CN100590109C - Extraction Technology of Active Components of Herb Cistanche - Google Patents
Extraction Technology of Active Components of Herb Cistanche Download PDFInfo
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- CN100590109C CN100590109C CN200810025392A CN200810025392A CN100590109C CN 100590109 C CN100590109 C CN 100590109C CN 200810025392 A CN200810025392 A CN 200810025392A CN 200810025392 A CN200810025392 A CN 200810025392A CN 100590109 C CN100590109 C CN 100590109C
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- cistanche
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- 238000000605 extraction Methods 0.000 title claims abstract description 54
- 241000005787 Cistanche Species 0.000 title claims abstract description 51
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000284 extract Substances 0.000 claims abstract description 26
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 18
- 229930182470 glycoside Natural products 0.000 claims abstract description 16
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-Phenylethanol Natural products OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 150000004676 glycans Chemical class 0.000 claims abstract description 15
- 235000010355 mannitol Nutrition 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- -1 phenylethanol glycosides Chemical class 0.000 claims abstract description 15
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 15
- 239000005017 polysaccharide Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011347 resin Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 241000336291 Cistanche deserticola Species 0.000 claims abstract 7
- 239000000843 powder Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 5
- 241000336315 Cistanche salsa Species 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000004480 active ingredient Substances 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000004108 freeze drying Methods 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 238000001694 spray drying Methods 0.000 claims 1
- 229930195725 Mannitol Natural products 0.000 abstract description 8
- 239000000594 mannitol Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000006837 decompression Effects 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 229940067107 phenylethyl alcohol Drugs 0.000 description 11
- 230000004071 biological effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000004062 sedimentation Methods 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 239000002178 crystalline material Substances 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 235000013372 meat Nutrition 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 206010027514 Metrorrhagia Diseases 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
本发明涉及一种肉苁蓉药材有效成份的提取工艺，属于中药成份提取技术领域。包括：将肉苁蓉烘干、粉碎，采用90-95%乙醇提取，提取液经浓缩、结晶、干燥得肉苁蓉D-甘露醇；提取残渣用浓度为60-80%的乙醇溶液提取，提取液通过大孔树脂，洗脱液经浓缩、干燥得肉苁蓉苯乙醇苷类；所得提取残渣继续加入蒸馏水加热提取，上清液经减压浓缩后加入3倍体积的95%乙醇沉淀，沉淀干燥即可获得肉苁蓉多糖。与传统方法相比，本发明同时获得肉苁蓉甘露醇、肉苁蓉苯乙醇苷类、肉苁蓉多糖三种肉苁蓉生物功效成分，弥补了传统提取方法中过分注重单一成分的缺点。使用的乙醇可在减压浓缩过程中进行回收，达到循环利用的效果，从而有效的降低了生产成本。
The invention relates to an extraction process of effective components of Cistanche medicinal materials, and belongs to the technical field of extraction of traditional Chinese medicine components. Including: drying and pulverizing Cistanche, extracting with 90-95% ethanol, concentrating, crystallizing and drying the extract to obtain Cistanche D-mannitol; extracting the residue with 60-80% ethanol solution, and passing the extract through large Pore resin, the eluate is concentrated and dried to obtain phenylethanol glycosides of Cistanche deserticola; the obtained extraction residue is further added to distilled water for heating and extraction, and the supernatant is concentrated under reduced pressure and then added with 3 times the volume of 95% ethanol for precipitation, and the precipitation is dried to obtain Cistanche deserticola. polysaccharides. Compared with the traditional method, the present invention simultaneously obtains three biofunctional components of Cistanche deserticola, mannitol, phenylethanol glycosides and polysaccharides of Cistanche deserticola, which makes up for the shortcoming of over-emphasizing a single component in the traditional extraction method. The used ethanol can be recovered during the decompression concentration process to achieve the effect of recycling, thereby effectively reducing the production cost.
