CN106800610A - A kind of preparation method of middle gelling beet pectin - Google Patents
A kind of preparation method of middle gelling beet pectin Download PDFInfo
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- CN106800610A CN106800610A CN201710042930.7A CN201710042930A CN106800610A CN 106800610 A CN106800610 A CN 106800610A CN 201710042930 A CN201710042930 A CN 201710042930A CN 106800610 A CN106800610 A CN 106800610A
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- 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
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Abstract
The invention discloses a kind of preparation method of middle gelling beet pectin, following steps are specifically included：S1. pre-process beet dry pulp, then through boiling, go out enzyme, acid extraction obtains extract and beet dry pulp waste residue, and the extract decolouring removal of impurities is obtained into upper prop liquid；S2. by the upper prop liquid water-bath, it is concentrated in vacuo to obtain concentrate；S3. the concentrate is cooled down, adjusts pH to 9.5 10, insulation, the 5h of cross-linking reaction 3 obtains reaction solution；S4. the reaction solution is cooled down, with the analysis of mixed liquor neutralized alcohol, adjusts pH to 4.0 4.5, be incubated 2h, press dry to obtain middle gelling beet pectin wet product and filtrate, dry the middle gelling beet pectin wet product, obtained final product.Preparation process is simple of the present invention, low production cost, the middle gelling beet pectin quality of production is high.
Description
Technical field
The invention belongs to pectin extraction technical field, more particularly to a kind of preparation method of middle gelling beet pectin.
Background technology
Beet pectin ordinary meaning refers to the plain edition pectin for not making degree of gelation requirement, conventionally produced or modified at present
Beet pectin prepared by method, the degree of gelation index to be reached is all below 100, and complex process, high cost.
Number of patent application 201611152719.2 discloses a kind of preparation method of gelling beet pectin high, and height gelling is sweet
Dish pectin is on the basis of low gelling pectin, to be obtained by two step chemical modifications, degree of gelation between 140~170, although
Excellent performance, can meet the requirement of in the market high-end customer, but technique is relative complex, and cost is of a relatively high.
Client's (particularly domestic correspondent) in the market is big to the pectin demand of degree of gelation 110-130, although tangerine
Skin, apple low-ester pectin can meet the demand of portions of client, but its complex process, and production cost is high.
In sum, propose that one kind has technique relatively easy, low cost, used device is saved, and degree of gelation is 110~130
Between beet pectin preparation method it is significant.
The content of the invention
In view of the defect that above-mentioned prior art is present, the purpose of the present invention is to propose to a kind of preparation of middle gelling beet pectin
Method, preparation process is simple of the present invention, low production cost, used device is saved, and the middle gelling beet pectin quality of production is high.
The purpose of the present invention will be achieved by the following technical programs：
A kind of preparation method of middle gelling beet pectin, specifically includes following steps：S1. the beet of beet dry pulp is pre-processed
Wet slag A, then beet wet slag B is obtained through boiling, the enzyme that goes out, acid extraction obtains extract and beet dry pulp waste residue, and the extract is decolourized
Removal of impurities obtains upper prop liquid；S2. by the upper prop liquid water-bath, it is concentrated in vacuo to obtain concentrate；S3. the concentrate is cooled down, adjusts pH
To 9.5-10, insulation, cross-linking reaction 3-5h obtains reaction solution；S4. the reaction solution is cooled down, with mixed liquor, then alcohol analysis is adjusted
Section pH to 4.0-4.5, is incubated 2h, press dry to obtain middle gelling beet pectin wet product and filtrate, dries the middle gelling beet pectin wet
Product, obtain final product.
The preparation method of above-mentioned a kind of middle gelling beet pectin, wherein, acid extraction described in S1 specifically includes following step
Suddenly：Plus go from water, 86-90 DEG C is heated to, stirring adds the beet wet slag B, adjusts pH value to 1.0-1.5, insulation, extraction
3 hours, obtain the extract.
