CN102335201B - Extract method of asteroid saponins - Google Patents
Extract method of asteroid saponins Download PDFInfo
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- CN102335201B CN102335201B CN2011102955244A CN201110295524A CN102335201B CN 102335201 B CN102335201 B CN 102335201B CN 2011102955244 A CN2011102955244 A CN 2011102955244A CN 201110295524 A CN201110295524 A CN 201110295524A CN 102335201 B CN102335201 B CN 102335201B
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- starfish
- saponin
- alkali
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- 229930182490 saponin Natural products 0.000 title claims abstract description 23
- 150000007949 saponins Chemical class 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- 235000017709 saponins Nutrition 0.000 title abstract description 18
- 239000000284 extract Substances 0.000 title abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 10
- 239000011347 resin Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 7
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 6
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000003480 eluent Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 230000006920 protein precipitation Effects 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract 3
- 241000258957 Asteroidea Species 0.000 claims description 25
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 19
- 239000003513 alkali Substances 0.000 claims description 11
- 238000010828 elution Methods 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- 239000004925 Acrylic resin Substances 0.000 claims 2
- 229920000178 Acrylic resin Polymers 0.000 claims 2
- 239000004367 Lipase Substances 0.000 claims 2
- 102000004882 Lipase Human genes 0.000 claims 2
- 108090001060 Lipase Proteins 0.000 claims 2
- 108091005804 Peptidases Proteins 0.000 claims 2
- 239000004365 Protease Substances 0.000 claims 2
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims 2
- 235000019421 lipase Nutrition 0.000 claims 2
- 229920005990 polystyrene resin Polymers 0.000 claims 2
- 239000002994 raw material Substances 0.000 abstract description 8
- 102000004190 Enzymes Human genes 0.000 abstract description 5
- 108090000790 Enzymes Proteins 0.000 abstract description 5
- 239000004480 active ingredient Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000012141 concentrate Substances 0.000 abstract 1
- 239000012634 fragment Substances 0.000 abstract 1
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 241000257468 Asterias amurensis Species 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- 241000699666 Mus <mouse, genus> Species 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- SMRPGWBDLOQHOS-UHFFFAOYSA-N 5-[4,5-dihydroxy-6-(hydroxymethyl)-3-(3,4,5-trihydroxy-6-methyloxan-2-yl)oxyoxan-2-yl]oxy-3,4-dihydroxy-6-[[9-hydroxy-4-(hydroxymethyl)-4,6a,6b,8a,11,11,14b-heptamethyl-14-oxo-2,3,4a,5,6,7,8,9,10,12,12a,14a-dodecahydro-1H-picen-3-yl]oxy]oxane-2-carboxylic acid Chemical compound OC1C(O)C(O)C(C)OC1OC1C(OC2C(OC(C(O)C2O)C(O)=O)OC2C(C3C(C4C(C5(CCC6(C)C(O)CC(C)(C)CC6C5=CC4=O)C)(C)CC3)(C)CC2)(C)CO)OC(CO)C(O)C1O SMRPGWBDLOQHOS-UHFFFAOYSA-N 0.000 description 1
- SHZGCJCMOBCMKK-UHFFFAOYSA-N D-mannomethylose Natural products CC1OC(O)C(O)C(O)C1O SHZGCJCMOBCMKK-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- SHZGCJCMOBCMKK-JFNONXLTSA-N L-rhamnopyranose Chemical compound C[C@@H]1OC(O)[C@H](O)[C@H](O)[C@H]1O SHZGCJCMOBCMKK-JFNONXLTSA-N 0.000 description 1
- PNNNRSAQSRJVSB-UHFFFAOYSA-N L-rhamnose Natural products CC(O)C(O)C(O)C(O)C=O PNNNRSAQSRJVSB-UHFFFAOYSA-N 0.000 description 1
- 241000699670 Mus sp. Species 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- BMWPBKOFJSHJAW-UHFFFAOYSA-N Saponin B Natural products CC1(C)CCC2(CCC3(C)C(=CCC4C5(C)CCC(OC6OC(CO)C(O)C(OC7OC(CO)C(O)C(O)C7O)C6=O)C(C)(C)C5CCC34C)C2C1)C(=O)O BMWPBKOFJSHJAW-UHFFFAOYSA-N 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000007954 hypoxia Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- PPRSVUXPYPBULA-UHFFFAOYSA-N saponin A Natural products CC1(C)CCC2(CCC3(C)C(=CCC4C5(C)CCC(OC6OC(CO)C(O)C(O)C6=O)C(C)(C)C5CCC34C)C2C1)C(=O)O PPRSVUXPYPBULA-UHFFFAOYSA-N 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Landscapes
- Saccharide Compounds (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses an extract method of asteroid saponins. The method comprises the main steps of: cleaning asteroids as a raw material; drying the raw material until the water content is less than 50%; crushing the dried raw material into fragments with grain size of 1 to 5 millimeters by using a crusher; adding 3-4 times of volume of deionized water; uniformly mixing; adding alkaline until the concentration is 4-5%; agitating the mixture for 36-48 hours at 0-4 DEG C; adding acetic acid to neutralize the alkaline until the pH is 6-8; adding 1.6-2.2% of complex biologic enzyme; hydrolyzing for 8 to 12 hours at 60 to 70 DEG C; adding ammonium sulfate until the final concentration is of 30-40%; then centrifuging at room temperature to remove protein precipitation; adsorbing supernate by macroporous adsorption resin; eluting with 40-60% ethanol the volume of which is 0.5-2 times of that of the resin; concentrating the eluent in vacuum; and drying the concentrate to obtain the asteroid saponins. The extract method has the advantages that: the whole process is implemented without high temperature, and therefore the active ingredients in the raw material can be retained.
