CN104211831B - A kind of preparation method of hypo-methoxy pectin - Google Patents

A kind of preparation method of hypo-methoxy pectin Download PDF

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CN104211831B
CN104211831B CN201410374367.XA CN201410374367A CN104211831B CN 104211831 B CN104211831 B CN 104211831B CN 201410374367 A CN201410374367 A CN 201410374367A CN 104211831 B CN104211831 B CN 104211831B
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CN104211831A (en
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肖勇
李学朋
沈伟伟
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XINJIANG FUFENG BIOTECHNOLOGY CO Ltd
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Abstract

The present invention relates to a kind of method that hypo-methoxy pectin is prepared in extraction from sunflower plate, with the sunflower plate after air-drying as raw material, after size-reduced 60 mesh standard sieves sieve, carry out pretreatment and remove pigment, impurity and soluble polysaccharide;After being washed to clearly, the solid-liquid ratio by 1: 30 adds extracting solution, adds appropriate cellulose and hemicellulase Hydrolysis At Room Temperature 30min in extracting solution;The pH of regulation extracting solution is 3.0, adds the extraction of appropriate ammonium oxalate, obtains pectin extracting soln after solid-liquid separation;Extracting solution concentrates after plate-and-frame filtration remove impurity;Concentrated solution adds acidifying alcohol and carries out alcohol analysis, precipitate 2~3 times by washing with alcohol after filtration, be vacuum dried to obtain pectin product.It is a feature of the present invention that operating procedure is simple, production cost is low, and the safety of product is good, extracts yield and purity is high, be suitable to industrialized production.

Description

A kind of preparation method of hypo-methoxy pectin
Technical field
The invention belongs to medicine and food industrial technical field, be specifically related to the preparation method of a kind of hypo-methoxy pectin.
Background technology
1825, Frenchman Bracennot extracted a kind of material first from Radix Dauci Sativae meat, and this material can be formed solidifying Glue, Bracennot by named for its extract " pectin ", in referred to herein as " pectin ".Pectin is that a kind of hydrophilic is planted Thing glue, its main component is D-galacturonic acid, and the World Food Programme (FAO) and European Union (EU) regulation, pectin must Must be widely present in green terrestrial plant intercellular substance containing the galacturonic acid of >=65%, fix water by its gelation Point, there is together with fiber the effect combining plant tissue.Pectin is the main component of dietary fiber in human body seven major nutrient, There is good diarrhea, anticancer, treatment effect such as diabetes and fat-reducing, and pectin has good gelation and emulsifying is steady Qualitative, it is widely used in the food industry, is also medicine and the indispensable adjuvant of cosmetics industry.Esterification degree pressed by commodity pectin The percentage rate of total hydroxyl value (the esterified hydroxy groups number account for) difference can be divided into two big classes, low methoxyl pectin (hypo-methoxy pectin, Low Methoxyl Pectin, LMP, methoxyl content is less than 7%, i.e. esterification degree is less than 42.9) and high-esterpectin (high methoxyl fruit Glue, High Methoxyl Pectin, HMP, methoxyl content is more than 7%, i.e. esterification degree is more than 42.9).
The extraction of pectin currently mainly has acid extraction method, ion-exchange-resin process, enzymatic isolation method, microwave-assisted extraction and micro-life Thing method etc..The oxalate denominationby of ammonium oxalate has used by the strongest metal-chelating, can will chelate with calcium ion in plant cell wall The water-insoluble pectin extraction formed is out.Further, since ammonium oxalate is a kind of alkalescence salt, to the pollution of environment well below Strong acid and strong base, in actual production, the corrosion to equipment to be far smaller than tradition acid system, and therefore, available ammonium oxalate is as extractant Industrial abstract pectin.
