous" means that the material as a whole has a uniform composition. For example, the gradient of a certain property (e.g., concentration) of a homogeneous material must not exceed 1% by weight of the calculated value of that property. According to the invention, the composition may contain pectin, wherein the pectin is homogeneous (i.e., the composition contains only one type of pectin). One type of pectin is understood herein to mean that the pectin used according to the invention is obtained from a single source of pectin and has a certain degree of amidation and a certain degree of esterification.

[0162] "Low-methoxylated pectin," "LM-aminated pectin," or "LMA pectin" refers to a modified form of LM pectin in which some or at least some of the methoxy groups are converted to carboxylic acid amides by ammonia. Preferably, LM-aminated pectin has an amidation degree of 5% to 30%.

[0163] A mixture is a substance containing two or more different components, and the term “mixing” refers to the methods and steps by which a mixture is formed.

[0164] "Pectin" refers to anionic, water-soluble plant cell wall polysaccharides containing chains of galacturonic acid units linked by α-1,4 glycosidic bonds. The galacturonic acid chains are partially esterified, meaning they contain methyl ester groups. Other chemicals, such as acetyl groups, can be incorporated into the galacturonic acid chains and may be important for distinguishing different types of pectin.

[0165] "Pectin gel" refers to a sample containing a three-dimensional (3D) network of pectin molecules. Pectin gels result from the binding of long segments of pectin polymer chains into conformationally ordered junctions, which are stabilized by an array of non-covalent interactions. Pectin gels exhibit the viscosity of a liquid and the elasticity of a solid, i.e., viscoelastic materials. Pectin gels have been known to those skilled in the art for decades, see, for example, MAVAxelos et al., "CHAPTER 11 - Rheology of Pectin Dispersions and Gels", The Chemistry and Technology of Pectin, Food Science and Technology, 1991, Pages 227-250, ISBN 978-0-08-092644-5, the entire contents of which are incorporated herein by reference.

[0166] "Gel temperature" (Tg) refers to the temperature at which a material undergoes reverse thermal gelation. Below this temperature, the material is soluble in water, while above it, the material undergoes a phase change to increase viscosity or form a semi-solid gel. For example, for gelling polysaccharides like pectin, the gel temperature (Tg) is the temperature at which a solution containing pectin changes from a liquid state to a gel state.

[0167] Composition

[0168] The compositions according to the invention possess a variety of desirable properties, which makes them suitable for use in a wide range of food and beverage products.

[0169] Composition: Gelation temperature

[0170] The composition may contain pectin and water.

[0171] 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, and most preferably 0.4% to 2% by weight relative to the total amount of pectin and water.

[0172] The composition has a gelation temperature (Tg) wherein, as the concentration of pectin relative to the total amount of pectin and water increases from 0.8 wt% to 1.4 wt%, the gelation temperature (Tg) varies 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, and most preferably 1.03°C to 1.27°C. Preferably, as the concentration of pectin in the water increases from 0.8 wt% to 1.4 wt% relative to the total amount of pectin and water, the gelation temperature (Tg) varies by 1.03°C to 1.27°C.

[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%, and 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%, and most preferably 16.0% to 22.1%.

[0175] The pectin in the composition may have a ratio of esterification degree (DE) to amidation degree (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, and 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%, and 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%, and most preferably 16.0% to 22.1%; and a ratio of esterification (DE) to amidation (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, and 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 esterification (DE) to amidation (DA) of 1.05 to 1.94.

[0177] Pectin can be derived from any one of the following: apple, apple pomace, citrus fruits, citrus peel, lemon, Chinese tangerine, grapefruit, sweet orange, pomelo, Clementine, sour orange, kumquat, bitter orange, blood orange, seedless mandarin orange, sweet orange, tangerine, or pomelo, or any combination thereof.

[0178] The composition may contain apple pectin, such as pectin extracted from apple pomace. The composition may contain apple pectin and water, and the gelation temperature is 1.27°C when the concentration of pectin in the water increases from 0.8% by weight to 1.4% by weight relative to the total amount of pectin and water. Preferably, the pectin also has a degree of esterification (DE) to degree of amidation (DA) ratio of 1.9 to 2.0, preferably 1.94. Preferably, the pectin present in the composition in its entirety is apple pectin.

[0179] The composition may contain citrus pectin, such as pectin extracted from citrus fruits (e.g., citrus peel). The composition may contain citrus pectin and water, and the gelation temperature is 1.03°C when the concentration of pectin in the water increases from 0.8% by weight to 1.4% by weight relative to the total amount of pectin and water. 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, the total amount of pectin present in the composition is citrus pectin.