The preparation method of above-mentioned a kind of middle gelling beet pectin, wherein, decolouring removal of impurities described in S1 specifically includes as follows
Step：The extract is diluted with water, upper prop k15 particle charcoal posts, 20~25ml/min of coutroi velocity obtains the upper prop liquid.
The preparation method of above-mentioned a kind of middle gelling beet pectin, wherein, bath temperature is 82-87 DEG C, vacuum in S2
It is ＞ -0.085WPA.
The preparation method of above-mentioned a kind of middle gelling beet pectin, wherein, concentrate is cooled to 23-27 DEG C described in S3；
The pH adjusting agent is food-grade ammonia spirit.
The preparation method of above-mentioned a kind of middle gelling beet pectin, wherein, reaction solution described in S4 is cooled to 0 DEG C.
The preparation method of above-mentioned a kind of middle gelling beet pectin, wherein, mixed liquor is hydrochloric acid, n-butanol and water in S4,
The hydrochloric acid: n-butanol: water is 20: 20: 60.
The preparation method of above-mentioned a kind of middle gelling beet pectin, wherein, mixed liquor described in S4 and the reaction solution
Amount ratio is 4.9-5.1: 1.
The purpose that mixed liquor is added in S4 of the present invention is excess of ammonia water when neutralizing cross-linking reaction.
Compared with prior art, the preparation method of a kind of middle gelling beet pectin that the present invention is provided, the technology effect for reaching
It is really：1st, gelling beet pectin quality is good and stable during the present invention is obtained：A, appearance luster are all shallow milk Huang, and compare tangerine peel
Deep yellow and apple low-ester pectin the light red of pectin can more be approved for market；B, degree of gelation are more than 110, and traditional handicraft is given birth to
Tangerine peel, the apple low-ester pectin degree of gelation of product are all between 100~110；2nd, low production cost, middle gelling beet pectin compared to
Tangerine peel pectin, apple low-ester pectin, production cost per ton can save 2~30,000 yuan, and the equipment investment of identical scale production quantities it is small by 3,
Simple production process, the present invention can separate out beet pectin after cross-linking reaction is modified, and be reduced using big relative to traditional handicraft
Amount ethanol carries out alcohol analysis step and obtains beet pectin；In sum, preparation method of the invention is middle gelling beet pectin entrance
Market provides superiority condition.
Below just in conjunction with the embodiments, specific embodiment of the invention is described in further detail, so that technical scheme is more
Should be readily appreciated that, grasp.
Specific embodiment
Below by specific embodiment, the present invention will be described, but the invention is not limited in this.In following embodiments
The experimental technique, unless otherwise specified, is conventional method；The reagent and material, unless otherwise specified, can be from business
Approach is obtained, and example below simultaneously is not used to limit the scope of the claims of the invention, all equivalence enforcements without departing from carried out by the present invention
Or change, it is intended to be limited solely by this patent protection domain.
Beet pectin ordinary meaning refers to the plain edition pectin for not making degree of gelation requirement, and the present invention presses the most important work(of pectin
Beet pectin is divided into low gelling, middle gelling, gelling high by energy index-degree of gelation, is defined as follows：
1st, the beet pectin of low gelling beet pectin, i.e. degree of gelation between 20~30 (uses U.S. FDA pectin degree of gelation
Assay method USA SAG)；
2nd, middle gelling beet pectin, i.e. beet pectin of the degree of gelation between 110~130；
3rd, the beet pectin of gelling beet pectin, i.e. degree of gelation high between 140~170.
