CN103232515A - Cyclocarya paliurus glucoside I preparation method - Google Patents
Cyclocarya paliurus glucoside I preparation method Download PDFInfo
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- CN103232515A CN103232515A CN 201310179384 CN201310179384A CN103232515A CN 103232515 A CN103232515 A CN 103232515A CN 201310179384 CN201310179384 CN 201310179384 CN 201310179384 A CN201310179384 A CN 201310179384A CN 103232515 A CN103232515 A CN 103232515A
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Abstract
The invention discloses a cyclocarya paliurus glucoside I preparation method. The cyclocarya paliurus glucoside I preparation method comprises the following steps of: (1) smashing dried cyclocarya paliurus leaves, soaking in 5-10 times amount of 50-80% methanol solution and extracting for 2-3 times, concentrating an extracting solution under reduced pressure till alcohol does not exist, adding the concentrated extracting solution to a macroporous resin column for absorption, washing with water till caramel does not exist, eluting by a 3-6 times column volume of 40-70% alcohol solution, collecting eluant, and concentrating under reduced pressure to obtain a concentrated solution; and (2) absorbing the concentrated solution by macroporous resin, drying to remove moisture, packing, carrying out gradient elution by ethyl acetate and methanol, collecting fractions, concentrating and drying under reduced pressure to obtain the cyclocarya paliurus glucoside I. The cyclocarya paliurus glucoside I preparation method has the characteristics that the operation is simple and convenient, the preparation quantity is large, and the industrial production is easy.
Description
Technical field
The invention belongs to the Separation of Natural Products field, relate in particular to a kind of method for preparing Cyclocarya paliurus glycosides I.
Background technology
Cyclocarya paliurus, money tree, numb willow again, Juglandaceae.Cydocaryap paliurus (Baud.) Iljinsk.leaf is made tea and is had adjusting blood sugar, activates the pancreas islet organ dysfunction, promotes the blood sugar metabolism, is epoch-making great discovery on the treating diabetes history.Cyclocarya paliurus glycosides I is sweet ingredient in the Cyclocarya paliurus, and is non-calorific value saponins, can satisfy hyperglycemic patients to the demand of sweet taste, and not increase the weight of the state of an illness, has good effect aspect hypoglycemic, lipopenicillinase, the step-down simultaneously.
Cyclocarya paliurus glycosides I (Cyclocarioside I) belongs to triterpene saponin, and molecular formula is C
41H
70O
12, molecular weight 755.01.
By searching document, preparation Cyclocarya paliurus glycosides I method adopts the silicagel column method to separate more, these class methods, and product yield is low, and produces a large amount of silica gel wastes, is not suitable for suitability for industrialized production.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of industrial method for preparing Cyclocarya paliurus glycosides I.
The present invention realizes by the following technical solutions: a kind of method for preparing Cyclocarya paliurus glycosides I is characterized in that comprising following steps:
(1) get the Cyclocarya paliurus dry leave and pulverize, soak with 5 ~ 10 times of amount 50 ~ 80% methanol solutions and extract 2 ~ 3 times, extracting solution is evaporated to does not have alcohol, add in the macroporous resin column and adsorb, wash no fried sugar, use 3 ~ 6 times of column volumes, 40 ~ 70% ethanolic soln wash-outs again, collect elutriant, concentrating under reduced pressure gets concentrated solution;
(2) above-mentioned concentrated solution adds in the macroporous resin and adsorbs, volatilize moisture after, the dress post, ethyl acetate, methyl alcohol gradient elution are collected flow point and are concentrated, drying under reduced pressure is namely.A kind of in the step (1), (2) among the optional ADS-21 of macroporous resin model, NK-II, AB-8 and the HPD-700.
Ethyl acetate, methyl alcohol gradient elution are in the step (2): (10 ~ 20:1) wash-out impurity are used 4 ~ 8 times of column volume ethyl acetate/methanol (5:3) wash-out effective constituent again with 5 ~ 10 times of column volume ethyl acetate/methanol earlier.
Adopt the present invention to prepare Cyclocarya paliurus glycosides I, simple to operate, the product yield height, and pollute little.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to the following example.
Embodiment:
Embodiment 1:
Getting Cyclocarya paliurus dry leave 10kg pulverizes, soak extraction 3 times with 8 times of amount 70% methanol solutions, each 3 hours, extracting solution is evaporated to does not have alcohol, add in the ADS-21 macroporous resin column and adsorb, wash no fried sugar, use 4 times of column volumes, 50% ethanolic soln wash-out again, collect elutriant, concentrating under reduced pressure gets concentrated solution, adds in the AB-8 macroporous resin to adsorb, volatilize moisture after, the dress post, with 6 times of column volume ethyl acetate/methanol (10:1) wash-out impurity, use 8 times of column volume ethyl acetate/methanol (5:3) wash-out effective constituent more earlier, collect flow point and concentrate, drying under reduced pressure gets white powder Cyclocarya paliurus glycosides I 180g, content 98.5%.
Embodiment 2:
Getting Cyclocarya paliurus dry leave 10kg pulverizes, soak extraction 3 times with 5 times of amount 60% methanol solutions, each 5 hours, extracting solution is evaporated to does not have alcohol, add in the NK-II macroporous resin column and adsorb, wash no fried sugar, use 6 times of column volumes, 60% ethanolic soln wash-out again, collect elutriant, concentrating under reduced pressure gets concentrated solution, adds in the HPD-700 macroporous resin to adsorb, volatilize moisture after, the dress post, with 8 times of column volume ethyl acetate/methanol (20:1) wash-out impurity, use 6 times of column volume ethyl acetate/methanol (5:3) wash-out effective constituent more earlier, collect flow point and concentrate, drying under reduced pressure gets white powder Cyclocarya paliurus glycosides I 205g, content 95.7%.