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

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

[0182] The composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source selected from apple, apple pomace, citrus fruits, citrus peel, lemon, Chinese mandarin orange, grapefruit, sweet orange, pomelo, Clementine, sour orange, kumquat, bitter orange, blood orange, seedless mandarin orange, sweet orange, tangerine, or any combination thereof.

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

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

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

[0186] The composition may additionally contain a gel-promoting medium and / or a buffer solution.

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

[0188] Preferably, the buffer solution comprises sodium citrate and water, and more preferably, the buffer solution contains sodium citrate such that the pH of the buffer solution is 3 to 4, more preferably 3.2 to 3.6, and 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 as the concentration of pectin relative to the total amount of pectin and water increases from 0.8% by weight to 1.4% by weight; and wherein the composition further comprises a gel-promoting medium and a buffer solution; wherein the gel-promoting medium comprises citric acid monohydrate, trisodium citrate dihydrate, sodium benzoate, calcium chloride dihydrate, and water; and wherein the buffer solution comprises sodium citrate and water.

[0190] Composition: Critical gelation concentration

[0191] The composition may contain pectin and water.

[0192] 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, and 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, and 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%, and 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%, and most preferably 16.0% to 22.1%.

[0196] The pectin in the composition may have a ratio of esterification degree (DE) to amidation degree (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, and 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%, and 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%, and most preferably 16.0% to 22.1%; and a ratio of esterification (DE) to amidation (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, and 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 esterification (DE) to amidation (DA) of 1.05 to 1.94.

[0198] Preferably, the composition may comprise pectin and water, wherein the critical gel concentration (CO) 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] Pectin can be derived from any one of the following: apple, apple pomace, citrus fruits, citrus peel, lemon, Chinese tangerine, grapefruit, sweet orange, pomelo, Clementine, sour orange, kumquat, bitter orange, blood orange, seedless mandarin orange, sweet orange, tangerine, or pomelo, or any combination thereof.

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

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

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

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

[0204] The composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source selected from apple, apple pomace, citrus fruits, citrus peel, lemon, Chinese mandarin orange, grapefruit, sweet orange, pomelo, Clementine, sour orange, kumquat, bitter orange, blood orange, seedless mandarin orange, sweet orange, tangerine, or any combination thereof.

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

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

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

[0208] The composition may additionally contain a gel-promoting medium and / or a buffer solution.

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

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

[0211] Preferably, the composition has a critical gel concentration (C0), wherein the critical gel concentration (C0) varies from 0.01% by weight to 0.2% by weight, 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.

[0212] Composition: Gelation temperature and critical gelation concentration

[0213] The composition may contain pectin and water.

[0214] 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, and most preferably 0.4% to 2% by weight relative to the total amount of pectin and water.

[0215] The composition has a gelation temperature (Tg) and a critical gelation concentration (C0), wherein when the concentration of pectin relative to the total amount of pectin and water increases from 0.8 wt% to 1.4 wt%, the gelation temperature (Tg) varies 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, and most preferably 1.03°C to 1.27°C, and wherein the critical gelation 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%, and most preferably 0.05 wt% to 0.12 wt%.

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

[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%, and 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%, and most preferably 16.0% to 22.1%.

[0219] The pectin in the composition may have a ratio of esterification degree (DE) to amidation degree (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, and 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%, and 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%, and most preferably 16.0% to 22.1%; and a ratio of esterification (DE) to amidation (DA) of 0.75 to 3.0, preferably 0.85 to 2.5, more preferably 0.95 to 2.0, and 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 esterification (DE) to amidation (DA) of 1.05 to 1.94.

[0221] Pectin can be derived from any one of the following: apple, apple pomace, citrus fruits, citrus peel, lemon, Chinese tangerine, grapefruit, sweet orange, pomelo, Clementine, sour orange, kumquat, bitter orange, blood orange, seedless mandarin orange, sweet orange, tangerine, or pomelo, or any combination thereof.

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

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

[0224] The composition comprises pectin and water, wherein the pectin is preferably extracted from a single pectin source selected from apple, apple pomace, citrus fruits, citrus peel, lemon, Chinese mandarin orange, grapefruit, sweet orange, pomelo, Clementine, sour orange, kumquat, bitter orange, blood orange, seedless mandarin orange, sweet orange, tangerine, or any combination thereof.

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

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

[0227] The composition may contain sugar. The sugar may be, but is not limited to, sucrose, dextrose, lactose, maltose, glucose, and / or galactose. Preferably, the sugar is sucrose. Preferably, the composition contains 20% to 60% by weight of the total weight of the composition, preferably 30% to 50% by weight, more preferably 35% to 45% by weight, and most preferably 40% by weight of the sugar.

[0228] The composition may additionally contain a gel-promoting medium and / or a buffer solution.

