CN104017099B - Microwave extraction, separation and purification method of pea polysaccharide - Google Patents
Microwave extraction, separation and purification method of pea polysaccharide Download PDFInfo
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- CN104017099B CN104017099B CN201410258054.8A CN201410258054A CN104017099B CN 104017099 B CN104017099 B CN 104017099B CN 201410258054 A CN201410258054 A CN 201410258054A CN 104017099 B CN104017099 B CN 104017099B
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- pea
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- polysaccharide
- ethanol
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 56
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 56
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 56
- 238000000874 microwave-assisted extraction Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000000746 purification Methods 0.000 title claims abstract description 20
- 238000000926 separation method Methods 0.000 title claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000006228 supernatant Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000003463 adsorbent Substances 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000010298 pulverizing process Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 230000000274 adsorptive effect Effects 0.000 claims description 2
- 235000010582 Pisum sativum Nutrition 0.000 abstract 7
- 241000219843 Pisum Species 0.000 abstract 5
- 240000004713 Pisum sativum Species 0.000 abstract 2
- 239000012141 concentrate Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 210000000582 semen Anatomy 0.000 abstract 1
- 239000000284 extract Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000002218 hypoglycaemic effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 150000002016 disaccharides Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002519 immonomodulatory effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a microwave extraction, separation and purification method of pea polysaccharide, which comprises the following steps: (1) taking fresh peas, and crushing the peas by using a crusher; (2) microwave extracting pulverized semen Pisi Sativi with 20wt% ethanol water for 3 times; (3) centrifuging the extracting solution after extraction, and collecting supernatant after centrifugation; (4) concentrating the supernatant until the weight of the concentrate is 20% of the weight of the original supernatant, and cooling the concentrated solution to room temperature after concentration; (5) passing the concentrated solution through D3520 macroporous adsorbent resin, collecting effluent liquid, and concentrating to obtain pea crude polysaccharide; (6) and purifying the pea crude polysaccharide with ethanol, purifying and drying to obtain the pea polysaccharide. The solution extraction rate of the pea polysaccharide prepared by the method is 12-16 wt%, and the yield can still reach 76-82% after separation and purification.
Description
Technical field
The present invention relates to a kind of method of extraction separation and purification of polysaccharide, particularly relate to a kind of microwave extraction separation purification method of pea polysaccharide.
Background technology
Polysaccharide is a kind of activeconstituents, and polysaccharide is obtained by condensation, dehydration by monosaccharide and disaccharide or other carbohydrates.Most of polysaccharide has good using value, as having immunomodulatory, the effect such as antibacterial, hypoglycemic.Polysaccharide is more common in plant, and average content can reach 10wt% to 30wt%.Because it has good pharmaceutical use, the polysaccharide therefore in each kind of plant is a study hotspot in corresponding field.
The current correlative study of pea polysaccharide is less, and pea polysaccharide known at present has the effects such as anti-oxidant, hypoglycemic.Extraction separation and purification method about pea polysaccharide is also less, and its average recoveries and purity are not high yet, these Problems existing, all limits the further application of pea polysaccharide.
Summary of the invention
The technical problem solved: conventional pea extraction method of polysaccharides is less, the problem that the pea purity of polysaccharide that known pea polysaccharide extract rate is lower, extraction obtains is lower.
Technical scheme: the microwave extraction separation purification method that the invention discloses a kind of pea polysaccharide, microwave extraction separation purification method comprises the following steps: (1) gets fresh pea, and pea pulverizer is carried out pulverization process; (2) the ethanol water of the pea 20wt% after pulverizing is carried out microwave extraction, solid-liquid ratio is 1:5 ~ 1:10, and microwave power is 200w, and the microwave extraction time is 3h, and extraction time is 3 times; (3) extracting solution is carried out centrifugal treating, collected after centrifugation upper strata supernatant liquor after extracting; (4) concentrated by supernatant liquor, being concentrated into enriched material weight is 20% of original supernatant weight, after concentrated, concentrated solution is cooled to room temperature; (5) concentrated solution is passed through D3520 macroporous adsorbent resin, collect effluent liquid, effluent liquid is concentrated, is concentrated into and obtains pea Crude polysaccharides; (6) again pea Crude polysaccharides ethanol is carried out purifying, ethanol and Crude polysaccharides weight ratio are 1:3 ~ 1:5, after purifying 2 times, prepare pea polysaccharide after drying.
In the microwave extraction separation purification method of described a kind of pea polysaccharide, on enriched material during D3520 macroporous adsorptive resins, loading speed is preferably 1.5 ~ 2BV/h, and elution speed is preferably 1.5BV/h ~ 2BV/h.
In the microwave extraction separation purification method of described a kind of pea polysaccharide, when pea Crude polysaccharides is carried out ethanol purification, described ethanol is preferably more than 99% purity.
