CN117088996A - Low-ester pectin with high gelation degree and preparation and application thereof in gel - Google Patents
Low-ester pectin with high gelation degree and preparation and application thereof in gel Download PDFInfo
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- CN117088996A CN117088996A CN202311011227.1A CN202311011227A CN117088996A CN 117088996 A CN117088996 A CN 117088996A CN 202311011227 A CN202311011227 A CN 202311011227A CN 117088996 A CN117088996 A CN 117088996A
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- 239000001814 pectin Substances 0.000 title claims abstract description 146
- 229920001277 pectin Polymers 0.000 title claims abstract description 146
- 235000010987 pectin Nutrition 0.000 title claims abstract description 146
- 238000001879 gelation Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000001035 drying Methods 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 230000032050 esterification Effects 0.000 claims abstract description 25
- 238000005886 esterification reaction Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 17
- 239000006228 supernatant Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 150000005846 sugar alcohols Chemical class 0.000 claims abstract description 12
- 230000001376 precipitating effect Effects 0.000 claims abstract description 11
- 230000001105 regulatory effect Effects 0.000 claims abstract description 11
- 241000207199 Citrus Species 0.000 claims abstract description 8
- 235000020971 citrus fruits Nutrition 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000499 gel Substances 0.000 claims description 61
- 239000000243 solution Substances 0.000 claims description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 150000002148 esters Chemical class 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 15
- 238000005119 centrifugation Methods 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 239000007853 buffer solution Substances 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 235000015110 jellies Nutrition 0.000 claims description 5
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 229910001424 calcium ion Inorganic materials 0.000 claims description 4
- 235000009508 confectionery Nutrition 0.000 claims description 4
- 239000008274 jelly Substances 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000005979 Citrus limon Nutrition 0.000 claims description 3
- 244000131522 Citrus pyriformis Species 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 240000000560 Citrus x paradisi Species 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- CEVCTNCUIVEQOY-STXHBLNNSA-N fumagillol Chemical compound C([C@@H](O)[C@H](C1[C@]2(C)[C@H](O2)CC=C(C)C)OC)C[C@@]21CO2 CEVCTNCUIVEQOY-STXHBLNNSA-N 0.000 abstract description 3
- 238000006911 enzymatic reaction Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- 239000004386 Erythritol Substances 0.000 description 9
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 description 9
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 description 9
- 229940009714 erythritol Drugs 0.000 description 9
- 235000019414 erythritol Nutrition 0.000 description 9
- 239000004744 fabric Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 108090000790 Enzymes Proteins 0.000 description 5
- 102000004190 Enzymes Human genes 0.000 description 5
- 206010016807 Fluid retention Diseases 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 238000007605 air drying Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000007068 beta-elimination reaction Methods 0.000 description 2
- 238000010170 biological method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 229940069078 citric acid / sodium citrate Drugs 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000005809 transesterification reaction Methods 0.000 description 2
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 229920001586 anionic polysaccharide Polymers 0.000 description 1
- 150000004836 anionic polysaccharides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000011942 biocatalyst Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000003278 egg shell Anatomy 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 235000004280 healthy diet Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 235000015094 jam Nutrition 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 108020004410 pectinesterase Proteins 0.000 description 1
- 239000008055 phosphate buffer solution Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 230000021317 sensory perception Effects 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 235000013618 yogurt Nutrition 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/231—Pectin; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G3/00—Sweetmeats; Confectionery; Marzipan; Coated or filled products
- A23G3/34—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
- A23G3/36—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by the composition containing organic or inorganic compounds
- A23G3/42—Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by the composition containing organic or inorganic compounds characterised by the carbohydrates used, e.g. polysaccharides
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L21/00—Marmalades, jams, jellies or the like; Products from apiculture; Preparation or treatment thereof
- A23L21/10—Marmalades; Jams; Jellies; Other similar fruit or vegetable compositions; Simulated fruit products
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
- C08B37/0048—Processes of extraction from organic materials
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Molecular Biology (AREA)
- Nutrition Science (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention belongs to the technical field of pectin, and discloses low-ester pectin with high gelation degree, and preparation and application thereof in gel. The preparation method of the high-gelation low-ester pectin comprises the following steps: 1) Mixing citrus peel residue with water, adjusting the pH to 1.5-2, extracting at 65-75 ℃, centrifuging, taking supernatant, performing alcohol precipitation washing, filtering, drying and crushing to obtain primary pectin; 2) And re-dissolving the primary pectin, regulating the pH value to be 0.5-1.1, reacting at 40-60 ℃, precipitating with alcohol, washing, drying and crushing to obtain the low-ester pectin. The method is simple and easy to operate, saves cost and is suitable for industrial production; the prepared low-ester pectin keeps a relatively complete pectin original structure, the esterification degree is 25-35%, the gelation degree is 120-150, and the low-ester pectin is obviously superior to low-ester pectin prepared by an alkaline method and an enzymatic method. The low-ester pectin is used for preparing gel, and the formed sugarless gel and sugar alcohol gel have higher hardness and water retention rate.