Description
Technical field
The invention belongs to a kind of extracting method of saponin, specifically a kind of extracting method of starfish saponin.
Technical background
It is multiple that starfish contains saponin, and a class soap class is poisonous, therefrom isolates two kinds of materials of saponin A and B.Another kind of saponin hydrolyzable goes out glucose, xylose, rhamnose etc.Its saponins antitumaous effect is the effect of cell sample.The Asterias amurensis Lutken extracting solution can resist and sprinkle the mouse spleen that the mud pine causes and alleviate and suppress mouse liver oxidation fat and react.Asterias amurensis Lutken can also extend the survival rate under mice normobaric hypoxia state.。
In recent years, the medical value of Asterias amurensis Lutken progressively is taken seriously, and many marine drugs or food enterprise have been developed the products such as Asterias amurensis Lutken nutrient capsules, but for the extraction of saponin contained in starfish and utilize shorter mention, and the more chemicals of extracting method use used, seriously polluted.
Summary of the invention
The present invention adopts the compound biological enzyme extracting method, extracts starfish saponin material under temperate condition, and after by the vacuum evaporation technology, saponin degree of depth purification being concentrated, lyophilization obtains high purity medical level saponin product.
The method step is as follows: 1. the raw material starfish is cleaned, oven dry is to being about 1/3rd of original weight, and water content lower than 50%, is generally 40～45% at this moment, is ground into the chip of 1～5 millimeter of particle diameter with pulverizer; 2. the starfish after pulverizing adds the deionized water of 3～4 times of volumes, and mixing adds the concentration of alkali to 4～5%, stirs 36～48 hours under 0～4 ℃; 3. with acetic acid with alkali pH6～8 that neutralize, add 1.6～2.2% compound biological enzyme, 60～70 ℃ of hydrolysis 8～12 hours; 4. adding ammonium sulfate is 30～40% to final concentration, and under room temperature, 5000g is centrifugal 15 minutes, removes protein precipitation; 5. supernatant is with acrylic compounds or polystyrene type absorption with macroporous adsorbent resin, and with 40～60% ethanol elutions of 0.5～2 times of resin volume, eluent vacuum concentration drying obtains starfish saponin.Reclaim after the ethanol condensation of evaporation.
Compared with prior art, the invention has the advantages that and not use high temperature in whole process, the active component in raw material is kept.
Specific embodiments
Example 1: a kind of extracting method of starfish saponin, the method comprises the following steps: 1. the raw material starfish is cleaned, oven dry is 45% to water content, is ground into the chip of 1 millimeter of particle diameter with pulverizer; 2. the starfish after pulverizing adds the deionized water of 4 times of volumes, and mixing adds the concentration of alkali to 4%, stirs 36 hours under 4 ℃; 3. with acetic acid with the alkali pH6 that neutralizes, add 2.2% compound biological enzyme, 60 ℃ of hydrolysis 8 hours; 4. adding ammonium sulfate is 30% to final concentration, and under room temperature, 5000g is centrifugal 15 minutes, removes protein precipitation; 5. supernatant acrylic compounds absorption with macroporous adsorbent resin, with 60% ethanol elution of 0.5 times of resin volume, eluent vacuum concentration drying obtains the starfish saponin.
Example 2: a kind of extracting method of starfish saponin, the method comprises the following steps: 1. the raw material starfish is cleaned, oven dry is 40% to water content, is ground into the chip of 5 millimeters of particle diameters with pulverizer; 2. the starfish after pulverizing adds the deionized water of 3 times of volumes, and mixing adds the concentration of alkali to 5%, stirs 48 hours under 1 ℃; 3. with acetic acid with the alkali pH8 that neutralizes, add 1.6% compound biological enzyme, 70 ℃ of hydrolysis 12 hours; 4. adding ammonium sulfate is 40% to final concentration, and under room temperature, 5000g is centrifugal 15 minutes, removes protein precipitation; 5. supernatant polystyrene type absorption with macroporous adsorbent resin, with 40% ethanol elution of 2 times of resin volumes, eluent vacuum concentration drying obtains the starfish saponin.
