CN100590109C - Technique for extracting cynamorlum herba cistanches medicinal materials effective component - Google Patents
Technique for extracting cynamorlum herba cistanches medicinal materials effective component 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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Abstract
The invention relates to a technology for extracting active ingredients from Herba Cistanches, and belongs to the technology field of traditional Chinese medicine component extraction. The extractiontechnology comprises the following steps: broomrape is dried and crushed, and is extracted by adopting ethanol ranging from 90 to 95 percent; extracting solution is concentrated, crystallized and dried to obtain broomrape D-mannite; residue is extracted by using ethanol solution the concentration of which ranges from 60 to 80 percent; the extracting solution passes through macroporous resin; eluent is concentrated and dried to obtain broomrape phenethyl alcohol glycosides; the obtained extracting residue is continuously added with distilled water for heat extraction; after being decompressed and concentrated, supernatant fluid is added with the ethanol of 95 percent for deposition, wherein, the volume of the ethanol is three times of the volume of the supernatant fluid; precipitate is dried to obtain broomrape polyoses. Compared with the traditional method, the technology obtains three broomrape biology bioactive components that are broomrape mannite, the broomrape phenethyl alcohol glycosides and the broomrape polyoses at the same time, and the disadvantage that single-component is emphasized excessively in the traditional extracting method is made up. The ethanol which is used can be recovered during the decompressing and concentrating process to achieve the recycling purpose, thereby effectively lowering 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%.
Claims (2)
1, the extraction process of Herba Cistanches medicinal material effective constituent, its step is as follows:
(1) with Saline Cistanche Herb (Cistanche salsa G.Beck) chylocaulous 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, 95% ethanol sedimentation of supernatant liquor 3 times of volumes of adding after concentrating left standstill 24 hours under 4 ℃, centrifugal back collecting precipitation, drying can obtain the Herba Cistanches polysaccharide.
2, the extraction process of Herba Cistanches medicinal material effective constituent according to claim 1 is characterized in that, the drying means in step (2), (3), (4) is reduced vacuum drying, spraying drying or lyophilize.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN115068975A (en) * | 2022-06-09 | 2022-09-20 | 新疆汇峰农业科技有限公司 | Production method of cistanche salsa stock solution |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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| 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 |
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| 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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