Description
Technical Field
The invention belongs to the technical field of pectin preparation, and particularly relates to a high-gelation low-ester pectin, a preparation method thereof and application thereof in sugarless gel and sugar alcohol gel.
Background
Pectin is a structurally complex anionic polysaccharide that is widely found in the intercellular layer and primary walls of higher plant cell walls. Pectin consists essentially of three domains, including HG, RG-I, RG-II. Pectin is classified into high-ester pectin (DE. Gtoreq.50%) and low-ester pectin (DE < 50%) based on the number of ester groups on HG main chain.
Pectin is widely used as a food additive in the food fields of jam, jelly, candy and the like. In addition, pectin can be used as bioactive substances in the field of pharmacy by reducing blood cholesterol, inhibiting atherosclerosis, etc.
The gel ability of pectin is of great significance to the structure adjustment and sensory perception of pectin-added foods such as jams, jellies and candies. Gel strength is therefore a great important criterion for measuring pectin quality. Different types of pectins tend to have different gel behaviour and mechanisms. High ester pectin is required to form a gel under a relatively severe environment (high acid and high sugar) by virtue of hydrophobic forces and hydrogen bonds between methoxy groups in the pectin chain. The low-ester pectin provides more binding sites for calcium ions due to the increase of carboxyl content in the pectin chain, and is more beneficial to forming a stable eggshell structure. Even at a broad acidity range, even under at least sugar or sugarless conditions, low ester pectin forms a gel with calcium alone. And the lower the esterification degree of the low-ester pectin is, the more favorable the formation of a gel permeation network structure is. Therefore, compared with high-ester pectin, the low-ester pectin has greater advantages in the application aspect of gel performance, and accords with the concept of healthy diet of consumers.
Pectin obtained by primary extraction of citrus peel residues is mostly high-ester pectin through detection. To expand its application, high ester pectins are usually subjected to transesterification by chemical and biological methods. The chemical method comprises acid treatment and alkali treatment, wherein the alkali treatment has the most remarkable effect of reducing the ester, but the molecular weight of pectin is greatly reduced due to the beta-elimination reaction in the process of reducing the ester, and the pectin structure is destroyed so as not to form gel or the formed gel degree is lower. Biological methods usually use biocatalysts to assist in reducing the ester by using the methylester, however, in the mass industrialized production, the enzyme consumption greatly increases the production cost, so that the application of the enzyme method in the industry is limited. However, these methods of reducing esters focus on the reduction of the degree of esterification alone, and have low interest in the application value of pectin after its ester reduction.
The application value of low-ester pectin is closely related to the gel property. The low-ester pectins on the market are generally defined only in terms of the degree of esterification, and their most important application property, gel properties, is often ignored. The gel properties of low-ester pectins are important in different fields of application. The low-ester pectin with good application value has the gelatinization degree of over 110 on the basis of meeting the esterification degree of less than 50 percent. In other words, the gel of the low-ester pectin does not reach a certain gelatinization degree or does not have the gelatinization property, and the application value of the gel is greatly reduced. For example, the dairy industry mainly utilizes the gel properties of low-ester pectins to apply low-ester pectins in stirred yogurt, and is consumed in large quantities. Therefore, the research of low-ester pectin cannot only pay attention to the esterification degree range, and the gel performance is an important standard for measuring the industrial application of the low-ester pectin.