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

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

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

[0232] Composition as pectin gel

[0233] The compositions described under the subheading “Composition” can be in the form of pectin gels. The pectin gels according to the invention possess various desirable properties, making them suitable for use in a wide range of food and beverage products.

[0234] Pectin gels comprise the compositions described under the subheading “Compositions”, namely, pectin gels comprise water and pectin.

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

[0236] The pectin gel may also contain additional materials, including 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 contains 20% to 60% by weight of the total weight of the pectin gel, preferably 30% to 50% by weight, more preferably 35% to 45% by weight, and most preferably 40% by weight of additional materials.

[0237] Pectin gels may also contain aroma agents, flavoring agents, coloring agents, preservatives, etc. Pectin gels may contain gel-promoting mediators, such as, but not limited to, calcium.

[0238] Pectin gels may contain one or more 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, a water-immiscible organic oil, or an aqueous matrix. Preferably, the water-immiscible material is, but is not limited to, fragrances, flavorings, pheromones, bactericides, insect attractants, insect repellents, animal attractants, agonists, insecticides, fungicides, pharmaceuticals, veterinary drugs, other volatile oils or organic materials, or any combination thereof.

[0239] Methods for preparing pectin

[0240] Another aspect of the present invention relates to a method for preparing pectin. Specifically, this aspect of the present invention relates to a method for preparing LM-amylated pectin.

[0241] In the method for 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 shown.

[0243] Step 1: Extract HM pectin from natural sources of pectin

[0244] First, following methods described elsewhere, natural sources of pectin were mixed in acidic hot water to extract HM pectin from the aqueous form of natural pectin, e.g., Endreb, H.-U., & Christensen, SH (2020). Pectins. In GO Philips & PA Williams (Eds.), Handbook of hydrocolloids (3rd ed., pp. 274-297). Cambridge: Woodhead Publishing Limited, the entire contents of which are incorporated herein by reference. Typically, natural sources of pectin are raw materials extracted from fruits.

[0245] In this method, the natural source of pectin can be fruit, such as apple, apple pomace, citrus fruits, citrus peel, lemon, Chinese mandarin orange, grapefruit, sweet orange, pomelo, Clementine, lime, kumquat, bitter orange, blood orange, seedless mandarin orange, sweet orange, tangerine, 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 acidic hot water is 1 to 20 hours, or 6 to 14 hours, or 7 to 13 hours, or 8 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 to 12 hours.

[0250] The aqueous form of HM pectin can then be clarified by using centrifugation, filtration, or other conventional separation techniques known in the art to obtain a 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] Alcohol can be added to concentrated aqueous form of HM pectin to precipitate the HM extract into a precipitate containing HM pectin. The amount of alcohol added depends on the amount required to precipitate the clarified HM extract from its aqueous form into a precipitate containing HM pectin.

[0253] Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, tert-butanol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutanol, isopropanol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentanol, 2-pentanol, 1,3-propanediol, propylene-1-ol, propylene glycol, and propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropanol.

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

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

[0256] Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, tert-butanol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutanol, isopropanol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentanol, 2-pentanol, 1,3-propanediol, propylene-1-ol, propylene glycol, and propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropanol.

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

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

[0259] Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, tert-butanol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutanol, isopropanol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentanol, 2-pentanol, 1,3-propanediol, propylene-1-ol, propylene glycol, and propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropanol.

[0260] The washed HM pectin can then undergo a drying step to form dried HM pectin. This drying step dries the washed HM pectin until it 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 carried out by pressure drying. The product of the drying step is dried HM pectin.

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

[0262] In order to make the product of the first step into the pectin of this invention, the parameters of the above process need to be strictly controlled.

[0263] Step 2: Amideation of dried HM pectin

[0264] Dry HM pectin can be placed in a suspension containing alcohol and ammonia to form amidated LM pectin.

[0265] Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, tert-butanol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutanol, isopropanol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentanol, 2-pentanol, 1,3-propanediol, propylene-1-ol, propylene glycol, and propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropanol.

[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, 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. More preferably, ammonia is present at 2.8% to 3.5% by weight of the total weight of the suspension.

[0268] Preferably, the suspension is maintained at a temperature of 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 suspension is maintained at a temperature of 10°C to 14°C.

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

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

[0271] LM-aminated pectin can be filtered from the suspension to produce a filtrate containing alcohol and a residue containing LM-aminated pectin. LM-aminated pectin can be filtered from the suspension using any filtration technique known in the art.

[0272] Preferably, the filtrate containing alcohol and ammonia is fed into the recovery step.