Description
One, technical field
The present invention relates to the method for extraction, separating effective ingredient from Chinese medicinal materials, particularly the method for high efficiency extraction D-N.F,USP MANNITOL, phenylethyl alcohol glycoside, polysaccharide from the Herba Cistanches medicinal material belongs to Chinese medicinal ingredients extractive technique field.
Two, technical background
Herba Cistanches (Cistanche salsa G.Beck) has another name called that sacsaoul rues greatly, smart bamboo shoot, essence, be China's rare Chinese medicine, pharmacopeia is included, and mainly is grown in desert regions such as China's West Inner Mongolia, Gansu, Xinjiang.Herba Cistanches beginning is stated from Shennong's Herbal, classifies as top gradely, has kidney invigorating and YANG supporting, benefiting essence and marrow, enriching blood and moistening for dryness, pleases look effect such as prolong life, and cures mainly under impotence in male, infertilitas feminis, the band, cards such as metrorrhagia, waist knee crymodynia, blood depletion constipation.
Contain biological effect compositions such as phenylethyl alcohol glycoside, D-N.F,USP MANNITOL, polysaccharide, trimethyl-glycine in the Herba Cistanches medicinal material.The extracting method of Herba Cistanches biological effect composition is a lot, but most extracting method only is confined in a kind of extraction of biological effect composition, has ignored the extraction of other biological functional component, causes the significant wastage of resource.
Three, summary of the invention
Technical problem
The object of the present invention is to provide a kind of extraction process of Herba Cistanches medicinal material effective ingredient, the processing method of high efficiency extraction phenylethyl alcohol glycoside, D-N.F,USP MANNITOL, polysaccharide from the Herba Cistanches medicinal material has simultaneously remedied the undue extraction of paying attention to single component in the traditional extraction process and the shortcoming of loss Other Meat desert cistanche biological effect composition.
Technical scheme
The extraction process of Herba Cistanches medicinal material effective ingredient, its step is as follows:
(1) with the Herba Cistanches medicinal material through 60 ℃ of oven dry, be ground into 40 orders;
(2) Herba Cistanches D-N.F,USP MANNITOL extracts: get the Herba Cistanches powder, adopting volume ratio content is the ethanolic soln extraction of 90-95%, the consumption that extracts solvent is 5-10 a times of Herba Cistanches weight, extraction time is 2-3 time, extracting method is the refluxing extraction method, and extracting solution is through concentrated, crystallization, the dry Herba Cistanches D-N.F,USP MANNITOL that gets.
(3) phenylethyl alcohol glycoside extracting method: with the extraction residue that obtains in the step 2, with volume by volume concentration is that the ethanolic soln of 60-80% extracts, the consumption that extracts solvent is 8-10 a times of Herba Cistanches weight, extraction time is 2-3 time, extracting method is the microwave auxiliary reflux extracting method, extracting solution is collected elutriant by macroporous resin, through concentrated, the dry Herba Cistanches phenylethyl alcohol glycoside that gets;
(4) extracting method of Herba Cistanches polysaccharide: go into the distilled water heating in the extraction residue that will from step 3, obtain and extract, the consumption that extracts solvent is 10-15 a times of Herba Cistanches weight, extraction time is 2-3 time, extracting method decocts extracting method for heating, after extract finishing, supernatant liquor adds 95% ethanol sedimentation of 3 times of volumes behind concentrating under reduced pressure, leaves standstill 24 hours under 4 ℃, centrifugal back collecting precipitation, drying can obtain the Herba Cistanches polysaccharide;
Herba Cistanches medicinal material in the extraction process of above-mentioned Herba Cistanches medicinal material effective constituent in the step (1) is a Saline Cistanche Herb Cistanche salsa G.Beck chylocaulous.Drying means in step (2), (3), (4) is reduced vacuum drying, spraying drying or lyophilize.
