CN102228488A - Preparation of Lysimachia capillipes Hemsl total saponin - Google Patents
Preparation of Lysimachia capillipes Hemsl total saponin Download PDFInfo
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- CN102228488A CN102228488A CN2011101514901A CN201110151490A CN102228488A CN 102228488 A CN102228488 A CN 102228488A CN 2011101514901 A CN2011101514901 A CN 2011101514901A CN 201110151490 A CN201110151490 A CN 201110151490A CN 102228488 A CN102228488 A CN 102228488A
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- China
- Prior art keywords
- preparation
- herba lysimachiae
- lysimachiae capillipedis
- total saponins
- total saponin
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- 229930182490 saponin Natural products 0.000 title claims abstract description 22
- 150000007949 saponins Chemical class 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000001397 quillaja saponaria molina bark Substances 0.000 title abstract description 7
- 241000941637 Lysimachia capillipes Species 0.000 title abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000284 extract Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 239000012528 membrane Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000012466 permeate Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 3
- 235000017709 saponins Nutrition 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229950000845 politef Drugs 0.000 claims description 3
- 229920006393 polyether sulfone Polymers 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 2
- 239000012510 hollow fiber Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- 238000001914 filtration Methods 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 235000013305 food Nutrition 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- 238000004042 decolorization Methods 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 239000012074 organic phase Substances 0.000 abstract 1
- 238000010791 quenching Methods 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 230000001476 alcoholic effect Effects 0.000 description 6
- 230000006837 decompression Effects 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 238000000502 dialysis Methods 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 206010011224 Cough Diseases 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 206010009944 Colon cancer Diseases 0.000 description 1
- 206010011469 Crying Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000019255 Menstrual disease Diseases 0.000 description 1
- 208000007443 Neurasthenia Diseases 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 241000208476 Primulaceae 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
- 206010044302 Tracheitis Diseases 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000000680 avirulence Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 208000029742 colonic neoplasm Diseases 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000005906 menstruation Effects 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000002611 ovarian Effects 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- LVTJOONKWUXEFR-UEZXSUPNSA-N protodioscin Chemical compound O([C@@H]1[C@@H](CO)O[C@H]([C@@H]([C@H]1O)O[C@H]1[C@@H]([C@H](O)[C@@H](O)[C@H](C)O1)O)O[C@@H]1CC2=CC[C@H]3[C@@H]4C[C@@H]5O[C@]([C@H]([C@@H]5[C@@]4(C)CC[C@@H]3[C@@]2(C)CC1)C)(O)CC[C@@H](C)CO[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@@H](C)[C@H](O)[C@@H](O)[C@H]1O LVTJOONKWUXEFR-UEZXSUPNSA-N 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- QDQWGYLCDZBAMD-UHFFFAOYSA-N saponin C Natural products CC1C2C3CCC4C5(C)CCC(O)C(C)(COC6OC(CO)C(O)C(O)C6O)C5CCC4(C)C3(C)CCC27C8OC8C1(C)OC7=O QDQWGYLCDZBAMD-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Cosmetics (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a preparation method of a Lysimachia capillipes Hemsl total saponin. The preparation method comprises the following steps of crushing a Lysimachia capillipes Hemsl medicinal material, adding 50 to 70% of ethanol into the crushed medicinal material, quenching, extracting, adding the extract into an ultrafiltration membrane system to carry out a filtering process, recovering ethanol from permeate, extracting concentrated liquid by water-saturated n-butyl alcohol, adding active carbon into an organic phase to carry out a decolorization process, carrying out a concentration process under reduced pressure, and drying to obtain a Lysimachia capillipes Hemsl total saponin. The preparation method of a Lysimachia capillipes Hemsl total saponin adopts an ultra-filtration technology and has the advantages of simple processes, low energy consumption, and good product characteristics of no solvent residue and direct applicability to foods and drugs.
Description
Technical field:
The present invention relates to a kind of preparation method of Herba lysimachiae capillipedis total saponins, particularly relate to a kind of hyperfiltration technique that utilizes and prepare the Herba lysimachiae capillipedis total saponins.