The invention is based on the low-ester pectin with the same esterification degree category, ensures that the pectin has good gel performance, and reaches the product application standard.
Disclosure of Invention
In view of the above drawbacks and deficiencies of the prior art, a primary object of the present invention is to provide a low-ester pectin with a high degree of gelation and a process for preparing the same.
It is a further object of the present invention to provide the use of a low ester pectin as described above. The low-ester pectin is used for preparing sugarless gel and/or sugar alcohol gel. The low-ester pectin disclosed by the invention is also applied to jelly, jam and soft sweets.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for preparing a low-ester pectin with high gelation degree, which comprises the following steps:
(1) Mixing citrus peel residue with water, adding acid to adjust the pH value to 1.5-2, extracting at 65-75 ℃, centrifuging, taking supernatant, carrying out alcohol precipitation washing, filtering, drying and crushing the precipitate to obtain primary pectin; the extraction is carried out under stirring;
(2) Re-dissolving the primary pectin obtained in the step (1), adding acid to adjust the pH value to 0.5-1.1, reacting at 40-60 ℃, precipitating with alcohol, washing, drying and crushing the precipitate to obtain the low-ester pectin.
The citrus peel residue in the step (1) is one or more of lemon peel residue, orange peel residue, pomelo peel residue and orange peel residue; the ratio of the citrus peel residue to the water is 1: (20-30).
The extraction time in the step (1) is 1-2.5 h.
The centrifugation in the step (1) means centrifugation at 8000-10000 rpm for 10-20 min.
The re-dissolution in the step (2) means that primary pectin is added into water to make the pectin concentration be 2-3wt%; the redissolution time is 1-3 h.
The reaction time in the step (2) is 60-72 h.
The acid in the step (1) and the step (2) is at least one of nitric acid, oxalic acid, hydrochloric acid and citric acid.
The precipitating agents of the alcohol precipitation in the step (1) and the step (2) are respectively ethanol solutions, the volume concentration purity of the ethanol solutions is not lower than 95%, and the volume ratio of the supernatant (concentrated solution) to the ethanol solutions is 1: (1-3); the sedimentation time is 0.5-1.5 h; the washing times are 1-3 times.
And (3) adjusting the pH value to 3.5-4 by adopting an alkali solution before the second alcohol washing in the step (2).
The drying in the step (1) and the step (2) respectively refer to forced air drying, rake drying or fluidized bed drying; the drying temperature is 50-65 ℃; the drying time is 1-4 h.
The esterification degree of the primary pectin is 55% -65%; the molecular weight is 500-600 kDa; the gelation degree is 200-220.
The esterification degree of the low-ester pectin prepared by the invention is 25% -35%; the gelation degree is 120-150.
The low ester pectin is used to prepare a gel.
The gel is prepared by the following method: and (3) re-dissolving the low-ester pectin, regulating the pH value of the pectin solution by using a buffer solution, boiling the mixed solution at high temperature, adding sugar alcohol or calcium chloride solution, and standing to obtain sugar alcohol gel or sugarless gel (namely the zero-sucrose low-ester pectin gel).
The esterification degree of the low-ester pectin is 25% -35%; the mass concentration of the pectin solution after re-dissolution is 1% -2%.
The buffer solution is a mixed solution of 60wt% of citric acid solution and 2.5M sodium hydroxide solution, and the volume ratio of the 60wt% of citric acid solution to the 2.5M sodium hydroxide solution is 3:1.
the pH is adjusted to 3-3.3.
After the calcium chloride is added, the content of calcium ions in the final gel system is 50-60 mg/g pectin.
The sugar alcohol is added in an amount of 0-30 g/100g gel.
The standing refers to that the thermal gel is cooled to room temperature and then is placed for 24 hours at 20-30 ℃.
The hardness of the low-ester pectin sugarless gel and the sugar alcohol gel prepared by the invention is 61.87g and 99.74g, and the water retention rate is as high as 97.73% and 98.92%.
