CN104211831A - Preparation method of low-methoxyl pectin - Google Patents
Preparation method of low-methoxyl pectin Download PDFInfo
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Abstract
The invention relates to a method for preparing low-methoxyl pectin from sunflower heads in an extraction manner. The method includes following steps: with air-dried sunflower heads as a raw material, crushing the sunflower heads; sieving the sunflower heads through a 60-mesh standard sieve; performing pre-treatment for removing pigments, impurities and soluble polysaccharide; washing the sunflower heads until water is clear; adding an extracting solution according to a feed liquid ratio of 1:30; adding proper amounts of cellulose and hemicellulase to the extracting solution; performing room-temperature hydrolysis for 30 min; adding the pH value of the extraction liquid to 3.0; adding a proper amount of ammonium oxalate for extraction; performing solid-liquid separation to obtain a pectin extract; performing sheet frame filtration to the extract for removing impurities and then performing concentration; adding acidized alcohol to a concentrated solution for carrying out alcohol-extraction; performing filtration; washing a precipitate with ethanol for 2-3 times; and performing a vacuum-drying process to obtain a pectin product. The method is simple in technology, is low in production cost, is high in safety of the product, is good in extraction yield and purity and is suitable for industrialized production.
Description
Technical field
The invention belongs to medicine and food industrial technical field, be specifically related to a kind of preparation method of low-methoxy pectin.
Background technology
1825, Frenchman Bracennot extracted a kind of material first from Radix Dauci Sativae meat, and this material can form gel, and Bracennot, by its extract called after " pectin ", is called " pectin " in Chinese.Pectin is a kind of hydrophilic plant glue, its main component is D-galacturonic acid, the World Food Programme (FAO) and European Union (EU) regulation, pectin must containing the galacturonic acid of >=65%, extensively be present in green terrestrial plant intercellular substance, fix moisture by its pectisation, there is the effect in conjunction with plant tissue together with fiber.Pectin is the main component of food fibre in human body seven major nutrient, there is good diarrhea, anticancer, effect such as treatment diabetes and fat-reducing etc., and pectin has good gelation and emulsifying stability, being widely used in the food industry, is also medicine and the indispensable auxiliary material of cosmetic industry.Commodity pectin can be divided into two large classes by gamma value (esterified hydroxy groups number accounts for the percentage of total hydroxyl value) difference, low-ester pectin (low-methoxy pectin, Low Methoxyl Pectin, LMP, methoxy content is less than 7%, and namely gamma value is less than 42.9) and high ester pectin (high methoxyl pectin, High Methoxyl Pectin, HMP, methoxy content is greater than 7%, and namely gamma value is greater than 42.9).
The extraction of pectin mainly contains acid extraction method, ion-exchange-resin process, enzymolysis process, microwave―assisted extraction and microbial method etc. at present.It is used that the oxalate denominationby of ammonium oxalate has very strong metal-chelating, can by the water-insoluble pectin extraction that formed with calcium ion chelating in plant cell wall out.In addition, because ammonium oxalate is a kind of weakly alkaline salt, to the pollution of environment well below strong acid and strong base, in actual production, will be far smaller than traditional acid system to the corrosion of equipment, therefore, available ammonium oxalate is as extraction agent industrial abstract pectin.
Sunflower Receptacle and soybean, rape, peanut, sesame are the large oil crops of China five.Sunflower Receptacle has the good characteristics such as breeding time short, high yield, high-quality, low cost, Salt And Alkali Tolerance, drought-resistant, wide adaptability, under the condition that cultivation step is extensive, still can obtain good harvest.Sunflower Receptacle Potential Comprehensive Utilization is large, and except sunflower seed oil expression, going pectin content in the sunflower plate of seed up to 17% ~ 25%, is good natural low-methoxy pectin source.