Embodiment 1
Pretreatment weighs 100g beet dry pulps, is put into 2000ml beakers, the water 2000ml that addition has been boiled, and stirs 5 points
Clock, after soaking 1 hour, is pressed dry, plus 500ml clear water is washed one time, then is pressed dry, and is repeated once, obtains beet wet slag A；
Boiling, go out enzyme：Plus 2000ml is gone in water to 2000ml beakers, 75 DEG C are heated to, stirring adds above-mentioned beet wet
Slag A is warmed up to 85 DEG C, insulation boiling 1 hour, and filter bag press filtration is to dry, plus the washing of 500ml clear water, then extracts, and repeats once,
Obtain beet wet slag B；
Acid extraction：Plus 2000ml is gone in water to 2000ml beakers, 86 DEG C are heated to, stirring adds beet wet slag B,
Again plus concentration 30-32% food grade hydrochloric acid 20ml, pH value 1.0-1.5 is adjusted, then insulation extraction 3 hours is extracted extract, must be extracted
Take liquid 1680ml and beet waste residue；
Decolouring removal of impurities：Above-mentioned extract is diluted with water to 4000ml, upper prop K15 particles charcoal post (QXH=5cm × 50cm)
20~25ml/min of coutroi velocity, obtains upper prop liquid 3800ml；
Vacuum concentration：By the water-bath of aforesaid liquid 85, more than -0.085WPA vacuums, 950ml is concentrated into；
Modification cross-linking reaction：Above-mentioned concentrate ice-water bath is cooled to 25 DEG C, plus food-grade ammonia spirit, pH is adjusted to respectively
9th, 9.5,9.6,9.7,9.8,9.9,10,25 DEG C ± 2 DEG C, insulation modification cross-linking reaction 4 hours；
Separate：Above-mentioned reaction solution 1000ml ice-water baths are cooled to 0 DEG C, plus 200ml mixed liquors (hydrochloric acid: n-butanol: water=
20: 20: 60) neutralized alcohol analysis, pH is adjusted to 4.0~4.5, it is incubated, after 2 hours, extrudes to dry, filter residue, soaked with 95% ethanol 300ml
Foam washing is washed half an hour, then is extracted, and is repeated once, obtains middle gelling beet pectin wet product, and filtrate is neutralized to pH7~7.5, essence
Recovery n-butanol is evaporated, use is returned；
Drying, finished product：By middle gelling beet pectin wet product, 65 DEG C, more than -0.085mpa vacuums, vacuum drying 2.5~
Pulverize and sieve within 3 hours, obtain middle gelling beet pectin finished product.
Optimum PH range selection in the modification cross-linking reaction of embodiment 2
Optimum PH range selection in the modification cross-linking reaction of table 1
After concentrate ammonification water, its concentrate appearance determination standard：Indicate that crystallization is separated out with " 1 ", " 0 " is indicated without knot
Partial crystallization goes out；
As shown in Table 1, in cross-linking reaction is modified, add the optimum range of food-grade ammonia spirit regulation pH for 9.5~
10。
Be gelled beet pectin in the preparation of embodiment 3
Pretreatment weighs 100g beet dry pulps, is put into 2000ml beakers, the water 2000ml that addition has been boiled, and stirs 5 points
Clock, after soaking 1 hour, is pressed dry, plus 500ml clear water is washed one time, then is pressed dry, and is repeated once, obtains beet wet slag A 270g；
Boiling, go out enzyme：Plus 2000ml is gone in water to 2000ml beakers, 75 DEG C are heated to, stirring adds above-mentioned beet wet
Slag A is warmed up to 85 DEG C, insulation boiling 1 hour, and filter bag press filtration is to dry, plus the washing of 500ml clear water, then extracts, and repeats once,
Beet wet slag B 265g are obtained,
Acid extraction：Plus 2000ml is gone in water to 2000ml beakers, 90 DEG C are heated to, stirring adds beet wet slag B,
Again plus the food grade hydrochloric acid 20ml of concentration 32%, pH value 1.5 is adjusted, then insulation extraction 3 hours extracts extract, obtain extract