Compared with the prior art, the invention has the following advantages:
(1) The acid incubation method of the invention carries out the transesterification reaction at a relatively mild temperature, reduces the hydrolysis reaction and the beta-elimination reaction as much as possible, and can relatively completely retain the original structure of pectin.
(2) The whole implementation flow of the acid incubation method is simple, convenient and easy to operate, is economical and feasible, and is easy for industrial production.
(3) The esterification degree of the low-ester pectin extracted by the method is 25-35%, belongs to low-ester pectin, and the gelation degree after standardization is 120-150, which is obviously superior to that of an alkaline method and an enzymatic method.
(4) The sugar-free gel and the sugar alcohol gel formed by the low-ester pectin prepared by the invention have higher hardness and water retention rate.
Drawings
FIG. 1 is a graph showing the morphology of gels formed from low ester pectins of examples 1-3 and comparative examples 1-3 according to the present invention; the gel in FIG. 1 is prepared from low ester pectin according to the SAG method in QS 2484-2000.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
The method for measuring the esterification degree is carried out by referring to a chemical titration method in food safety national standard GB 25533-2010.
The degree of gelation was measured according to the jelly SAG method (SAG method) specified in the light industry Standard QS 2484-2000.
Example 1
(1) 40g of orange peel residues are weighed and dissolved in 800g of water, stirred and mixed uniformly, the pH value of a concentrated nitric acid regulating system is added to be 1.7, the mixture is stirred and extracted for 1.5 hours in a water bath kettle at 70 ℃, the reacted pectin suspension is centrifuged for 15 minutes at 9000rpm, the supernatant after centrifugation is precipitated by 2 times of 95% ethanol, the supernatant is left for 1 hour and washed by alcohol again, the pectin precipitate is obtained by filtering with 400-mesh filter cloth, and the pectin precipitate is obtained by crushing, wherein the esterification degree is 57.63%, the molecular weight is 562kDa and the gelation degree is 209.48 after forced air drying (the drying temperature is 60 ℃ and the drying time is 3.5 hours).
(2) Weighing 6g of primary pectin obtained in the step (1), dissolving in 200g of water to obtain a 3% pectin solution, fully dissolving, adding concentrated nitric acid to adjust the pH value of the solution to 0.7, stirring in a water bath kettle at 40 ℃ for reaction for 72 hours, precipitating the reacted concentrated solution with 95% ethanol with 2 times of volume, adjusting the pH value of a mixed system to 3.5 with an ammonia water solution, standing for 1 hour, washing with alcohol again, filtering with 400-mesh filter cloth to obtain pectin precipitate, drying with air blast (the drying temperature is 60 ℃ for 3.5 hours), and crushing to obtain pectin esterification degree 29.04% and gelation degree 125.93.
Example 2
(1) 40g of orange peel residues are weighed and dissolved in 800g of water, stirred and mixed uniformly, the pH value of a concentrated nitric acid regulating system is added to be 2.0, stirred and extracted for 2 hours in a water bath kettle at 75 ℃, the reacted pectin suspension is centrifuged for 20 minutes at 8000rpm, the supernatant after centrifugation is precipitated by 3 times of 95% ethanol, the supernatant is subjected to secondary alcohol washing after standing for 1 hour, the pectin precipitate is obtained by filtering with 400-mesh filter cloth, and primary pectin is obtained by crushing, wherein the esterification degree is 56.45%, the molecular weight is 555kDa and the gelation degree is 220.82 after rake drying (the drying temperature is 65 ℃ and the drying time is 3 hours).
(2) Weighing 12g of primary pectin obtained in the step (1), dissolving in 400g of water to obtain a 3% pectin solution, fully dissolving, adding concentrated nitric acid to adjust the pH value of the solution to 0.5, stirring in a water bath kettle at 45 ℃ for reaction for 66 hours, precipitating the reacted concentrated solution with 95% ethanol with 3 times of volume, adjusting the pH value of a mixed system to 3.8 with sodium hydroxide solution, standing for 1 hour, washing with alcohol again, filtering with 400-mesh filter cloth to obtain pectin precipitate, drying with a rake (the drying temperature is 65 ℃ for 3 hours), and crushing to obtain the pectin esterification degree 29.09% and the gelation degree 124.08.