Helianthi and Semen sojae atricolor, Brassica campestris L, Semen arachidis hypogaeae, Semen Sesami are the big oil crop of China five.Helianthi has that period of duration is short, high yield, The good characteristics such as high-quality, low cost, Salt And Alkali Tolerance, drought-resistant, wide adaptability, still can obtain under conditions of cultivation step is extensive Preferably harvest.Helianthi Potential Comprehensive Utilization is big, in addition to Semen Helianthi extracts oil, goes the pectin content in the sunflower plate of seed high Reach 17%~25%, be good natural hypo-methoxy pectin source.
Summary of the invention
It is an object of the invention to provide a kind of high-efficiency environment friendly, simple, cost is relatively low, is suitable to a kind of low first of industrialized production The preparation method of epoxide pectin.Using tradition acidity extraction pectin, not only extraction efficiency is low, and equipment corrosion-vulnerable, to ring Environment pollution is relatively big, and the oxalate denominationby of ammonium oxalate has used by the strongest metal-chelating, can by plant cell wall with calcium ion The water-insoluble pectin extraction that chelating is formed out, the invention provides the preparation method of a kind of hypo-methoxy pectin.
The invention provides the preparation method of a kind of hypo-methoxy pectin, the method comprise the steps: pretreatment of raw material, enzymolysis, Extract, filter, decolour, concentrate, precipitate, wash, drying and crushing and side-product processing;
It specifically includes:
(1) pretreatment of raw material: choose air-dry after remove seed sunflower plate, with vegetable drug pulverizer pulverize after, cross 60 mesh standard sieves; Weigh sunflower plate powder 30g to be placed in container, be under conditions of 10.0 temperature are 70 DEG C at pH, soak 15-20min, then 200 turns/min is centrifuged 5 minutes, collects precipitation and liquid;
(2) enzymolysis: add deionized water 900ml in step (1) gained precipitates, is added thereto to 100U cellulase and 60U half Cellulase, is then 4.5-5.0 with the salt acid for adjusting pH value of 1M, room temperature enzymolysis 30min;
(3) extraction: the pH of the enzymolysis solution obtained with the sulphuric acid regulating step (2) of 1M is 3.0, is subsequently adding ammonium oxalate 7.2g, has treated After CL, under the conditions of temperature is 85 DEG C, stirring in water bath extracts 4h;
(4) filter: extracting solution step (3) obtained is centrifuged 3 minutes through 4000 turns/min and carries out solid-liquid separation, collect supernatant, Supernatant collects filtrate and impurity through plate-and-frame filtration;
(5) decolouring: adding activated carbon 7g in step (4) gained filtrate, then regulation pH value is 7.0, is 50 in temperature Being incubated 30min under the conditions of DEG C and carry out desolventing technology, then filtering and impurity removing obtains pectin extracting soln;
(6) concentrate: the pectin extracting soln after decolouring is concentrated into the 1/3 of original solution volume through ceramic membrane ultrafitration, obtains concentrated solution;
(7) precipitation: add the hydrochloric acid of the 1M of account for concentrated solution cumulative volume 1% in concentrated solution, add isopyknic with concentrated solution 95% (V/V) ethanol, at room temperature after precipitation 4h, is collected by filtration precipitation;
(8) washing: add 80% (V/V) washing with alcohol 2 times of two volumes in gained precipitates, 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 60-65 DEG C, is dried 12-15h, after pulverizing under the conditions of 0.17Mpa Pack and i.e. obtain hypo-methoxy pectin;
(10) side-product processing: step (1) gained liquid and step (4) gained impurity are mixed to get complex A, the most past Adding Semen Maydis powder, Sorghum vulgare Pers. powder, bean dregs and Testa Tritici in complex A, interpolation limit, limit is stirred to pasty state;Finally it is passed through steam to be warming up to 110 DEG C, distill 15 minutes;Then, after distillation drying, pulverizing, zinc sulfate, vitamin E and chlorogenic acid, mixing are added Uniformly, it is thus achieved that pig feed;Wherein, Semen Maydis powder, Sorghum vulgare Pers. powder, bean dregs and Testa Tritici account for the 7% of complex A mass respectively, and 6%, 3 % and 2%, zinc sulfate, vitamin E and chlorogenic acid account for respectively complex A mass ten thousand/.