Summary of the invention
The object of the present invention is to provide a kind of high-efficiency environment friendly, simple, cost is lower, is suitable for the preparation method of a kind of low-methoxy pectin of suitability for industrialized production.Adopt traditional acidity extraction pectin, not only extraction efficiency is low, and equipment corrosion-vulnerable, environmental pollution is larger, it is used that the oxalate denominationby of ammonium oxalate has very strong metal-chelating, by the water-insoluble pectin extraction that formed with calcium ion chelating in plant cell wall out, a kind of preparation method of low-methoxy pectin can be the invention provides.
The invention provides a kind of preparation method of low-methoxy pectin, the method comprises the steps: raw materials pretreatment, enzymolysis, lixiviate, filtration, decolouring, concentrated, precipitation, washing, drying and crushing and byproduct processing;
It specifically comprises:
(1) raw materials pretreatment: choose air-dry after remove seed sunflower plate, with vegetable drug pulverizer pulverize after, cross 60 mesh standard sieves; Take sunflower plate powder 30g and be placed in container, under be 10.0 temperature being the condition of 70 DEG C at pH, soak 15-20min, then centrifugal 5 minutes of 200 turns/min, collecting precipitation and liquid;
(2) enzymolysis: adding deionized water 900ml in step (1) gained precipitation, add 100U cellulase and 60U hemicellulase wherein, is then 4.5-5.0 with the salt acid for adjusting pH value of 1M, room temperature enzymolysis 30min;
(3) lixiviate: the pH of the enzymolysis solution obtained with the sulfuric acid regulating step (2) of 1M is 3.0, then adds ammonium oxalate 7.2g until completely dissolved, is that extraction 4h is stirred in 85 DEG C of Water Under baths in temperature;
(4) filter: extracting solution step (3) obtained carries out solid-liquid separation in centrifugal 3 minutes through 4000 turns/min, collect supernatant liquor, supernatant liquor collects filtered liquid and impurity through Plate Filtration;
(5) decolour: in step (4) gained filtered liquid, add gac 7g, then adjust ph is 7.0, and under temperature is 50 DEG C of conditions, is incubated 30min carries out desolventing technology, then filtering and impurity removing obtains pectin extracting soln;
(6) concentrated: the pectin extracting soln after decolouring is concentrated into 1/3 of original solution volume through ceramic membrane ultrafitration, obtains concentrated solution;
(7) precipitate: add in concentrated solution account for concentrated solution cumulative volume 1% the hydrochloric acid of 1M, then add isopyknic 95% (V/V) ethanol with concentrated solution, after at room temperature precipitating 4h, collected by filtration;
(8) wash: 80% (V/V) washing with alcohol 2 times adding two volumes in gained precipitation, through screw press after washing, remove unnecessary alcohol and water, obtain wet product pectin;
(9) drying and crushing: by step (8) gained wet product pectin dry 12-15h under 60-65 DEG C, 0.17Mpa condition, after pulverizing, namely packaging obtains low-methoxy pectin;
(10) byproduct processing: step (1) gained liquid and step (4) gained impurity are mixed to get mixture A, then in mixture A, add Semen Maydis powder, sorghum flour, bean dregs and wheat bran, interpolation limit, limit is stirred to pasty state; Finally pass into steam and be warming up to 110 DEG C, distill 15 minutes; Then by after distillment oven dry, pulverizing, add zinc sulfate, vitamin-E and chlorogenic acid, mix, obtain pig feed; Wherein, Semen Maydis powder, sorghum flour, bean dregs and wheat bran account for 7%, 6%, 3% and 2% of mixture A quality respectively, zinc sulfate, vitamin-E and chlorogenic acid account for respectively mixture A quality ten thousand/.