Example 3
(1) 40g of orange peel residues are weighed and dissolved in 800g of water, stirred and mixed uniformly, the pH value of a concentrated nitric acid regulating system is added to be 1.5, the mixture is stirred and extracted for 1.5 hours in a water bath kettle at 70 ℃, the reacted pectin suspension is centrifuged for 15 minutes at 8000rpm, the supernatant after centrifugation is precipitated by 3 times of 95% ethanol, the supernatant is left for 1 hour and washed by alcohol again, the pectin precipitate is obtained by filtering with 400-mesh filter cloth, the pectin precipitate is dried by a fluidized bed (the drying temperature is 60 ℃ and the drying time is 4 hours), primary pectin is obtained by crushing, the esterification degree is 57.99%, the molecular weight is 578kDa, and the gelation degree is 222.97.
(2) Weighing 12g of primary pectin obtained in the step (1), dissolving in 400g of water to obtain a 3% pectin solution, fully dissolving, adding concentrated nitric acid to adjust the pH value of the solution to 0.9, stirring in a water bath kettle at 40 ℃ for reaction for 72 hours, precipitating the reacted concentrated solution with 95% ethanol with 3 times of volume, adjusting the pH value of a mixed system to 4.0 with sodium carbonate solution, standing for 1 hour, washing with alcohol again, filtering with 400-mesh filter cloth to obtain pectin precipitate, drying with a fluidized bed (the drying temperature is 60 ℃, the drying time is 4 hours), and crushing to obtain pectin with the esterification degree of 30.21% and the gelation degree of 120.75.
Comparative example 1
The low-ester pectin is prepared by adopting an alkali treatment method.
(1) Primary pectin was obtained on the basis of step (1) of example 1.
(2) Weighing 12g of primary pectin obtained in the step (1), dissolving in 400g of water to obtain a 3% pectin solution, adding 15mL of 2.5M NaOH solution after full dissolution, stirring in a water bath kettle at 30 ℃ for reaction for 1.5h, and adding 5mL of concentrated nitric acid after reaction for continuous reaction for 3h. Precipitating the reacted concentrated solution with 95% ethanol with 2 times volume, regulating pH value of the mixed system to 3.5 with ammonia water solution, standing for 1 hr, washing with alcohol again, filtering with 400 mesh filter cloth to obtain pectin precipitate, air drying (drying temperature is 60deg.C, drying time is 3.5 hr), pulverizing to obtain pectin with esterification degree of 24.62% and gelatinization degree of 100.00.
Comparative example 2
The low-ester pectin is prepared by adopting an enzyme treatment method.
(1) Primary pectin was obtained on the basis of step (1) of example 2.
(2) Weighing 12g of primary pectin obtained in the step (1), dissolving in 400g of phosphate buffer solution, regulating the pH value of the solution to 3.5, adding 200 mu L of pectin methylesterase after the primary pectin is fully dissolved in a water bath kettle at 50 ℃ for reacting for 1.5h, and heating at 95 ℃ for 5min to inactivate enzymes. Precipitating the reacted concentrated solution with 95% ethanol with 3 times volume, regulating pH value of the mixed system to 3.8 with sodium hydroxide solution, standing for 1 hr, washing with alcohol again, filtering with 400 mesh filter cloth to obtain pectin precipitate, harrowing, drying (drying temperature 65 deg.C for 3 hr), pulverizing to obtain pectin with esterification degree of 30.99% and gelatinization degree of 105.34.
Comparative example 3
The low-ester pectin is prepared by adopting a citric acid/sodium citrate method.
10g of lemon peel residue is weighed and dissolved in 250mL of citric acid/sodium citrate buffer solution with pH value of 8, stirred in a water bath kettle with the temperature of 85 ℃ for reaction for 2 hours, the reacted pectin suspension is centrifuged for 15 minutes at 8000rpm, the supernatant after centrifugation is precipitated by 3 times of 95% ethanol, meanwhile, the pH value of a mixed system is adjusted to be 4.0 by sodium carbonate solution, the mixture is stood for 1 hour, washed by alcohol for the second time, the pectin precipitate is obtained by filtering by 400-mesh filter cloth, and is dried by a fluidized bed (the drying temperature is 60 ℃ and the drying time is 4 hours), and the pectin is crushed to obtain the pectin esterification degree of 32.16 percent, so that gel cannot be formed.