Compared with existing pectous extracting method technology, advantages of the present invention specifically includes that
(1) use ammonium oxalate extraction process, compared with tradition acid system, not only reduce the corrosion to equipment, it is often more important that it is right to be The protection of environment;
(2) method carrying out enzymolysis by addition cellulose and hemicellulose compound enzyme, the release of the most intracellular pectin substance, from And effectively raise pectin extraction rate;
(3) compared with traditional vacuum concentration method, inoranic membrane separation ultrafiltration concentration technology is used not only to effectively reduce energy consumption, Er Qieqi Operating procedure is simple, can remove the sugar impurity in pectin extracting soln and oligomer simultaneously, thus improve the quality of pectin, also Without heating, to pectin quality not damaged;
(4) owing to the present invention is with the sunflower plate of main producing region, Xinjiang as raw material, go the pectin content in the sunflower plate of seed be up to 17%~ 25%, it is good natural hypo-methoxy pectin source, by enzymolysis and ammonium oxalate compound collecting, it is possible to effectively reduce and produce into This, product meets the World Food Programme (FAO) and European Union (EU) regulation, also complies with the food of China GB 25533-2010 The standard of product additive pectin, it is possible to be directly entered market as products in circulation.
(5) present invention efficiently utilizes refuse, is prepared for pig feed, it is achieved that turn waste into wealth.
Detailed description of the invention
Based on above extracting method, below technical solution of the present invention concrete operations are described in detail, but the protection model of the present invention Enclose and be not limited solely to described example, simply the present invention is further illustrated.
Embodiment 1
A kind of preparation method of hypo-methoxy pectin, the method comprise the steps: pretreatment of raw material, enzymolysis, extract, filter, Decolour, concentrate, precipitate, wash, drying and crushing and side-product processing;
(1) pretreatment of raw material: choose air-dry after remove seed sunflower plate, with vegetable drug pulverizer pulverize after, cross 60 mesh standard sieves; Weigh sunflower plate powder 30g to be placed in container, be under conditions of 10.0 temperature are 70 DEG C at pH, soak 15min, then 200 Turn/min is centrifuged 5 minutes, collects precipitation and liquid;
(2) enzymolysis: add deionized water 900ml in step (1) gained precipitates, is added thereto to 100U cellulase and 60U half Cellulase, is then 4.5 with the salt acid for adjusting pH value of 1M, room temperature enzymolysis 30min;
(3) extraction: the pH of the enzymolysis solution obtained with the sulphuric acid regulating step (2) of 1M is 3.0, is subsequently adding ammonium oxalate 7.2g, has treated After CL, under the conditions of temperature is 85 DEG C, stirring in water bath extracts 4h;
(4) filter: extracting solution step (3) obtained is centrifuged 3 minutes through 4000 turns/min and carries out solid-liquid separation, collect supernatant, Supernatant collects filtrate and impurity through plate-and-frame filtration;
(5) decolouring: adding activated carbon 7g in step (4) gained filtrate, then regulation pH value is 7.0, is 50 in temperature Being incubated 30min under the conditions of DEG C and carry out desolventing technology, then filtering and impurity removing obtains pectin extracting soln;
(6) concentrate: the pectin extracting soln after decolouring is concentrated into the 1/3 of original solution volume through ceramic membrane ultrafitration, obtains concentrated solution;
(7) precipitation: add the hydrochloric acid of the 1M of account for concentrated solution cumulative volume 1% in concentrated solution, add isopyknic with concentrated solution 95% (V/V) ethanol, at room temperature after precipitation 4h, is collected by filtration precipitation;
(8) washing: add 80% (V/V) washing with alcohol 2 times of two volumes in gained precipitates, 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, is dried 12h under the conditions of 0.17Mpa, after pulverizing, packaging is i.e. Obtain hypo-methoxy pectin;
(10) side-product processing: step (1) gained liquid and step (4) gained impurity are mixed to get complex A, the most past Adding Semen Maydis powder, Sorghum vulgare Pers. powder, bean dregs and Testa Tritici in complex A, interpolation limit, limit is stirred to pasty state;Finally it is passed through steam to be warming up to 110 DEG C, distill 15 minutes;Then, after distillation drying, pulverizing, zinc sulfate, vitamin E and chlorogenic acid, mixing are added Uniformly, it is thus achieved that pig feed;Wherein, Semen Maydis powder, Sorghum vulgare Pers. powder, bean dregs and Testa Tritici account for the 7% of complex A mass respectively, and 6%, 3 % and 2%, zinc sulfate, vitamin E and chlorogenic acid account for respectively complex A mass ten thousand/.