Beneficial effect
Extracting method of the present invention is compared with traditional extraction process, has the following advantages:
1. the extracting method among the present invention is compared with traditional extraction process, can obtain Herba Cistanches N.F,USP MANNITOL, cistanche glycosides, three kinds of Herba Cistanches biological effects of Herba Cistanches polysaccharide composition simultaneously, utilize the Herba Cistanches raw material to greatest extent, remedied the undue extraction of paying attention to single component in the traditional extraction process and the shortcoming of loss Other Meat desert cistanche biological effect composition.
2. the ethanol that uses among the present invention can reclaim in the concentrating under reduced pressure process, continues to use in the leaching process, reaches the effect of recycle, thereby has effectively reduced production cost.
Four, description of drawings
The operational path of high efficiency extraction phenylethyl alcohol glycoside, D-N.F,USP MANNITOL, polysaccharide in Fig. 1 Herba Cistanches medicinal material
Five, embodiment:
Embodiment 1:
Herba Cistanches powder 1kg, adding 10 times of amount concentration is the ethanol of 90% (V/V), extracts 2 hours, with 8 times of amount 90% (V/V) extraction using alcohols, merges extracted twice liquid again, through concentrating under reduced pressure, crystallization, the dry crystalline material 16g that gets, the D-mannitol content is 50%.Extract residue, continuing with concentration is that 80% (V/V) ethanolic soln extracts 2 times, and extracting solution gets Herba Cistanches alcohol extract 300g through concentrating under reduced pressure, spraying drying, contains phenylethyl alcohol glycoside 5%.To extract the distilled water that continues to add 10 times of amounts in the residue, heating extracts twice, and supernatant liquor adds 95% ethanol sedimentation of 3 times of volumes behind concentrating under reduced pressure, left standstill under 4 ℃ 24 hours, centrifugal back collecting precipitation, drying can obtain Herba Cistanches polysaccharide 60g, and purity is 75%.
Embodiment 2:
Herba Cistanches powder 1kg adds 10 times of amount 95% (V/V) ethanol, extracts 2 hours, with 8 times of amount 95% (V/V) extraction using alcohols, merges extracted twice liquid again, and through concentrating under reduced pressure, crystallization, the dry crystallizing and drying thing 20g that gets, the D-mannitol content is 64%.Extract residue, continuing with 10 times of amount concentration is that 80% (V/V) ethanolic soln extracted 2 hours, is that 70% (V/V) ethanolic soln extracted extracting solution 2 hours with concentration again, get phenylethyl alcohol glycoside 350g through concentrating under reduced pressure, spraying drying, phenylethyl alcohol glycoside content is 7%.To extract the distilled water that continues to add 15 times of amounts in the residue, heating is extracted 2 times, and supernatant liquor adds 95% ethanol sedimentation of 3 times of volumes behind concentrating under reduced pressure, left standstill under 4 ℃ 24 hours, centrifugal back collecting precipitation, drying can obtain Herba Cistanches polysaccharide 60g, and purity is 60%.
Embodiment 3:
Herba Cistanches powder tkg adds 8 times of amount 90% (V/V) ethanol, extracts 2 hours, extracts twice, merges extracted twice liquid, and through concentrating under reduced pressure, crystallization, the dry crystalline material 10g that gets, the D-mannitol content is 50%.Extract residue, continuing with 10 times of amount concentration is that 70% (V/V) ethanolic soln carries out refluxing extraction 2 times, and extracting solution is by the D101 macroporous resin, the collection elutriant, and getting phenylethyl alcohol glycoside content through concentrating under reduced pressure, spraying drying is 80% purifying thing 10g.Extract twice with extracting the distilled water that continues to add 15 times of amounts in the residue, decocting, supernatant liquor adds 95% ethanol sedimentation of 3 times of volumes behind concentrating under reduced pressure, left standstill under 4 ℃ 24 hours, centrifugal back collecting precipitation, drying can obtain Herba Cistanches polysaccharide 70g, and purity is 70%.