[0273] Preferably, the residue containing LM-amidated pectin can be washed to form washed LM-amidated pectin. Preferably, the residue containing LM-amidated pectin is washed with an alcohol. Preferably, the residue containing LM-amidated pectin is washed with an alcohol comprising 50% to 70% by weight, or 55% to 65% by weight, or 60% by weight of the total alcohol. Preferably, the alcohol used is isopropanol. Preferably, the alcohol used is one or more of isopropanol, tert-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, tert-butanol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutanol, isopropanol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentanol, 2-pentanol, 1,3-propanediol, propylene-1-ol, propylene glycol, and propylene glycol methyl ether, or any combination thereof. Preferably, the alcohol is isopropanol.

[0274] Preferably, the pH of the washed LM amidated pectin can be 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-aminated pectin is adjusted with an acid to form pH-adjusted LM-aminated pectin. Preferably, the acid is citric acid.

[0276] LM amidated pectin that has been pH adjusted can be washed with alcohol to form LM amidated pectin that has been washed twice.

[0277] Preferably, the alcohol is any one of tert-amyl alcohol, benzyl alcohol, 1,4-butanediol, 1,2,4-butanetriol, butanol, 1-butanol, 2-butanol, tert-butanol, diethylene glycol, ethanol, ethylene glycol, 2-ethylhexanol, furfuryl alcohol, glycerol, isobutanol, isopropanol, methanol, 2-(2-methoxyethoxy)ethanol, 2-methyl-1-butanol, 2-methyl-1-pentanol, 3-methyl-2-butanol, neopentanol, 2-pentanol, 1,3-propanediol, propylene-1-ol, propylene glycol, propylene glycol methyl ether, isopropanol, or any combination thereof. Preferably, the alcohol is isopropanol.

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

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

[0280] LM amidated pectin that has undergone two washing steps can be dried to form dried LM amidated pectin.

[0281] Preferably, the drying step is carried out by pressure drying.

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

[0283] Dry LM-amidated pectin is LM-amidated pectin prepared for use in compositions according to the present invention. Dry LM-amidated pectin can be blended with sugars to form standardized LM-amidated pectin.

[0284] To ensure that the product of the second step becomes the pectin of this invention, several key parameters of the above process need to be controlled during the amidation reaction. These parameters include the weight percentage of alcohol and ammonia in the suspension, the residence time of HM pectin in the suspension, and the temperature of the suspension. By controlling these parameters, the desired degree of esterification and amidation can be obtained.

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

[0286] Method for preparing compositions containing pectin

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

[0288] (a) Provides pectin; and

[0289] (b) Combining pectin with water to form a composition.

[0290] The composition may contain pectin at a concentration 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, and most preferably 0.4% to 2% by weight relative to the total amount of pectin and water.

[0291] The composition may additionally contain 0.001 to 10 mM, preferably 0.005 to 0.005 mM, and most preferably 0.01 to 8 mM of a gel-promoting medium. Preferably, the gel-promoting medium is calcium.

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

[0293] The composition may additionally contain sugar. The composition may contain 20% to 60% by weight, or 30% to 50% by weight, or 35% to 45% by weight, or 40% by weight of sugar, of the total weight of the composition. Preferably, the sugar is, but is not limited to, sucrose, dextrose, lactose, maltose, glucose, and / or galactose.

[0294] Method for preparing compositions as pectin gels

[0295] Another aspect of the present invention relates to a method for preparing a pectin gel, wherein the pectin gel comprises the composition described under the subheading "Composition," i.e., wherein the pectin gel comprises pectin and water. The method for preparing a pectin gel includes the following steps:

[0296] (a) Mix pectin, gel facilitator and water to form a solution;

[0297] (b) Heat the solution until pectin and gel promote the dissolution of the medium;

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

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

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

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

[0302] Compositions for use in food or beverage products

[0303] Another aspect of the invention relates to compositions for use in food or beverage products, wherein the compositions are as described under the subheading “Compositions”.

[0304] The composition may be incorporated into dairy products, including but not limited to milk, condensed milk, dehydrated milk, milk beverages, cheese, butter, yogurt, curd, custard, farm cheese, cream cheese, curd, frozen dairy products such as frozen custard, frozen yogurt and ice cream, gelato, milk powder, sweetened condensed milk, sour cream, yogurt, whey, whey protein or whipped cream.

[0305] The composition may be incorporated into sweetened products, including but not limited to confectionery products, reduced-sugar jams, fruit products, jellies, sugar coatings, and spray coatings.

[0306] Preferably, the composition is incorporated into meat products, poultry products, fish products, dairy products (e.g., milk, ice cream, yogurt, cheese, pudding, and flavored dairy beverages), baked goods (e.g., bread, cakes, cookies, crackers, biscuits, pies, donuts, pretzels, and potato chips), non-dairy spreads, mayonnaise, soups, sauces, dips, condiments, frozen desserts, fruit products, jams and jellies, beverages, hydrogels, sweet jellies, or low-fat spreads.