Compared with existing pectous extracting method technology, advantage of the present invention mainly comprises:
(1) adopt ammonium oxalate extraction process, compared with traditional acid system, not only reduce the corrosion to equipment, the more important thing is the protection be environment;
(2) carrying out the method for enzymolysis by adding Mierocrystalline cellulose and hemicellulose prozyme, being conducive to the release of pectin substance in cell, thus effectively raising pectin extraction rate;
(3) compared with traditional vacuum method of enrichment, adopt mineral membrane to be separated ultrafiltration and concentration technology and not only effectively reduce energy consumption, and its operating procedure is simple, the sugar impurity in pectin extracting soln and oligopolymer can be removed simultaneously, thus improve the quality of pectin, also without the need to heating, to pectin quality not damaged;
(4) due to the present invention with the sunflower plate of main producing region, Xinjiang for raw material, go pectin content in the sunflower plate of seed up to 17% ~ 25%, it is good natural low-methoxy pectin source, by enzymolysis and ammonium oxalate compound collecting, production cost can be effectively reduced, product meets the World Food Programme (FAO) and European Union (EU) regulation, also meet the standard of the foodstuff additive pectin of China GB 25533-2010, can directly come into the market as products in circulation.
(5) the present invention efficiently utilizes refuse, has prepared pig feed, has achieved and turn waste into wealth.
Embodiment
Based on above extracting method, below technical solution of the present invention concrete operations are described in detail, but protection scope of the present invention is not only confined to described example, just further illustrates of the present invention.
Embodiment 1
A preparation method for low-methoxy pectin, the method comprises the steps: raw materials pretreatment, enzymolysis, lixiviate, filtration, decolouring, concentrated, precipitation, washing, drying and crushing and byproduct processing;
(1) raw materials pretreatment: choose air-dry after remove seed sunflower plate, with vegetable drug pulverizer pulverize after, cross 60 mesh standard sieves; Take sunflower plate powder 30g and be placed in container, under be 10.0 temperature being the condition of 70 DEG C at pH, soak 15min, then centrifugal 5 minutes of 200 turns/min, collecting precipitation and liquid;
(2) enzymolysis: adding deionized water 900ml in step (1) gained precipitation, add 100U cellulase and 60U hemicellulase wherein, is then 4.5 with the salt acid for adjusting pH value of 1M, room temperature enzymolysis 30min;
(3) lixiviate: the pH of the enzymolysis solution obtained with the sulfuric acid regulating step (2) of 1M is 3.0, then adds ammonium oxalate 7.2g until completely dissolved, is that extraction 4h is stirred in 85 DEG C of Water Under baths in temperature;
(4) filter: extracting solution step (3) obtained carries out solid-liquid separation in centrifugal 3 minutes through 4000 turns/min, collect supernatant liquor, supernatant liquor collects filtered liquid and impurity through Plate Filtration;
(5) decolour: in step (4) gained filtered liquid, add gac 7g, then adjust ph is 7.0, and under temperature is 50 DEG C of conditions, is incubated 30min carries out desolventing technology, then filtering and impurity removing obtains pectin extracting soln;
(6) concentrated: the pectin extracting soln after decolouring is concentrated into 1/3 of original solution volume through ceramic membrane ultrafitration, obtains concentrated solution;
(7) precipitate: add in concentrated solution account for concentrated solution cumulative volume 1% the hydrochloric acid of 1M, then add isopyknic 95% (V/V) ethanol with concentrated solution, after at room temperature precipitating 4h, collected by filtration;
(8) wash: 80% (V/V) washing with alcohol 2 times adding two volumes in gained precipitation, through screw press after washing, remove unnecessary alcohol and water, obtain wet product pectin;
(9) drying and crushing: by step (8) gained wet product pectin at 60 DEG C, dry 12h under 0.17Mpa condition, after pulverizing, namely packaging obtains low-methoxy pectin;
(10) byproduct processing: step (1) gained liquid and step (4) gained impurity are mixed to get mixture A, then in mixture A, add Semen Maydis powder, sorghum flour, bean dregs and wheat bran, interpolation limit, limit is stirred to pasty state; Finally pass into steam and be warming up to 110 DEG C, distill 15 minutes; Then by after distillment oven dry, pulverizing, add zinc sulfate, vitamin-E and chlorogenic acid, mix, obtain pig feed; Wherein, Semen Maydis powder, sorghum flour, bean dregs and wheat bran account for 7%, 6%, 3% and 2% of mixture A quality respectively, zinc sulfate, vitamin-E and chlorogenic acid account for respectively mixture A quality ten thousand/.