After testing, extraction hypo-methoxy pectin is 3.69kg, and extraction ratio is 12.3%, and it is 88.7 that galacturonic acid acid system measures purity %.
Embodiment 2
A kind of preparation method of hypo-methoxy pectin, the method comprise the steps: pretreatment of raw material, enzymolysis, extract, filter, Decolour, concentrate, precipitate, wash, drying and crushing and side-product processing;
(1) pretreatment of raw material: choose air-dry after remove seed sunflower plate, with vegetable drug pulverizer pulverize after, cross 60 mesh standard sieves; Weigh sunflower plate powder 30g to be placed in container, be under conditions of 10.0 temperature are 70 DEG C at pH, soak 20min, then 200 Turn/min is centrifuged 5 minutes, collects precipitation and liquid;
(2) enzymolysis: add deionized water 900ml in step (1) gained precipitates, is added thereto to 100U cellulase and 60U half Cellulase, is then 5.0 with the salt acid for adjusting pH value of 1M, room temperature enzymolysis 30min;
(3) extraction: the pH of the enzymolysis solution obtained with the sulphuric acid regulating step (2) of 1M is 3.0, is subsequently adding ammonium oxalate 7.2g, has treated After CL, under the conditions of temperature is 85 DEG C, stirring in water bath extracts 4h;
(4) filter: extracting solution step (3) obtained is centrifuged 3 minutes through 4000 turns/min and carries out solid-liquid separation, collect supernatant, Supernatant collects filtrate and impurity through plate-and-frame filtration;
(5) decolouring: adding activated carbon 7g in step (4) gained filtrate, then regulation pH value is 7.0, is 50 in temperature Being incubated 30min under the conditions of DEG C and carry out desolventing technology, then filtering and impurity removing obtains pectin extracting soln;
(6) concentrate: the pectin extracting soln after decolouring is concentrated into the 1/3 of original solution volume through ceramic membrane ultrafitration, obtains concentrated solution;
(7) precipitation: add the hydrochloric acid of the 1M of account for concentrated solution cumulative volume 1% in concentrated solution, add isopyknic with concentrated solution 95% (V/V) ethanol, at room temperature after precipitation 4h, is collected by filtration precipitation;
(8) washing: add 80% (V/V) washing with alcohol 2 times of two volumes in gained precipitates, 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, is dried 15h under the conditions of 0.17Mpa, after pulverizing, packaging is i.e. Obtain hypo-methoxy pectin;
(10) side-product processing: step (1) gained liquid and step (4) gained impurity are mixed to get complex A, the most past Adding Semen Maydis powder, Sorghum vulgare Pers. powder, bean dregs and Testa Tritici in complex A, interpolation limit, limit is stirred to pasty state;Finally it is passed through steam to be warming up to 110 DEG C, distill 15 minutes;Then, after distillation drying, pulverizing, zinc sulfate, vitamin E and chlorogenic acid, mixing are added Uniformly, it is thus achieved that pig feed;Wherein, Semen Maydis powder, Sorghum vulgare Pers. powder, bean dregs and Testa Tritici account for the 7% of complex A mass respectively, and 6%, 3 % and 2%, zinc sulfate, vitamin E and chlorogenic acid account for respectively complex A mass ten thousand/.