[0307] Compositions for use in non-food or non-beverage products

[0308] Another aspect of the invention relates to compositions for use in non-food or non-beverage products, wherein the compositions are as described under the subheading “Compositions”.

[0309] This composition can be incorporated into other products related to nutrition, bioactive substances, cosmetics, and pharmaceuticals.

[0310] Method for producing compositions for use in food or beverage products

[0311] Another aspect of the present invention relates to a method for preparing a food or beverage product comprising a composition as described under the subheading “Composition”. The method for preparing the food or beverage product includes the following steps:

[0312] (a) providing the composition; and

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

[0314] Method for producing compositions for use in non-food or non-beverage products

[0315] Another aspect of the present invention relates to a method for preparing a non-food or non-beverage product comprising a composition as described under the subheading “Composition”. The method for preparing the non-food or non-beverage product includes the following steps:

[0316] (a) providing the 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 embodiments for discussing the advantages of the invention with reference to tables and figures. The embodiments described herein are merely examples among many possible embodiments.

[0320] Materials used in the embodiments

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

[0322] The novel pectin was compared with commercially available pectin supplied by Cargill.

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

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

[0325]

[0326] The composition of commercially available pectin is shown in Table 2.

[0327] Table 2: Composition of commercially available pectin .

[0328]

[0329] GalA refers to the content of galacturonic acid (GalA) in each pectin.

[0330] Example 1: Extraction of LM-amylated pectin

[0331] Step 1: Extraction of HM pectin

[0332] First, citrus peels or apple pomace are mixed in acidic hot water to extract HM pectin from the citrus peels or apple pomace as an aqueous form of HM pectin. The acidic hot water is at a temperature of 68°C to 72°C, a pH of 1.50 to 1.70, and a residence time of 8 to 12 hours.

[0333] HM pectin was clarified in its aqueous form by centrifugation and filtration to form a clarified aqueous form.

[0334] The clarified aqueous form of HM pectin is then concentrated to form a concentrated aqueous form of HM pectin.

[0335] Isopropanol was added to concentrated HM pectin in aqueous form to precipitate the HM extract as a precipitate containing HM pectin. The precipitate containing HM pectin was present in the alcohol (isopropanol) / water mixture.

[0336] The precipitate containing HM pectin was separated from the alcohol / water mixture by mechanical separation.

[0337] The precipitate containing HM pectin obtained from the separation was then washed three times with isopropanol, which accounts for 60% by weight of the total alcohol, to form washed HM pectin.

[0338] 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.

[0339] Step 2: Amideation of dried HM pectin

[0340] The dried HM pectin was placed in a suspension containing an alcohol (isopropanol) and ammonia. The alcohol was present at 60% to 70% by weight of the total weight of the suspension, and the ammonia was present at 2.8% to 3.5% by weight of the total weight of the suspension. The suspension was maintained at a temperature of 10°C to 14°C. The dried HM pectin was held in the suspension for 5 to 8 hours. After 5 to 8 hours, the dried HM pectin underwent amidation to form LM amidated pectin.

[0341] To stop further reactions occurring in the suspension, LM-aminated pectin is filtered off from the alcohol and ammonia. The alcohol and ammonia proceed to the recovery step. The LM-aminated pectin is washed with isopropanol at 60% by weight of the total alcohol to form washed LM-aminated pectin.

[0342] Adjust the pH of the washed LM amidated pectin to form pH-adjusted LM amidated pectin. Adjust the pH of the washed LM amidated pectin until it is between 4.0 and 4.5. Adjust the pH with nitric acid.

[0343] LM amidated pectin, which has been pH adjusted, was washed three times with isopropanol to form LM amidated pectin that has been washed twice.

[0344] The LM-aminated pectin, after two washings, undergoes a drying step to form dried LM-aminated pectin. The drying step dries the LM-aminated pectin after two washings until it has a moisture content of 10% by weight of the total weight of the dried LM-aminated pectin.

[0345] Example 2: Structural characterization of LM-amylated pectin

[0346] In this non-limiting embodiment of the invention, the degree of esterification (DE), degree of amidation (DA), and galacturonic acid (GalA) of pectin are determined using a titration method (see National Research Council, 1981, Yu, et al, 2021, the disclosure of which is incorporated herein by reference in its entirety). The method for measuring the degree of esterification (DE), degree of amidation (DA), and galacturonic acid (GalA) involves washing the pectin sample with acidified aqueous isopropanol to remove any cations, salts, and normalized 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, and then neutralized with an exact equivalent of 0.5 M hydrochloric acid, such that the released acid groups can be titrated with 0.1 M sodium hydroxide. A strong alkaline distillation solution can then be used to release ammonia from the amide groups of the amidated pectin. Ammonia is estimated using the same 0.1 M sodium hydroxide by a back-titration procedure. After titration, the ratios of amidation, esterification, and galacturonic acid content were calculated according to the method described in National Research Council, 1981, Yu, et al, 2021 (the entire contents of which are incorporated herein by reference).