After testing, extraction low-methoxy pectin is 3.69kg, and extraction yield is 12.3%, and it is 88.7% that galacturonic acid system measures purity.
Embodiment 2
A preparation method for low-methoxy pectin, the method comprises the steps: raw materials pretreatment, enzymolysis, lixiviate, filtration, decolouring, concentrated, precipitation, washing, drying and crushing and byproduct processing;
(1) raw materials pretreatment: choose air-dry after remove seed sunflower plate, with vegetable drug pulverizer pulverize after, cross 60 mesh standard sieves; Take sunflower plate powder 30g and be placed in container, under be 10.0 temperature being the condition of 70 DEG C at pH, soak 20min, then centrifugal 5 minutes of 200 turns/min, collecting precipitation and liquid;
(2) enzymolysis: adding deionized water 900ml in step (1) gained precipitation, add 100U cellulase and 60U hemicellulase wherein, is then 5.0 with the salt acid for adjusting pH value of 1M, room temperature enzymolysis 30min;
(3) lixiviate: the pH of the enzymolysis solution obtained with the sulfuric acid regulating step (2) of 1M is 3.0, then adds ammonium oxalate 7.2g until completely dissolved, is that extraction 4h is stirred in 85 DEG C of Water Under baths in temperature;
(4) filter: extracting solution step (3) obtained carries out solid-liquid separation in centrifugal 3 minutes through 4000 turns/min, collect supernatant liquor, supernatant liquor collects filtered liquid and impurity through Plate Filtration;
(5) decolour: in step (4) gained filtered liquid, add gac 7g, then adjust ph is 7.0, and under temperature is 50 DEG C of conditions, is incubated 30min carries out desolventing technology, then filtering and impurity removing obtains pectin extracting soln;
(6) concentrated: the pectin extracting soln after decolouring is concentrated into 1/3 of original solution volume through ceramic membrane ultrafitration, obtains concentrated solution;
(7) precipitate: add in concentrated solution account for concentrated solution cumulative volume 1% the hydrochloric acid of 1M, then add isopyknic 95% (V/V) ethanol with concentrated solution, after at room temperature precipitating 4h, collected by filtration;
(8) wash: 80% (V/V) washing with alcohol 2 times adding two volumes in gained precipitation, through screw press after washing, remove unnecessary alcohol and water, obtain wet product pectin;
(9) drying and crushing: by step (8) gained wet product pectin at 65 DEG C, dry 15h under 0.17Mpa condition, after pulverizing, namely packaging obtains low-methoxy pectin;
(10) byproduct processing: step (1) gained liquid and step (4) gained impurity are mixed to get mixture A, then in mixture A, add Semen Maydis powder, sorghum flour, bean dregs and wheat bran, interpolation limit, limit is stirred to pasty state; Finally pass into steam and be warming up to 110 DEG C, distill 15 minutes; Then by after distillment oven dry, pulverizing, add zinc sulfate, vitamin-E and chlorogenic acid, mix, obtain pig feed; Wherein, Semen Maydis powder, sorghum flour, bean dregs and wheat bran account for 7%, 6%, 3% and 2% of mixture A quality respectively, zinc sulfate, vitamin-E and chlorogenic acid account for respectively mixture A quality ten thousand/.
After testing, extraction low-methoxy pectin is 3.72kg, and extraction yield is 12.4%, and purity is 88.6%.
Embodiment 3
The Performance Detection of byproduct pig feed of the present invention:
Choose a month large weanling pig 200, be divided into two groups, often organize 100, the wherein diet prepared by the embodiment of the present invention 1 of experimental group, every 50kg about 250 yuan, control group with honest feed (SSB-25 model), according to the about 300 yuan of calculating of every 50kg.Raise after 6 weeks and detect indices see table 1.