In the microwave extraction separation purification method of described a kind of pea polysaccharide, described drying mode is preferably lyophilize.
In the microwave extraction separation purification method of described a kind of pea polysaccharide, described D3520 macroporous adsorbent resin is preferably past the D3520 macroporous adsorbent resin after activation.
Beneficial effect: the method that the present invention extracts by adopting second alcohol and water two kinds of compositions simultaneously, while guarantee pea polysaccharide extract rate, eliminates certain impurity, improves the purity of pea polysaccharide.The solution extraction yield of the pea polysaccharide that method of the present invention prepares is 12wt% to 16wt%, and after separation and purification, yield still can reach 76% to 82%.
Embodiment
Embodiment 1
(1) get fresh pea 500g, pea pulverizer is carried out pulverization process; (2) the ethanol water of the pea 20wt% after pulverizing is carried out microwave extraction, solid-liquid ratio is 1:5, and microwave power is 200w, and the microwave extraction time is 3h, and extraction time is 3 times; (3) after extracting, extracting solution is carried out centrifugal treating, centrifugal rotational speed is 4000rpm, and the time is 20min, collected after centrifugation upper strata supernatant liquor; (4) concentrated by supernatant liquor, being concentrated into enriched material weight is 20% of original supernatant weight, after concentrated, concentrated solution is cooled to room temperature; (5) concentrated solution is passed through D3520 macroporous adsorbent resin, loading speed is 1.5BV/h, and elution speed is preferably 2BV/h, collects effluent liquid, is concentrated by effluent liquid, be concentrated into and obtain pea Crude polysaccharides; (6) again pea Crude polysaccharides ethanol is carried out purifying, ethanol and Crude polysaccharides weight ratio are 1:3, after purifying 2 times, prepare pea polysaccharide after lyophilize.
Embodiment 2
(1) get fresh pea 300g, pea pulverizer is carried out pulverization process; (2) the ethanol water of the pea 20wt% after pulverizing is carried out microwave extraction, solid-liquid ratio is 1:7, and microwave power is 200w, and the microwave extraction time is 3h, and extraction time is 3 times; (3) after extracting, extracting solution is carried out centrifugal treating, centrifugal rotational speed is 4000rpm, and the time is 20min, collected after centrifugation upper strata supernatant liquor; (4) concentrated by supernatant liquor, being concentrated into enriched material weight is 20% of original supernatant weight, after concentrated, concentrated solution is cooled to room temperature; (5) concentrated solution is passed through D3520 macroporous adsorbent resin, loading speed is preferably 2BV/h, and elution speed is preferably 1.5BV/h, collects effluent liquid, is concentrated by effluent liquid, be concentrated into and obtain pea Crude polysaccharides; (6) again pea Crude polysaccharides ethanol is carried out purifying, ethanol and Crude polysaccharides weight ratio are 1:5, after purifying 2 times, prepare pea polysaccharide after lyophilize.
Embodiment 3
(1) get fresh pea 400g, pea pulverizer is carried out pulverization process; (2) the ethanol water of the pea 20wt% after pulverizing is carried out microwave extraction, solid-liquid ratio is 1:10, and microwave power is 200w, and the microwave extraction time is 3h, and extraction time is 3 times; (3) after extracting, extracting solution is carried out centrifugal treating, centrifugal rotational speed is 4000rpm, and the time is 20min, collected after centrifugation upper strata supernatant liquor; (4) concentrated by supernatant liquor, being concentrated into enriched material weight is 20% of original supernatant weight, after concentrated, concentrated solution is cooled to room temperature; (5) concentrated solution is passed through D3520 macroporous adsorbent resin, loading speed is preferably 2BV/h, and elution speed is preferably 2BV/h, collects effluent liquid, is concentrated by effluent liquid, be concentrated into and obtain pea Crude polysaccharides; (6) again pea Crude polysaccharides ethanol is carried out purifying, ethanol and Crude polysaccharides weight ratio are 1:4, after purifying 2 times, prepare pea polysaccharide after lyophilize.
The microwave extraction extraction yield of pea polysaccharide of the present invention, the numerical value of purification yield are as follows.
The mixed solvent of second alcohol and water is adopted to extract, in addition microwave-assisted again, while raising pea purity of polysaccharide, effectively raises the extraction yield of pea polysaccharide, the solution extraction yield of the pea polysaccharide prepared is 12wt% to 16wt%, and after separation and purification, yield still can reach 76% to 82%.