[0347] The degree of amidation, degree of esterification, and galacturonic acid content of LM amidated pectin are shown in Table 3.

[0348] Table 3: Chemical composition of pectin .

[0349]

[0350] Example 3: Measurement of the intrinsic viscosity of LM-amylated pectin

[0351] In this non-limiting embodiment of the invention, the intrinsic viscosity of pectin was determined by size exclusion chromatography-multi-angle laser scattering (SEC-MALLS), as described in Hellin, P., Ralet, MC, Bonnin, E., & Thibault, JF (2005). Homogalacturonic acid from lime pectin exhibits a uniform charge density and molar mass distribution. A method for determining the intrinsic viscosity of pectin is disclosed in Carbohydrate Polymers, 60(3), 307-317, specifically on page 309, the entire disclosure of which is incorporated herein by reference.

[0352] A 5 mg / mL aqueous solution of pectin 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 entire contents of which are incorporated herein by reference) and TriSec software (Version 3.0, Voscotek, Houston, TX, the entire contents of which are incorporated herein by reference). All analyses were performed in triplicate, and the average value was taken.

[0353] The average intrinsic viscosity of pectin is shown in Table 4.

[0354] Table 4: Intrinsic viscosity of pectin .

[0355]

[0356] Example 4: Preparation of a composition containing LM-amylated pectin and water

[0357] In this non-limiting embodiment, individual compositions comprising each pectin as shown in Table 1 were prepared. The compositions comprise pectin and water: each composition comprises one of pectin 1-5. The compositions were prepared such that the resulting pectin concentration was from 0.4% to 2.0% by weight of the total weight of the composition, wherein sucrose was 40% by weight.

[0358] To prepare each composition, a pre-solution of pectin was first prepared by dissolving each type of pectin in distilled water by mechanical stirring at 90°C for 10 minutes.

[0359] After dissolving pectin in distilled water, 190 to 320 g of a heat buffer solution and a gel-promoting medium are added to the distilled water and pectin solution.

[0360] The buffer solution contains a sufficient concentration of sodium citrate to achieve a pH of 3.4. The sodium citrate is dissolved in distilled water. The buffer solution is heated to the same temperature (90°C) as the distilled water and pectin solution before being added. The buffer solution also contains CaCl2 (8.4 mM) and sucrose.

[0361] The gel-promoting medium was added to a solution containing distilled water and pectin to achieve a concentration of 8.4 mM in water. The composition of the gel-promoting medium is shown in Table 5.

[0362] Table 5: Gel-promoting media .

[0363]

[0364] 5 liters of pH 3.4 buffer stock solution.

[0365] Advantageously, the ionic strength of the gel-promoting medium plays a significant role in the gelation temperature and critical gelation concentration. Higher ionic strength of the gel-promoting medium results in a higher gelation temperature and a lower critical gelation concentration.

[0366] The resulting composition with a final calcium chloride (CaCl2) concentration of 3 mM was stirred at 90 °C for 5 minutes. The final pH of each prepared composition was 3.4.

[0367] Table 6 shows the types of pectin contained in each composition.

[0368] Table 6: Pectin used to prepare each composition .

[0369]

[0370] Example 5: Measurement of gelation temperature (Tg)

[0371] In this non-limiting embodiment, the gelation temperature (Tg) of each composition was measured. For each composition, the gelation temperature (Tg) was measured in the range of 0.8 wt% to 1.4 wt% (of the total weight of the composition) of pectin concentration.

[0372] The composition analyzed was the composition prepared in Example 4.

[0373] To measure the gelation temperature (Tg) of each composition, dynamic oscillation (or small deformation) measurements were performed on each composition using either an ARES-G2 strain-controlled rheometer (TAInstruments) or an MCR 92 stress-controlled rheometer (Anton Paar Physica). Both rheometers were equipped with a Couette apparatus.

[0374] During measurement, each composition (as described in Example 4 above) was covered with a thin layer of paraffin oil to prevent evaporation during the measurement.

[0375] Before measurement, each composition was poured (separately) into the Couette apparatus (preheated at 80°C) and pre-sheared (10 s) first. -1 The sample entry record of the composition was cleared for 2 minutes. The composition was then exposed to a temperature scan test from 80°C to 10°C (2°C / min). Viscoelastic experiments were performed using an ARES-G2 strain-controlled rheometer and an MCR 92 stress-controlled rheometer at strains of 0.4% and 10% and a frequency of 0.8 Hz, respectively. Both strain amplitudes were confirmed in the LVE domain.