1680ml and beet waste residue；
Decolouring removal of impurities：Above-mentioned extract is diluted with water to 4000ml, upper prop K15 particles charcoal post (QXH=5cm × 50cm)
Coutroi velocity 25ml/min, obtains upper prop liquid 3800ml；
Vacuum concentration：By 85 DEG C of water-baths of aforesaid liquid, more than -0.085WPA vacuums, 950ml is concentrated into；
Modification cross-linking reaction：Above-mentioned concentrate ice-water bath is cooled to 26 DEG C, plus food-grade ammonia spirit, pH to 9.5 is adjusted
Between, 26 DEG C of insulations modify cross-linking reaction 4 hours, obtain reaction solution 1500ml；
Separate：Above-mentioned reaction solution 1500ml ice-water baths are cooled to 0 DEG C, plus 300ml mixed liquors (hydrochloric acid: n-butanol: water=
20: 20: 60) neutralized alcohol analysis, pH is adjusted to 4.5, it is incubated, after 2 hours, extrudes to dry, filter residue, soaked with 95% ethanol 300ml and washed
Wash half an hour, then extract, repeat once, obtain middle gelling beet pectin wet product 62g, filtrate neutralizes pH to 7.5, and rectifying is returned
N-butanol is received, use is returned；
Drying, finished product：By middle gelling beet pectin wet product, more than 65 DEG C, -0.085mpa vacuums, vacuum drying 3 is small
When pulverize and sieve, obtain middle gelling beet pectin 15.2g.
Be gelled beet pectin in the preparation of embodiment 4
Pretreatment：100g beet dry pulps are weighed, is put into 2000ml beakers, the water 2000ml that addition has been boiled stirs 5 points
Clock, after soaking 1 hour, is pressed dry, plus 500ml clear water is washed one time, then is pressed dry, and is repeated once, obtains beet wet slag A 268g；
Boiling, go out enzyme：Plus 2000ml is gone in water to 2000ml beakers, 75 DEG C are heated to, stirring adds above-mentioned beet wet
Slag is warmed up to 85 DEG C, insulation boiling 1 hour, and filter bag press filtration is to dry, plus the washing of 500ml clear water, then extracts, and repeats once,
Obtain beet wet slag B 262g；
Acid extraction：Plus 2000ml is gone in water to 2000ml beakers, 88 DEG C are heated to, stirring adds beet wet slag B,
Again plus the food grade hydrochloric acid 20ml of concentration 30%, the insulation extraction 3 hours of 1.0,88 DEG C of pH value is adjusted, extract is then extracted, must be extracted
Liquid 1638ml and beet waste residue；
Decolouring removal of impurities：Above-mentioned extract is diluted with water to 4000ml, upper prop K15 particles charcoal post (QXH=5cm × 50cm)
Coutroi velocity 20ml/min, obtains upper prop liquid 3850ml；
Vacuum concentration：By the water-bath of aforesaid liquid 85, more than -0.085WPA vacuums, 930ml is concentrated into；
Modification cross-linking reaction：Above-mentioned concentrate ice-water bath is cooled to 27 DEG C, plus food-grade ammonia spirit, pH to 9.8 is adjusted
Between, 27 DEG C of insulations modify cross-linking reaction 4 hours, obtain reaction solution 1200ml；
Separate：Above-mentioned reaction solution 1200ml ice-water baths are cooled to 0 DEG C, plus 240ml mixed liquors (hydrochloric acid: n-butanol: water=
20: 20: 60) neutralized alcohol analysis, pH is adjusted to 4.0, and insulation, alcohol analysis after 2 hours, are extruded to dry, filter residue, are soaked with 95% ethanol 300ml
Foam washing is washed half an hour, then is extracted, and is repeated once, obtains middle gelling beet pectin wet product 63.5g, filtrate, and it is 7 to be neutralized to pH,
N-butanol is reclaimed in rectifying, returns use；
Drying, finished product：By middle gelling beet pectin wet product, 65 DEG C, more than -0.085mpa vacuums, vacuum drying 2.5 is small
When pulverize and sieve, obtain middle gelling beet pectin 15.2g.