Claims (3)
1. the extracting method of a starfish saponin, is characterized in that the method includes the steps of: the starfish water is cleaned, then dry water content lower than 50%, be ground into the chip of 1 ~ 5 millimeter of particle diameter with pulverizer; The deionized water that starfish after pulverizing is added 3 ~ 4 times of volumes, mixing adds the concentration of alkali to 4 ~ 5%, stirs 36 ~ 48 hours under 0 ~ 4 ℃; With alkali pH6 ~ 8 that neutralize, add 1.6 ~ 2.2% lipase, the mixture of protease with acetic acid, 60 ~ 70 ℃ of hydrolysis 8 ~ 12 hours; Adding ammonium sulfate is 30 ~ 40% to final concentration, and under room temperature, 5000g is centrifugal 15 minutes, removes protein precipitation; Supernatant adsorbs with acrylic resin or polystyrene resin, and with 40 ~ 60% ethanol elutions of 0.5～2 times of resin volume, eluent vacuum concentration drying obtains the starfish saponin.
2. a kind of extracting method of starfish saponin as claimed in claim 1 is characterized in that the method includes the steps of: the starfish water is cleaned, then oven dry is 40 ~ 45% to water content, is ground into the chip of 2 ~ 4 millimeters of particle diameters with pulverizer; The deionized water that starfish after pulverizing is added 3 ~ 4 times of volumes, mixing adds the concentration of alkali to 4.2 ~ 4.7%, stirs 40 ~ 45 hours under 1 ~ 3 ℃; With alkali pH6 ~ 8 that neutralize, add 1.8 ~ 2.0% lipase, the mixture of protease with acetic acid, 62 ~ 65 ℃ of hydrolysis 8 ~ 12 hours; Adding ammonium sulfate is 33% to final concentration, and under room temperature, 5000g is centrifugal 15 minutes, removes protein precipitation; Supernatant adsorbs with acrylic resin or polystyrene resin, and with 50 ~ 55% ethanol elutions of 0.8～1.2 times of resin volume, eluent vacuum concentration drying obtains the starfish saponin.
3. a kind of extracting method of starfish saponin as claimed in claim 1, is characterized in that described alkali is sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102955244A CN102335201B (en) | 2011-09-30 | 2011-09-30 | Extract method of asteroid saponins |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102955244A CN102335201B (en) | 2011-09-30 | 2011-09-30 | Extract method of asteroid saponins |
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| Publication Number | Publication Date |
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| CN102335201A CN102335201A (en) | 2012-02-01 |
| CN102335201B true CN102335201B (en) | 2013-06-12 |
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| CN2011102955244A Active CN102335201B (en) | 2011-09-30 | 2011-09-30 | Extract method of asteroid saponins |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106070336A (en) * | 2016-06-19 | 2016-11-09 | 青岛科光生物技术有限公司 | The manufacture method of Asterias amurensis Lutken extracting solution |
| CN106173056A (en) * | 2016-07-08 | 2016-12-07 | 肇庆医学高等专科学校 | Health-care herbal tea capable of enhancing immunity and preparation method thereof |
| CN106577774A (en) * | 2016-12-09 | 2017-04-26 | 熊廷珍 | Production method of marine animal pesticide |
| CN113940427A (en) * | 2021-11-01 | 2022-01-18 | 大连海洋大学 | Preparation process of asterias amurensis Lutken saponin with antioxidant activity |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840539A (en) * | 2005-03-29 | 2006-10-04 | 郭承华 | Salangane saponin and preparation method and use thereof |
| CN101760490A (en) * | 2008-11-07 | 2010-06-30 | 南通芯迎设计服务有限公司 | Extraction and separation method for sand starfish mucopolysaccharide |
| CN102002110A (en) * | 2010-11-24 | 2011-04-06 | 刘全胜 | Preparation method of polysaccharides from sea cucumber |
| CN102138939A (en) * | 2011-03-28 | 2011-08-03 | 山东大学威海分校 | Preparation method of asterias amurensis polysaccharide extractive and medical applications thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5199919B2 (en) * | 2008-03-04 | 2013-05-15 | 地方独立行政法人北海道立総合研究機構 | Glucose level rise inhibitor comprising star decollagen peptide as active ingredient and method for producing dedecollagen peptide |
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2011
- 2011-09-30 CN CN2011102955244A patent/CN102335201B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840539A (en) * | 2005-03-29 | 2006-10-04 | 郭承华 | Salangane saponin and preparation method and use thereof |
| CN101760490A (en) * | 2008-11-07 | 2010-06-30 | 南通芯迎设计服务有限公司 | Extraction and separation method for sand starfish mucopolysaccharide |
| CN102002110A (en) * | 2010-11-24 | 2011-04-06 | 刘全胜 | Preparation method of polysaccharides from sea cucumber |
| CN102138939A (en) * | 2011-03-28 | 2011-08-03 | 山东大学威海分校 | Preparation method of asterias amurensis polysaccharide extractive and medical applications thereof |
Non-Patent Citations (1)
| Title |
|---|
| 樊廷俊等.水溶性海星皂苷的分离纯化及其抗真菌活性研究.《山东大学学报（理学版）》.2008,第43卷(第9期),第1-5页. * |
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| CN102335201A (en) | 2012-02-01 |
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