Background technology:
Herba lysimachiae capillipedis again the row's of crying perfume, Lysimachia capillipes Hemsl, Rhizoma et radix valerianae, Herba lysimachiae capillipedis, hair handle Herba Lysimachiae Clethroids (Radix Seu Herba Lysimachiae Clethroidis), close blood grass, MANSHANXIANG, be the herb of Primulaceae plant Herba lysimachiae capillipedis.Have and dispel the wind, cough-relieving, the effect of regulating menstruation is used for the treatment of cold cough, tracheitis, asthma, menoxenia, neurasthenia etc.Modern medicine study is found, there are a large amount of saponin to have antitumor action in the Herba lysimachiae capillipedis, China Medical Sciences Academy Medical Plants Institute is partly studied the polarity of Herba lysimachiae capillipedis (Herba lysimachiae capillipedis) herb, therefrom separates to obtain 25 chemical compounds and identify the wherein structure of 16 chemical compounds.Wherein Herba lysimachiae capillipedis saponin B (LC-2) and Herba lysimachiae capillipedis saponin C (LC-3) have obvious inhibitory action to Proliferation of Human Ovarian Cell, and LC-2, LC-3 also have the inhibition effect to human oral cavity epithelial cancerous cell, human colon cancer cell.
The existing Herba lysimachiae capillipedis total saponins that extracts has extraction and column chromatography." utilize macroporous resin to prepare the method and the purposes of Herba lysimachiae capillipedis total saponin extracts " as patent (application number 200910096786), the method of this Patent publish is with the Herba lysimachiae capillipedis pulverizing medicinal materials or directly uses the Herba lysimachiae capillipedis decoction pieces, add water or ethanol, heating and refluxing extraction, filter, merge extractive liquid, concentrates; Filtration or centrifugal back wash resin earlier with water by being filled with the chromatographic column of macroporous resin, and water elution liquid discards; Reuse aquiferous ethanol eluting is collected ethanol elution; The ethanol elution concentrating under reduced pressure, decompression or spray drying get the Herba lysimachiae capillipedis total saponins.As mentioned above, existing preparation west stalk Herba Pelargonii Graveolentis total saponins method, energy consumption is bigger, and it is more especially to produce waste liquid in the macroporous resin separation process, is unfavorable for environmental protection.
Summary of the invention
The objective of the invention is provides a kind of preparation method of Herba lysimachiae capillipedis total saponins in order to overcome the deficiencies in the prior art, adopts hyperfiltration technique, simple to operate, the industrialization degree height.
The technology of the present invention solution is as follows:
A kind of extracting method of Herba lysimachiae capillipedis saponin, it is characterized in that getting the Herba lysimachiae capillipedis pulverizing medicinal materials, adding 50-70% ethanol merceration extracts, filter, add ultrafiltration membrance filter, permeate reclaims ethanol, concentrated solution water saturation n-butanol extraction, organic addition activated carbon decolorizing, concentrating under reduced pressure is drying to obtain total saponins.
Described ultrafilter membrane is the hollow fiber ultrafiltration film of molecular cut off 3000-10000, a kind of in the optional Fypro of material, polyether sulfone, the politef.
Described active carbon is medicinal class active carbon, and consumption is the 1-3% of liquid.
Advantage of the present invention is:
1. method adopts the ultrafilter membrane ultrafiltration, removes macromolecular substances, belongs to physical method, and energy consumption is low, does not use reagent, and cost is low, and is pollution-free.
2. avirulence reagent uses in whole technical process, and the product nonhazardous is residual, meets the requirement of food and medicine.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1
The Herba lysimachiae capillipedis pulverizing medicinal materials, get 5kg, add 30kg50% alcoholic solution merceration 12 hours, extract 3 times, extracting solution filters and adds the filtration of molecular cut off 3000 hollow nylon ultrafiltration membrane system, add an amount of 50% alcoholic solution dialysis, the permeate decompression recycling ethanol, concentrated solution adds isopyknic water-saturated n-butanol extraction 3 times, extract adds 80 ℃ of decolourings of 1% medicinal class active carbon 2 hours, reclaim under reduced pressure n-butyl alcohol, vacuum drying, obtain off-white color and divide powder Herba lysimachiae capillipedis total saponins 102g, content 85%.