Table 1
| Index (every piglet) | Control group | Of the present invention group |
| Weanling pig body weight (kg) | 5.37 | 5.42 |
| Within 6 weeks, put on weight (kg) | 12.98 | 13.24 |
| Survive number | 91 | 95 |
| Consume feed (kg) | 15.5 | 16.1 |
| Feed for nursing cost (unit) | 93 | 80.5 |
Pig feed cost prepared by the present invention is cheap compared with market common feedstuffs, and feeding effect is good, and belongs to the recycle again of refuse, achieves and turns waste into wealth, energy-saving and emission-reduction.
Finally, it is also to be noted that what enumerate above is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (3)
1. a preparation method for low-methoxy pectin, is characterized in that, described preparation method comprises the steps: raw materials pretreatment, enzymolysis, lixiviate, filtration, decolouring, concentrated, precipitation, washing, drying and crushing and byproduct processing.
2. preparation method as claimed in claim 1, it is characterized in that, described preparation method comprises the steps:
(1) raw materials pretreatment: choose air-dry after remove seed sunflower plate, with vegetable drug pulverizer pulverize after, cross 60 mesh standard sieves; Take sunflower plate powder 30g and be placed in container, under be 10.0 temperature being the condition of 70 DEG C at pH, soak 15-20min, then centrifugal 5 minutes of 200 turns/min, collecting precipitation and liquid;
(2) enzymolysis: adding deionized water 900ml in step (1) gained precipitation, add 100U cellulase and 60U hemicellulase wherein, is then 4.5-5.0 with the salt acid for adjusting pH value of 1M, room temperature enzymolysis 30min;
(3) lixiviate: the pH of the enzymolysis solution obtained with the sulfuric acid regulating step (2) of 1M is 3.0, then adds ammonium oxalate 7.2g until completely dissolved, is that extraction 4h is stirred in 85 DEG C of Water Under baths in temperature;
(4) filter: extracting solution step (3) obtained carries out solid-liquid separation in centrifugal 3 minutes through 4000 turns/min, collect supernatant liquor, supernatant liquor collects filtered liquid and impurity through Plate Filtration;
(5) decolour: in step (4) gained filtered liquid, add gac 7g, then adjust ph is 7.0, and under temperature is 50 DEG C of conditions, is incubated 30min carries out desolventing technology, then filtering and impurity removing obtains pectin extracting soln;
(6) concentrated: the pectin extracting soln after decolouring is concentrated into 1/3 of original solution volume through ceramic membrane ultrafitration, obtains concentrated solution;
(7) precipitate: add in concentrated solution account for concentrated solution cumulative volume 1% the hydrochloric acid of 1M, then add isopyknic 95% (V/V) ethanol with concentrated solution, after at room temperature precipitating 4h, collected by filtration;
(8) wash: 80% (V/V) washing with alcohol 2 times adding two volumes in gained precipitation, through screw press after washing, remove unnecessary alcohol and water, obtain wet product pectin;
(9) drying and crushing: by step (8) gained wet product pectin dry 12-15h under 60-65 DEG C, 0.17Mpa condition, after pulverizing, namely packaging obtains low-methoxy pectin;
(10) byproduct processing.