The physicochemical parameters of the pectins prepared in examples 1 to 3 and comparative examples 1 to 3 are shown in Table 1.
Table 1 physicochemical parameters of pectins prepared in examples 1 to 3 and comparative examples 1 to 3
As is clear from Table 1, the esterification degree of the low-ester pectin obtained was about 29% + -5%. However, the degree of gelation varies greatly. The degree of gelation in examples 1 to 3 was 120 to 130, whereas comparative examples 1 and 2 had degrees of gelation of only 100.00 and 105.34, and comparative example 3 could not even form a gel. Therefore, the low-ester pectin prepared by the invention has remarkable superiority in gelling capability.
FIG. 1 is a graph showing the morphology of gels formed from low ester pectins of examples 1-3 and comparative examples 1-3 in accordance with the present invention.
The sugarless gel and the sugar alcohol gel were applied as described in example 1 below, and examples 1 to 3 in CN 111602804B were used as comparative examples 4 to 6 of the present invention.
Example 4
1.5g of the low-ester pectin obtained in example 1 is weighed and fully dissolved in 75mL of distilled water, a buffer solution consisting of 60% (w/v) citric acid and 2.5M sodium hydroxide is used for adjusting the pH of the solution to 3.3, 12.5mL of 1.66% (w/v) anhydrous calcium chloride solution (the content of calcium ions in a final gel system is 50mg/g pectin) is added in the mixture solution through boiling, and the mass of the boiled gel is 150g; cooling the thermocoagulant solution to 25 ℃ and standing for 24 hours to obtain the low-ester sugarless gel.
Example 5
The difference from example 4 is only that 15g of erythritol are added after the mixture is boiled, so that the mass ratio of erythritol in the final gel system is 10%.
Example 6
The difference from example 4 is only that 30g of erythritol is added after the mixture is boiled, so that the mass ratio of erythritol in the final gel system is 20%.
Example 7
The difference from example 4 is only that 45g of erythritol is added after the mixture is boiled, so that the mass ratio of erythritol in the final gel system is 30%.
Comparative example 4
CN 111602804B example 1.
Comparative example 5
CN 111602804B example 2.
Comparative example 6
CN 111602804B example 3.
Hardness testing:
measured using a cylindrical probe having a diameter of 0.5 inches. The gel was compressed at a constant speed of 1.0mm/s until 50% of the initial height was reached.
Water retention test:
the gel was allowed to stand at 4℃for 24 hours and then centrifuged at 8000rpm for 10 minutes using a centrifuge. The water thrown out was sucked up with filter paper, and the mass of the gel before centrifugation was recorded as M 1 After centrifugation the mass of the gel was recorded as M 2 . The water holding capacity of the gel is calculated according to the following formula: water holding ratio=m 2 /M 1 ×100％。
The hardness and water holding ratios of examples 4 to 7 and comparative examples 4 to 6 are shown in Table 2.
TABLE 2 hardness and Water holdup of examples 4-7 and comparative examples 4-6
As can be seen from Table 2, examples 5-7 have higher hardness and higher water retention than example 4, indicating that the addition of a certain amount of erythritol favors gel formation. The hardness and water holding ratio of example 6 were higher than those of examples 5 and 7, indicating that the optimum range of the erythritol addition amount was found, and when the addition amount exceeded the optimum amount, the gel began to weaken and the network structure was unstable. Examples 5-7 the low ester pectin extracted according to the present invention resulted in a higher hardness and a higher water retention of the sugar alcohol gel formed from the low ester pectin compared to comparative examples 4-6 at the same erythritol addition level.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit of the present invention are to be considered as equivalent substitutions, and are included in the scope of the present invention.