Be gelled beet pectin in the preparation of embodiment 5
Pretreatment weighs 100g beet dry pulps, is put into 2000ml beakers, the water 2000ml that addition has been boiled, and stirs 5 points
Clock, after soaking 1 hour, is pressed dry, plus 500ml clear water is washed one time, then is pressed dry, and is repeated once, obtains beet wet slag A 273g；
Boiling, go out enzyme：Plus 2000ml is gone in water to 2000ml beakers, 75 DEG C are heated to, stirring adds above-mentioned beet wet
Slag is warmed up to 85 DEG C, insulation boiling 1 hour, and filter bag press filtration is to dry, plus the washing of 500ml clear water, then extracts, and repeats once,
Obtain beet wet slag B 270g；
Acid extraction：Plus 2000ml is gone in water to 2000ml beakers, 87 DEG C are heated to, stirring adds above-mentioned beet wet
Slag B, then add the food grade hydrochloric acid of concentration 31%, pH is adjusted to 1.2,87 DEG C, then insulation extraction 3 hours extracts extract, must extract
Liquid 1686ml and beet waste residue；
Decolouring removal of impurities：Above-mentioned extract is diluted with water to 4000ml, upper prop K15 particles charcoal post (QXH=5cm × 50cm)
Coutroi velocity 23ml/min, obtains upper prop liquid 3750ml；
Vacuum concentration：By 85 DEG C of water-baths of aforesaid liquid, more than -0.085WPA vacuums, 958ml is concentrated into；
Modification cross-linking reaction：Above-mentioned concentrate ice-water bath is cooled to 26 DEG C, plus food-grade ammonia spirit, pH is adjusted to 9.8,
26 DEG C of insulations modify cross-linking reaction 4 hours；
Separate：Above-mentioned reaction solution 1380ml ice-water baths are cooled to 0 DEG C, plus 280ml mixed liquors (hydrochloric acid: n-butanol: water=
20: 20: 60) neutralized alcohol analysis, pH is adjusted to 4.3, and insulation, alcohol analysis after 2 hours, are extruded to dry, filter residue, are soaked with 95% ethanol 300ml
Foam washing is washed half an hour, then is extracted, and is repeated once, obtains middle gelling beet pectin wet product 62g.Filtrate, neutralizes to pH7.5, essence
Recovery n-butanol is evaporated, use is returned；
Drying, finished product：By middle gelling beet pectin wet product, 65 DEG C, more than -0.085mpa vacuums, vacuum drying 2.8 is small
When pulverize and sieve, obtain middle gelling beet pectin 15.4g.
Be gelled beet pectin performance test in embodiment 6, the results are shown in Table 2
Be gelled beet pectin performance test in table 2
Note：The grams of gelling beet pectin in the beet dry pulp production of yield=100 gram.
With pectin indices of the prior art be compared beet pectin prepared by the present invention by embodiment 7, as a result
It is shown in Table 3.
Table 3 compares beet pectin with pectin of the prior art
Note：Beet pectin 1 is according to the beet pectin obtained by preparation method of the present invention；Beet pectin 2 is according to traditional work
Beet pectin obtained by skill.
Described above has shown and described some preferred embodiments of the invention, but as previously described, it should be understood that the present invention
Be not limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and can be used for various other combinations,
Modification and environment, and can be in invention contemplated scope described herein, by above-mentioned teaching or the technology or knowledge of association area
It is modified.And the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention, then all should be in this hair
In the protection domain of bright appended claims.