After testing, extraction hypo-methoxy pectin is 3.72kg, and extraction ratio is 12.4%, and purity is 88.6%.
Embodiment 3
The performance detection of side-product pig feed of the present invention:
Choosing a month big ablactational baby pig 200, be divided into two groups, often group 100, wherein the experimental group present invention implements The diet of example 1 preparation, every 50kg about 250 yuan, matched group is with honest feedstuff (SSB-25 model), according to every 50kg About 300 yuan of calculating.Detect indices after raising 6 weeks and see table 1.
Table 1
Index (every piglet) Matched group Of the present invention group
Ablactational baby pig body weight (kg) 5.37 5.42
Within 6 weeks, put on weight (kg) 12.98 13.24
Survive number 91 95
Consume feedstuff (kg) 15.5 16.1
Feed for nursing cost (first) 93 80.5
Pig feed cost prepared by the present invention is cheap compared with market common feedstuffs, and feeding effect is good, and the recovery again belonging to refuse should With, it is achieved that turn waste into wealth, energy-saving and emission-reduction.
Finally, in addition it is also necessary to be only several specific embodiments of the present invention it is noted that listed above.Obviously, the present invention is not It is limited to above example, it is also possible to have many deformation.Those of ordinary skill in the art directly can lead from present disclosure The all deformation gone out or associate, are all considered as protection scope of the present invention.

Claims (1)

1. the preparation method of a hypo-methoxy pectin, it is characterised in that described preparation method comprises the steps:
Step (1) pretreatment of raw material: choose air-dry after remove seed sunflower plate, with vegetable drug pulverizer pulverize after, cross 60 mesh standard sieves;Weigh to day Certain herbaceous plants with big flowers dish powder 30g is placed in container, is under conditions of 10.0 temperature are 70 DEG C at pH, soaks 15-20min, and then 200 turns/min is centrifuged 5 points Clock, collects precipitation and liquid;
Step (2) enzymolysis: add deionized water 900ml in step (1) gained precipitates, be added thereto to 100U cellulase and 60U hemicellulase, Then it is 4.5-5.0 with the salt acid for adjusting pH value of 1M, room temperature enzymolysis 30min;
Step (3) extracts: the pH of the enzymolysis solution obtained with the sulphuric acid regulating step (2) of 1M is 3.0, is subsequently adding ammonium oxalate 7.2g, until completely dissolved, Under the conditions of temperature is 85 DEG C, stirring in water bath extracts 4h;
Step (4) filters: extracting solution step (3) obtained is centrifuged 3 minutes through 4000 turns/min and carries out solid-liquid separation, collects supernatant, and supernatant is through plate Frame is collected by filtration filtrate and impurity;
Step (5) is decoloured: adding activated carbon 7g in step (4) gained filtrate, then regulation pH value is 7.0, is incubated 30min under the conditions of temperature is 50 DEG C Carrying out desolventing technology, then filtering and impurity removing obtains pectin extracting soln;
Step (6) concentrates: the pectin extracting soln after decolouring is concentrated into the 1/3 of original solution volume through ceramic membrane ultrafitration, obtains concentrated solution;
Step (7) precipitates: adds the hydrochloric acid of the 1M of account for concentrated solution cumulative volume 1% in concentrated solution, adds 95% (V/V) isopyknic with concentrated solution Ethanol, at room temperature after precipitation 4h, is collected by filtration precipitation;
Step (8) is washed: adding 80% (V/V) washing with alcohol 2 times of two volumes in gained precipitates, through screw press after washing, it is unnecessary to remove Second alcohol and water, obtains wet product pectin;
Step (9) drying and crushing: by step (8) gained wet product pectin at 60-65 DEG C, is dried 12-15h, packs and i.e. obtain low first after pulverizing under the conditions of 0.17Mpa Epoxide pectin;
Step (10) side-product is processed.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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