3. preparation method as claimed in claim 1 or 2, it is characterized in that, the processing of described step (10) byproduct comprises the steps: step (1) gained liquid and step (4) gained impurity to be mixed to get mixture A, then in mixture A, add Semen Maydis powder, sorghum flour, bean dregs and wheat bran, interpolation limit, limit is stirred to pasty state; Finally pass into steam and be warming up to 110 DEG C, distill 15 minutes; Then by after distillment oven dry, pulverizing, add zinc sulfate, vitamin-E and chlorogenic acid, mix, obtain pig feed; Wherein, Semen Maydis powder, sorghum flour, bean dregs and wheat bran account for 7%, 6%, 3% and 2% of mixture A quality respectively, zinc sulfate, vitamin-E and chlorogenic acid account for respectively mixture A quality ten thousand/.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884928A (en) * | 2016-04-26 | 2016-08-24 | 华中农业大学 | Method using ammonium exchange method to prepare low-methoxyl pectin |
| CN108402252A (en) * | 2018-05-17 | 2018-08-17 | 大连民族大学 | A kind of Schisandra chinensis multiple elements design tea beverage |
| CN110357986A (en) * | 2019-06-21 | 2019-10-22 | 杨晓军 | A kind of preparation method of low fat pectin |
| CN110386993A (en) * | 2019-08-15 | 2019-10-29 | 上海辉文生物技术股份有限公司 | A kind of cape jasmine fruit pectin and preparation method thereof and the application in food processing |
| CN111303312A (en) * | 2019-09-09 | 2020-06-19 | 侯士国 | Low-methoxy pectin of Ficus awkeotsang Makino and preparation method thereof |
| CN111333070A (en) * | 2020-03-10 | 2020-06-26 | 天津科技大学 | Method for utilizing all components of sunflower disc raw material |
| CN113501891A (en) * | 2021-05-17 | 2021-10-15 | 淮北凯乐生物科技有限公司 | Preparation process and application of micromolecule pectin |
| 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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| CN103073657A (en) * | 2013-01-15 | 2013-05-01 | 中北大学 | Method for manufacturing sunflower low-fat pectins |
| CN103641930A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from pineapple peels and residue by enzymatic process |
| CN103641931A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from pineapple peels and residue |
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| CN1034659A (en) * | 1987-12-31 | 1989-08-16 | 云南省轻工业科学研究所 | From papaya, extract edible pectin |
| CN103073657A (en) * | 2013-01-15 | 2013-05-01 | 中北大学 | Method for manufacturing sunflower low-fat pectins |
| CN103641930A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from pineapple peels and residue by enzymatic process |
| CN103641931A (en) * | 2013-11-27 | 2014-03-19 | 威海市桢昊生物技术有限公司 | Method for extraction of pectin from pineapple peels and residue |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884928B (en) * | 2016-04-26 | 2018-05-25 | 华中农业大学 | A kind of method that ammonium exchange process prepares low-ester pectin |
| CN105884928A (en) * | 2016-04-26 | 2016-08-24 | 华中农业大学 | Method using ammonium exchange method to prepare low-methoxyl pectin |
| CN108402252A (en) * | 2018-05-17 | 2018-08-17 | 大连民族大学 | A kind of Schisandra chinensis multiple elements design tea beverage |
| CN110357986A (en) * | 2019-06-21 | 2019-10-22 | 杨晓军 | A kind of preparation method of low fat pectin |
| CN110386993A (en) * | 2019-08-15 | 2019-10-29 | 上海辉文生物技术股份有限公司 | A kind of cape jasmine fruit pectin and preparation method thereof and the application in food processing |
| CN111303312B (en) * | 2019-09-09 | 2022-05-31 | 侯士国 | Low-methoxy pectin of Ficus awkeotsang Makino and preparation method thereof |
| CN111303312A (en) * | 2019-09-09 | 2020-06-19 | 侯士国 | Low-methoxy pectin of Ficus awkeotsang Makino and preparation method thereof |
| CN111333070A (en) * | 2020-03-10 | 2020-06-26 | 天津科技大学 | Method for utilizing all components of sunflower disc raw material |
| CN111333070B (en) * | 2020-03-10 | 2022-09-16 | 天津科技大学 | Method for utilizing whole components of sunflower disc raw material |
| CN113501891A (en) * | 2021-05-17 | 2021-10-15 | 淮北凯乐生物科技有限公司 | Preparation process and application of micromolecule pectin |
| CN113501891B (en) * | 2021-05-17 | 2024-04-09 | 淮北凯乐生物科技有限公司 | Preparation process and application of small molecule pectin |
| 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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