Claims (8)
1. it is a kind of it is middle gelling beet pectin preparation method, it is characterised in that specifically include following steps：S1. beet is pre-processed
The beet wet slag A of the dry dregs of rice, then beet wet slag B is obtained through boiling, the enzyme that goes out, acid extraction obtains extract and beet dry pulp waste residue, will be described
Extract decolouring removal of impurities obtains upper prop liquid；S2. by the upper prop liquid water-bath, it is concentrated in vacuo to obtain concentrate；S3. it is the concentrate is cold
But, pH to 9.5-10 is adjusted, insulation, cross-linking reaction 3-5h obtains reaction solution；S4. the reaction solution is cooled down, is neutralized with mixed liquor
Alcohol is analysed, and adjusts pH to 4.0-4.5, is incubated 2h, press dry to obtain middle gelling beet pectin wet product and filtrate, dries the middle gelling beet
Pectin wet product, obtains final product.
2. it is according to claim 1 it is a kind of it is middle gelling beet pectin preparation method, it is characterised in that described in S1 acid extraction
Take and specifically include following steps：Plus go from water, 86-90 DEG C is heated to, stirring adds the beet wet slag B, adjusts pH value extremely
1.0-1.5, insulation is extracted 3 hours, obtains the extract.
3. it is according to claim 2 it is a kind of it is middle gelling beet pectin preparation method, it is characterised in that described in S1 decolourize
Removal of impurities specifically includes following steps：The extract is diluted with water, upper prop k15 particle charcoal posts, 20~25ml/ of coutroi velocity
Min, obtains the upper prop liquid.
4. it is according to claim 1 it is a kind of it is middle gelling beet pectin preparation method, it is characterised in that bath temperature in S2
It it is 82-87 DEG C, vacuum is ＞ -0.085WPA.
5. it is according to claim 4 it is a kind of it is middle gelling beet pectin preparation method, it is characterised in that described in S3 concentrate
Liquid is cooled to 23-27 DEG C；The pH adjusting agent is food-grade ammonia spirit.
6. it is according to claim 4 it is a kind of it is middle gelling beet pectin preparation method, it is characterised in that described in S4 react
Liquid is cooled to 0 DEG C.
7. it is according to claim 4 it is a kind of it is middle gelling beet pectin preparation method, it is characterised in that mixed liquor is in S4
Hydrochloric acid, n-butanol and water, the hydrochloric acid: n-butanol: water is 20: 20: 60.
8. it is according to claim 4 it is a kind of it is middle gelling beet pectin preparation method, it is characterised in that described in S4 mix
The amount ratio 5: 1 of liquid and the reaction solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417936A (en) * | 2022-10-23 | 2022-12-02 | 华南理工大学 | Method for extracting pectin from waste beet pulp after sugar production by double-enzyme method |
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| CN1052027A (en) * | 1990-08-29 | 1991-06-12 | 黑龙江省红光糖厂 | Prepare the pectin new method by beet pulp |
| CN1016937B (en) * | 1987-09-24 | 1992-06-10 | 大同市新技术开发研究所 | Method for producing modified beet pectine |
| CN104725527A (en) * | 2013-12-18 | 2015-06-24 | 中粮营养健康研究院有限公司 | Beet pectin and extraction method thereof |
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2017
- 2017-01-20 CN CN201710042930.7A patent/CN106800610A/en active Pending
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| CN1016937B (en) * | 1987-09-24 | 1992-06-10 | 大同市新技术开发研究所 | Method for producing modified beet pectine |
| CN1052027A (en) * | 1990-08-29 | 1991-06-12 | 黑龙江省红光糖厂 | Prepare the pectin new method by beet pulp |
| CN104725527A (en) * | 2013-12-18 | 2015-06-24 | 中粮营养健康研究院有限公司 | Beet pectin and extraction method thereof |
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| 文奋武等: "甜菜渣提取果胶的研究——酸法萃取、乙醇沉淀工艺", 《兰州大学学报(自然科学版)》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417936A (en) * | 2022-10-23 | 2022-12-02 | 华南理工大学 | Method for extracting pectin from waste beet pulp after sugar production by double-enzyme method |
| CN115417936B (en) * | 2022-10-23 | 2023-04-07 | 华南理工大学 | Method for extracting pectin from waste beet pulp after sugar production by double-enzyme method |
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