Claims (1)
1. a microwave extraction separation purification method for pea polysaccharide, is characterized in that microwave extraction separation purification method comprises the following steps: (1) gets fresh pea, pea pulverizer is carried out pulverization process; (2) the ethanol water of the pea 20wt% after pulverizing is carried out microwave extraction, solid-liquid ratio is 1:5 ~ 1:10, and microwave power is 200w, and the microwave extraction time is 3h, and extraction time is 3 times; (3) extracting solution is carried out centrifugal treating, collected after centrifugation upper strata supernatant liquor after extracting; (4) concentrated by supernatant liquor, being concentrated into enriched material weight is 20% of original supernatant weight, after concentrated, concentrated solution is cooled to room temperature; (5) concentrated solution is passed through D3520 macroporous adsorbent resin, collect effluent liquid, effluent liquid is concentrated, is concentrated into and obtains pea Crude polysaccharides; (6) again pea Crude polysaccharides ethanol is carried out purifying, ethanol and Crude polysaccharides weight ratio are 1:3 ~ 1:5, after purifying 2 times, prepare pea polysaccharide after drying;
Wherein, on enriched material during D3520 macroporous adsorptive resins, loading speed is 1.5 ~ 2BV/h, and elution speed is 1.5BV/h ~ 2BV/h;
When pea Crude polysaccharides is carried out ethanol purification, described ethanol is more than 99% purity;
Described drying mode is lyophilize;
Described D3520 macroporous adsorbent resin is the D3520 macroporous adsorbent resin after overactivation.
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| CN201410258054.8A CN104017099B (en) | 2014-06-12 | 2014-06-12 | Microwave extraction, separation and purification method of pea polysaccharide |
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| CN201410258054.8A CN104017099B (en) | 2014-06-12 | 2014-06-12 | Microwave extraction, separation and purification method of pea polysaccharide |
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| CN104017099B true CN104017099B (en) | 2016-04-06 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104844721B (en) * | 2015-04-20 | 2017-01-25 | 苏州经贸职业技术学院 | Extraction and separation method of Agrocybe aegirit polysaccharides |
| CN105542028A (en) * | 2016-02-23 | 2016-05-04 | 华南理工大学 | Water-soluble pea polysaccharide and preparation method thereof |
| CN111903916A (en) * | 2020-08-20 | 2020-11-10 | 福建顶旺食品有限公司 | Preparation method of pea powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1739094A1 (en) * | 2005-06-30 | 2007-01-03 | Faculté Universitaire des Sciences Agronomiques de Gembloux | Method for the purification of electrically charged polysaccharides |
| CN1970578A (en) * | 2006-11-30 | 2007-05-30 | 华南理工大学 | Microwave method for extracting water-soluble soybean polysaccharide from bean dregs |
| CN101177460A (en) * | 2007-12-05 | 2008-05-14 | 浙江工商大学 | Method for extracting water-soluble soybean polysaccharide from soya bean waste and soybean dregs |
| CN101575383A (en) * | 2009-04-29 | 2009-11-11 | 河南中医学院 | Preparation method for separating polyose from White Hyacinth Bean |
| CN102558378A (en) * | 2012-01-11 | 2012-07-11 | 上海理工大学 | Preparation method of water-soluble soybean polysaccharide |
-
2014
- 2014-06-12 CN CN201410258054.8A patent/CN104017099B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1739094A1 (en) * | 2005-06-30 | 2007-01-03 | Faculté Universitaire des Sciences Agronomiques de Gembloux | Method for the purification of electrically charged polysaccharides |
| CN1970578A (en) * | 2006-11-30 | 2007-05-30 | 华南理工大学 | Microwave method for extracting water-soluble soybean polysaccharide from bean dregs |
| CN101177460A (en) * | 2007-12-05 | 2008-05-14 | 浙江工商大学 | Method for extracting water-soluble soybean polysaccharide from soya bean waste and soybean dregs |
| CN101575383A (en) * | 2009-04-29 | 2009-11-11 | 河南中医学院 | Preparation method for separating polyose from White Hyacinth Bean |
| CN102558378A (en) * | 2012-01-11 | 2012-07-11 | 上海理工大学 | Preparation method of water-soluble soybean polysaccharide |
Non-Patent Citations (2)
| Title |
|---|
| "豌豆多糖的抗氧化与抑菌活性研究";王发春等;《安徽农业科学》;20110910;第39卷(第26期);第16431-16432页和第16440页 * |
| "青海豌豆多糖提取工艺的研究";王发春;《青海师范大学学报（自然科学版）》;20110315(第1期);第67-70页 * |
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Address after: 024000 Aohan banner Industrial Park, Chifeng City, Inner Mongolia Autonomous Region Patentee after: Aohan North Granary Agricultural Products Wholesale Market Co.,Ltd. Address before: 024000 Aohan banner Industrial Park, Chifeng City, Inner Mongolia Autonomous Region Patentee before: Inner Mongolia yuyantang Biotechnology Co.,Ltd. |