Embodiment 3:
Getting Cyclocarya paliurus dry leave 10kg pulverizes, soak extraction 2 times with 10 times of amount 80% methanol solutions, each 4 hours, extracting solution is evaporated to does not have alcohol, add in the AB-8 macroporous resin column and adsorb, wash no fried sugar, use 5 times of column volumes, 40% ethanolic soln wash-out again, collect elutriant, concentrating under reduced pressure gets concentrated solution, adds in the HPD-700 macroporous resin to adsorb, volatilize moisture after, the dress post, with 5 times of column volume ethyl acetate/methanol (15:1) wash-out impurity, use 6 times of column volume ethyl acetate/methanol (5:3) wash-out effective constituent more earlier, collect flow point and concentrate, drying under reduced pressure gets white powder Cyclocarya paliurus glycosides I 190g, content 97.1%.
Embodiment 4:
Getting Cyclocarya paliurus dry leave 10kg pulverizes, soak extraction 2 times with 7 times of amount 80% methanol solutions, each 5 hours, extracting solution is evaporated to does not have alcohol, add in the NK-II macroporous resin column and adsorb, wash no fried sugar, use 5 times of column volumes, 60% ethanolic soln wash-out again, collect elutriant, concentrating under reduced pressure gets concentrated solution, adds in the AB-8 macroporous resin to adsorb, volatilize moisture after, the dress post, with 7 times of column volume ethyl acetate/methanol (13:1) wash-out impurity, use 6 times of column volume ethyl acetate/methanol (5:3) wash-out effective constituent more earlier, collect flow point and concentrate, drying under reduced pressure gets white powder Cyclocarya paliurus glycosides I 212g, content 96.3%.
Claims (3)
1. method for preparing Cyclocarya paliurus glycosides I is characterized in that comprising following steps:
(1) get the Cyclocarya paliurus dry leave and pulverize, soak with 5 ~ 10 times of amount 50 ~ 80% methanol solutions and extract 2 ~ 3 times, extracting solution is evaporated to does not have alcohol, add in the macroporous resin column and adsorb, wash no fried sugar, use 3 ~ 6 times of column volumes, 40 ~ 70% ethanolic soln wash-outs again, collect elutriant, concentrating under reduced pressure gets concentrated solution;
(2) above-mentioned concentrated solution adds in the macroporous resin and adsorbs, volatilize moisture after, the dress post, ethyl acetate, methyl alcohol gradient elution are collected flow point and are concentrated, drying under reduced pressure is namely.
2. the method for preparing Cyclocarya paliurus glycosides I as claimed in claim 1 is characterized in that in described step (1), (2) a kind of among the optional ADS-21 of macroporous resin model, NK-II, AB-8 and the HPD-700.
3. the method for preparing Cyclocarya paliurus glycosides I as claimed in claim 1, it is characterized in that ethyl acetate, methyl alcohol gradient elution are in the described step (2): (10 ~ 20:1) wash-out impurity are used 4 ~ 8 times of column volume ethyl acetate/methanol (5:3) wash-out effective constituent again with 5 ~ 10 times of column volume ethyl acetate/methanol earlier.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201310179384 CN103232515A (en) | 2013-05-15 | 2013-05-15 | Cyclocarya paliurus glucoside I preparation method |
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| CN 201310179384 CN103232515A (en) | 2013-05-15 | 2013-05-15 | Cyclocarya paliurus glucoside I preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554209A (en) * | 2013-11-15 | 2014-02-05 | 中国人民解放军第四一一医院 | Method for preparing ginsenoside Rg1 from pseudo-ginseng |
| CN104971090A (en) * | 2015-08-03 | 2015-10-14 | 中国药科大学 | Application of cyclocarya paliurus effective part in preparation of medicine used for treating non-alcoholic fatty liver disease |
| CN109364119A (en) * | 2018-12-26 | 2019-02-22 | 浙江大学 | Preparation has the method and application of the total triterpene of hypoglycemic effect from Qingqian Willow leaf |
| CN112625080A (en) * | 2021-01-04 | 2021-04-09 | 湖南华诚生物资源股份有限公司 | Cyclocarya paliurus triterpenoid saponin monomer separation method |
-
2013
- 2013-05-15 CN CN 201310179384 patent/CN103232515A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554209A (en) * | 2013-11-15 | 2014-02-05 | 中国人民解放军第四一一医院 | Method for preparing ginsenoside Rg1 from pseudo-ginseng |
| CN103554209B (en) * | 2013-11-15 | 2015-04-22 | 中国人民解放军第四一一医院 | Method for preparing ginsenoside Rg1 from pseudo-ginseng |
| CN104971090A (en) * | 2015-08-03 | 2015-10-14 | 中国药科大学 | Application of cyclocarya paliurus effective part in preparation of medicine used for treating non-alcoholic fatty liver disease |
| CN109364119A (en) * | 2018-12-26 | 2019-02-22 | 浙江大学 | Preparation has the method and application of the total triterpene of hypoglycemic effect from Qingqian Willow leaf |
| CN109364119B (en) * | 2018-12-26 | 2021-10-01 | 浙江大学 | Method for preparing total triterpenoids with blood sugar reducing effect from cyclocarya paliurus leaves and application of total triterpenoids |
| CN112625080A (en) * | 2021-01-04 | 2021-04-09 | 湖南华诚生物资源股份有限公司 | Cyclocarya paliurus triterpenoid saponin monomer separation method |
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Application publication date: 20130807 |