Embodiment 2
The Herba lysimachiae capillipedis pulverizing medicinal materials, get 5kg, add 50kg70% alcoholic solution merceration 12 hours, extract 2 times, extracting solution filters and adds molecular cut off 10000 hollow poly (ether-sulfone) ultrafiltration membrane system filtrations, add an amount of 70% alcoholic solution dialysis, the permeate decompression recycling ethanol, the water-saturated n-butanol that concentrated solution adds the 2BV volume extracts 2 times, extract adds 70 ℃ of decolourings of 3% medicinal class active carbon 2 hours, reclaim under reduced pressure n-butyl alcohol, vacuum drying, obtain off-white color and divide powder Herba lysimachiae capillipedis total saponins 101g, content 87%.
Embodiment 3:
The Herba lysimachiae capillipedis pulverizing medicinal materials, get 5kg, add 30kg60% alcoholic solution merceration 12 hours, extract 3 times, extracting solution filters and adds the filtration of molecular cut off 3000 hollow politef ultrafiltration membrane system, add an amount of 60% alcoholic solution dialysis, the permeate decompression recycling ethanol, concentrated solution adds isopyknic water-saturated n-butanol extraction 4 times, extract adds 75 ℃ of decolourings of 2% medicinal class active carbon 2 hours, reclaim under reduced pressure n-butyl alcohol, vacuum drying, obtain off-white color and divide powder Herba lysimachiae capillipedis total saponins 114g, content 86%.
Claims (3)
1. the preparation method of a Herba lysimachiae capillipedis total saponins, it is characterized in that: get the Herba lysimachiae capillipedis pulverizing medicinal materials, adding 50-70% ethanol merceration extracts, filter, add ultrafiltration membrance filter, permeate reclaims ethanol, concentrated solution water saturation n-butanol extraction, organic addition activated carbon decolorizing, concentrating under reduced pressure is drying to obtain total saponins.
2. according to the preparation method of the described Herba lysimachiae capillipedis total saponins of claim 1, it is characterized in that described ultrafilter membrane is the hollow fiber ultrafiltration film of molecular cut off 3000-10000, a kind of in the optional Fypro of material, polyether sulfone, the politef.
3. according to the preparation method of the described Herba lysimachiae capillipedis total saponins of claim 1, it is characterized in that described active carbon is medicinal class active carbon, consumption is the 1-3% of liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101514901A CN102228488A (en) | 2011-06-07 | 2011-06-07 | Preparation of Lysimachia capillipes Hemsl total saponin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101514901A CN102228488A (en) | 2011-06-07 | 2011-06-07 | Preparation of Lysimachia capillipes Hemsl total saponin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102228488A true CN102228488A (en) | 2011-11-02 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101514901A Pending CN102228488A (en) | 2011-06-07 | 2011-06-07 | Preparation of Lysimachia capillipes Hemsl total saponin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102228488A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037483A (en) * | 2015-08-18 | 2015-11-11 | 苏州求是本草健康科技有限公司 | Preparation method and application of lysimachia capillipes saponin A |
| CN105695096A (en) * | 2016-02-21 | 2016-06-22 | 湖南城市学院 | Lysimachia capillipes extract and preparation method thereof |
| CN106177609A (en) * | 2016-09-30 | 2016-12-07 | 云南乐知竹生物技术有限公司 | The method obtaining fresh culm leaf active component |
| CN110772548A (en) * | 2019-11-13 | 2020-02-11 | 常熟求是科技有限公司 | Lysimachia capillipes extract and preparation method and application thereof |
| CN114264763A (en) * | 2021-12-22 | 2022-04-01 | 金绿源(中国)生物科技有限公司 | A kind of sampling method of fine stem herb |
-
2011
- 2011-06-07 CN CN2011101514901A patent/CN102228488A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037483A (en) * | 2015-08-18 | 2015-11-11 | 苏州求是本草健康科技有限公司 | Preparation method and application of lysimachia capillipes saponin A |
| CN105695096A (en) * | 2016-02-21 | 2016-06-22 | 湖南城市学院 | Lysimachia capillipes extract and preparation method thereof |
| CN106177609A (en) * | 2016-09-30 | 2016-12-07 | 云南乐知竹生物技术有限公司 | The method obtaining fresh culm leaf active component |
| CN110772548A (en) * | 2019-11-13 | 2020-02-11 | 常熟求是科技有限公司 | Lysimachia capillipes extract and preparation method and application thereof |
| CN114264763A (en) * | 2021-12-22 | 2022-04-01 | 金绿源(中国)生物科技有限公司 | A kind of sampling method of fine stem herb |
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Legal Events
| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111102 |