Claims (10)
1. A preparation method of low-ester pectin with high gelation degree is characterized by comprising the following steps: the method comprises the following steps:
(1) Mixing citrus peel residue with water, adding acid to adjust the pH value to 1.5-2, extracting at 65-75 ℃, centrifuging, taking supernatant, carrying out alcohol precipitation washing, filtering, drying and crushing the precipitate to obtain primary pectin;
(2) Re-dissolving the primary pectin obtained in the step (1), adding acid to adjust the pH value to 0.5-1.1, reacting at 40-60 ℃, precipitating with alcohol, washing, drying and crushing the precipitate to obtain the low-ester pectin.
2. The method for preparing a high-gelling low-ester pectin according to claim 1, wherein: the extraction time in the step (1) is 1-2.5 h;
the reaction time in the step (2) is 60-72 h.
3. The method for preparing a high-gelling low-ester pectin according to claim 1, wherein:
the citrus peel residue in the step (1) is one or more of lemon peel residue, orange peel residue, pomelo peel residue and orange peel residue; the mass ratio of the citrus peel residue to the water is 1: (20-30);
the extraction in step (1) is carried out under stirring;
the centrifugation in the step (1) means centrifugation at 8000-10000 rpm for 10-20 min;
the re-dissolution in the step (2) means that primary pectin is added into water to make the pectin concentration be 2-3wt%.
4. The method for preparing a high-gelling low-ester pectin according to claim 1, wherein: the precipitating agent for alcohol precipitation in the step (1) is ethanol solution, and the volume concentration of the ethanol solution is more than or equal to 95%; the volume ratio of the supernatant to the ethanol solution is 1: (1-3); the sedimentation time is 0.5-1.5 h; the washing times are 1 to 3 times;
the acid in the step (1) and the step (2) is at least one of nitric acid, oxalic acid, hydrochloric acid and citric acid respectively;
the drying in the step (1) and the step (2) is respectively blast drying, rake drying or fluidized bed drying; the drying temperature is 50-65 ℃; the drying time is 1-4 h.
5. The method for preparing a high-gelling low-ester pectin according to claim 1, wherein: the precipitating agent for alcohol precipitation in the step (2) is ethanol solution, and the volume concentration of the ethanol solution is more than or equal to 95%; the volume ratio of the supernatant to the ethanol solution is 1: (1-3); the washing times are 1-3 times, the pH value of the precipitation system is regulated to 3.5-4 by adopting a regulator before the 2 nd or 3 rd alcohol washing, and then the precipitation system is kept stand for 0.5-1.5 h; the regulator is ammonia water, sodium hydroxide or sodium carbonate solution;
the esterification degree of the primary pectin is 55% -65%; the molecular weight is 500-600 kDa; the gelation degree is 200-220.
6. A high-gelling low-ester pectin obtained by the process according to any one of claims 1 to 5, characterized in that: the esterification degree of the low-ester pectin is 25% -35%; the gelation degree is 120-150.
7. Use of a high gelling degree low ester pectin according to claim 6, wherein: the low ester pectin is used to prepare a gel.
8. The use according to claim 7, characterized in that: the gel is prepared by the following method: and (3) re-dissolving the low-ester pectin, regulating the pH of the pectin solution by using a buffer solution, boiling at a high temperature, adding a sugar alcohol or calcium chloride solution, and standing to obtain sugar alcohol gel or sugarless gel.
9. The use according to claim 8, characterized in that: the esterification degree of the low-ester pectin is 25% -35%; the mass concentration of the pectin solution after re-dissolution is 1% -2%;
the buffer solution is a mixed solution of 60wt% of citric acid solution and 2.5M sodium hydroxide solution, and the volume ratio of the 60wt% of citric acid solution to the 2.5M sodium hydroxide solution is 3:1, a step of;
the pH is regulated to 3 to 3.3;
after the calcium chloride solution is added, the content of calcium ions in a final gel system is 50-60 mg/g pectin;
the standing refers to that the thermal gel is cooled to room temperature and then is placed for 24 hours at 20-30 ℃.
10. Use of a high gelling degree low ester pectin according to claim 6, wherein: the low-ester pectin with high gelatinization degree is applied to jelly, jam and soft sweets.
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