Embodiment 4:
Herba Cistanches powder 1kg adds 15 times of amount 90% (V/V) ethanol, extracts 2 hours, be the ethanol of 90% (V/V) with 10 times of amount concentration again, extracted 2 hours, merge extracted twice liquid, through concentrating under reduced pressure, crystallization, the dry crystalline material 25g that gets, the D-mannitol content is 35%.Extract residue, continue to extract 2 hours for ethanolic soln, extract twice with 10 times of amount concentration 70% (V/V), united extraction liquid, extracting solution is collected elutriant by the D101 macroporous resin, and getting phenylethyl alcohol glycoside content through concentrating under reduced pressure, spraying drying is 85% purifying thing 8g.To extract the distilled water that continues to add 15 times of amounts in the residue, heating is extracted 2 times, and supernatant liquor adds 95% ethanol sedimentation of 3 times of volumes behind concentrating under reduced pressure, left standstill under 4 ℃ 24 hours, centrifugal back collecting precipitation, drying can obtain Herba Cistanches polysaccharide 100g, and purity is 50%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810025392A CN100590109C (en) | 2008-04-25 | 2008-04-25 | Extraction Technology of Active Components of Herb Cistanche |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810025392A CN100590109C (en) | 2008-04-25 | 2008-04-25 | Extraction Technology of Active Components of Herb Cistanche |
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| CN101265161A CN101265161A (en) | 2008-09-17 |
| CN100590109C true CN100590109C (en) | 2010-02-17 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102670436B (en) * | 2012-03-13 | 2013-09-25 | 珈侬生化科技(中国)有限公司 | Skin-whitening anti-aging cosmetic containing Cistanche tubulosa extract and its preparation method |
| CN103301206A (en) * | 2013-05-21 | 2013-09-18 | 盛晋华 | Integrated technology for unitedly extracting various effectives component of cistanche and manufacturing extract by classes |
| CN104262414B (en) * | 2014-09-17 | 2017-03-22 | 中国科学院过程工程研究所 | Method for preparing phenylethanoid glycoside, mannitol, oligosaccharide syrup and polysaccharide from broomrape |
| CN104804106B (en) * | 2015-04-15 | 2017-07-18 | 江苏天晟药业有限公司 | A kind of purification process of high-purity wheat-based diet |
| CN105796656A (en) * | 2016-05-17 | 2016-07-27 | 杏辉天力（杭州）药业有限公司 | Cistanche tubulosa extract and preparation method thereof |
| CN107082791A (en) * | 2017-03-21 | 2017-08-22 | 青海伊纳维康生物科技有限公司 | A kind of method that phenylethanoid glycosides are extracted from saline cistanche |
| CN109106760B (en) * | 2018-09-29 | 2021-03-23 | 辽宁中医药大学 | New use of cistanche phenylethanoid glycosides in improving sleep and application thereof |
| CN109824738B (en) * | 2019-02-13 | 2021-12-21 | 江苏康缘药业股份有限公司 | Desalination and decoloration method of total oligosaccharide from cistanche deserticola |
| CN115227741A (en) * | 2022-06-09 | 2022-10-25 | 新疆汇峰农业科技有限公司 | Cistanche deserticola extract purification method and equipment |
| CN115068975B (en) * | 2022-06-09 | 2024-05-17 | 新疆汇峰农业科技有限公司 | Cistanche stock solution production method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041677A (en) * | 2007-04-23 | 2007-09-26 | 和田帝辰医药生物科技有限公司 | Producing raw material containing benzyl carbinol glycosides from Cistanche deserticola by using membrane separation technique and preparation method thereof |
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- 2008-04-25 CN CN200810025392A patent/CN100590109C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041677A (en) * | 2007-04-23 | 2007-09-26 | 和田帝辰医药生物科技有限公司 | Producing raw material containing benzyl carbinol glycosides from Cistanche deserticola by using membrane separation technique and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 肉苁蓉有效成分提取集成方法的研究. 欧阳杰，赵兵，王晓东，王玉春.武汉植物学研究，第21卷第6期. 2003 * |
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