[0376] In all such small-scale variations, each measurement was repeated three times using a new formulation (of the same composition). The average of the three measurements was taken.

[0377] At the end of the measurement, the gelation temperature (Tg) representing the crossover point between the storage modulus (G') and the loss modulus (G") was collected from the gelation kinetic data obtained after the temperature scan test (as described above). The storage modulus G' and loss modulus (G") values ​​were collected from the mechanical spectra using an automated data export program from Rheocompass software (Anton Paar). The crossover point between the storage modulus (G') and the loss modulus (G") was determined, as shown... Figure 2 As shown. Figure 2 Data points for composition 1 with a pectin concentration of 1.4% in water are displayed. The mean Tg and corresponding standard deviation of the data obtained from three parallel measurements were then calculated.

[0378] Then the measurements were repeated for each composition (separately).

[0379] The average values ​​of the gelation temperature (Tg) measurements are shown in Table 7.

[0380] Table 7: Average gelation temperature (Tg) of each composition .

[0381]

[0382] Example 6: Measurement of Critical Gelatinization Concentration (C0)

[0383] In this non-limiting embodiment, the critical gel concentration of each composition was measured.

[0384] The composition analyzed was the composition prepared in Example 4.

[0385] 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 MCR 92 stress-controlled rheometer (Anton Paar Physica). Both rheometers are equipped with a Couette apparatus.

[0386] During measurement, each composition prepared as described above was covered with a thin layer of paraffin oil to prevent evaporation during the measurement.

[0387] Before measurement, each composition was poured (separately) into the Couette apparatus (preheated at 80°C) and pre-sheared (10 s) first. -1The sample entry record of the instrument was cleared for 2 minutes. Each composition was then exposed to a temperature scan test (2 °C / min) decreasing from 80 °C to 10 °C, followed by a time scan experiment at a frequency of 0.8 Hz for 30 minutes to ensure that the resulting gel reached equilibrium due to reorganization (structural rearrangement). To ensure viscoelastic measurements in the LVE domain, strain scan experiments from 0.01% to 40% were performed at 0.8 Hz. Viscoelastic experiments were conducted using an ARES-G2 strain-controlled rheometer and an MCR 92 stress-controlled rheometer at strains of 0.4% and 10%, respectively. Both strain amplitudes were confirmed in the LVE domain.

[0388] In all such small-scale variations, each measurement was repeated three times using a new formulation (of the same composition). The average value was taken.

[0389] Then, the following steps are performed to determine C0:

[0390] (i) Storage modulus (G') and loss modulus (G") values ​​were collected from the mechanical spectrum using an automated data export program from Rheocompass software (Anton Paar), and plotted on a logarithmic scale as a function of pectin concentration C (%). Examples of such plots include... Figure 3 As shown, it illustrates experimental and calculated data on the storage modulus (G') of composition 1 as a function of pectin concentration (the calculated data were obtained using the following formula: G' = 1700). (C-C0) 2.19 Where C0 = 0.05%, such as Figure 3 As shown; Figure 3 The second equation shown (G' = 1733.2) C 2.19 R² = 0.9974 refers to the fitted model of the experimental data, where the exponential value reflects the structural level of the gel, and R² is the statistical measure of the fit, indicating how much change in the dependent variable is interpreted by the independent values ​​in the regression model: when R² is close to 1 (as in this example), the fitted model is reliable.

[0391] (ii) Fit the data using a power-law relationship to obtain the formula G' = kC n Where G' is the storage modulus, k represents the scaling factor, C (%) is the pectin concentration, and n is the exponent value (the formulas for calculation and experimental data are shown in step (i) above); and

[0392] (iii) Following the methods described in the literature (e.g., de Gennes, P.-G. (1979). Scaling Concepts in Polymer Physics. Cornell University Press: Ithaca and London, New York.; Jones, JL, & Marques, CM (1990). Rigid polymer network models. Journal de Physique, 51, 1113-1127.; Ross-Murphy, SB (1987) and Physicalgelation of biopolymers. Food Hydrocolloids, 1, 485-495., the contents of which are incorporated herein by reference in their entirety), linear regression was used to transform the equation G' = kC n After mathematical transformation, it becomes G' = k'(C - C0). n Form. In this second formula, k' represents the scaling factor, and C0 represents the concentration below which gel-like behavior cannot be achieved.

[0393] Based on the condition G' = kC n = k'(C - C0) n Linear regression was performed on all products studied, where the two exponents (n) had the same value and C > C0.

[0394] The effectiveness of the critical gel concentration (C0) determined using the above-described fitting model was then verified by evaluating the rheological behavior of compositions 1, 2, 3, 4, and 5 under the same conditions.

[0395] Then, the measurements were repeated for each composition (separately). For each composition formulation, the measurements were repeated three times, and the average value was taken.

[0396] The average values ​​of the critical gel concentration (C0) measurements are shown in Table 8.

[0397] Table 8: Average Critical Gelatinization Concentration (C0) of Each Composition .

[0398]

[0399] Advantageously, a low critical gel concentration (C0) results in highly functional products. The lower the critical gel concentration (C0) of the composition, the less composition is required to achieve a gel in food and / or beverage products. The compositions of the present invention have a low critical gel concentration (C0), thus requiring less composition to achieve a gel in food and / or beverage products. This is advantageous for manufacturing cheaper food and / or beverage products because less composition is needed in the food and / or beverage products.

[0400] Furthermore, the lower the ratio of degree of esterification (DE) to degree of amidation (DA), the lower the critical gel concentration (C0).

[0401] Furthermore, the aforementioned advantages of the final product formulation can help identify new pathways for rational product formulation (thereby reducing usage costs) and continuously optimize pectin processing conditions.

Claims

1. A pectin, said pectin having: Degree of esterification (DE) of 15% to 45%; 5% to 30% degree of amidation (DA); and The ratio of the degree of esterification (DE) to the degree of amidation (DA) is between 0.5 and 9.

0.

2. The pectin according to claim 1, wherein the pectin has a galacturonic acid (GalA) content of 85% or higher, or 90% or higher, or 85% to 95%, or 88% to 94%, or 93.0%.

3. The pectin according to claim 1, wherein the pectin has a galacturonic acid (GalA) content 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%.

4. The pectin according to any one of claims 1 to 3, wherein: The degree of esterification (DE) is 18% to 40%, or 20% to 35%, or 23% to 31%, or 23.3% to 31.0%. The degree of amidation (DA) is 12% to 25%, or 15% to 23%, or 16.0% to 22.1%; and / or The ratio of 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.

5. The pectin according to claim 1, claim 2, or claim 4, wherein: The degree of esterification (DE) is 15% to 28%, or 19% to 26%, or 21% to 25%, or 22% to 24%, or 23.3%; The degree of amidation (DA) is 5% to 30%, or 10% to 25%, or 20% to 23%, or 22.1%; and / or, The ratio of the degree of esterification (DE) to the degree of amidation (DA) is 0.5 to 1.5, or 0.75 to 1.25, or 0.9 to 1.1, or 1.05; The pectin therein has a galacturonic acid (GalA) content of 85% or higher, or 90% or higher, or 85% to 95%, or 88% to 94%, or 93.0%.

6. The pectin according to claim 5, wherein: The degree of esterification (DE) is 23.3%; The degree of amidation (DA) is 22.1%; and The ratio of the degree of esterification (DE) to the degree of amidation (DA) is 1.05; and The galacturonic acid (GalA) content is 93.0%.

7. The pectin according to claim 5 or claim 6, wherein the pectin is derived from citrus peel.

8. The pectin according to claim 1, claim 3, or claim 4, wherein: The degree of esterification (DE) is 25% to 35%, or 30% to 32%, or 31.0%; The degree of amidation (DA) is 10% to 20%, or 12.5% ​​to 17.5%, or 16.0%; 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, The pectin therein has a galacturonic acid (GalA) content 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%.

9. The pectin according to claim 8, wherein: The degree of esterification (DE) is 31.0%; The degree of amidation (DA) is 16.0%; The ratio of the degree of esterification (DE) to the degree of amidation (DA) is 1.94; The galacturonic acid (GalA) content is 59.0%; and / or, The pectin mentioned above is derived from apple pomace.

10. The pectin according to any one of claims 1 to 9, 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; and / or The pectin is a low-methoxyl (LM) amidated pectin, and optionally the low-methoxyl (LM) amidated pectin has a methylation degree of less than 50%.

11. The use of pectin in food and / or beverage products according to any one of claims 1 to 10, Optionally, the food and / or beverage products mentioned are dairy products, confectionery products, reduced-sugar jam products, fruit products, and coatings.

12. A method for preparing pectin according to any one of claims 1 to 10, 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; and, The amidated low-methoxyl (LM) pectin is dried to form pectin; Optionally, 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.

13. A composition comprising: Pectin; and, water; in, The pectin is the pectin according to any one of claims 1 to 10; Optionally, 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 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.

14. Use of the composition according to claim 13 in food and / or beverage products, Optionally, the food and / or beverage product is a dairy product.

15. A method for preparing the composition according to claim 13, the method comprising: Provides pectin; The pectin is combined with water to form a composition; Wherein, the pectin is the pectin according to any one of claims 1 to 10; Optionally, the composition comprises the pectin at the following concentrations: 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.

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