CN101775049A - Method for extracting and purifying salidroside from glossy privet fruit - Google Patents
Method for extracting and purifying salidroside from glossy privet fruit Download PDFInfo
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- CN101775049A CN101775049A CN201010111783A CN201010111783A CN101775049A CN 101775049 A CN101775049 A CN 101775049A CN 201010111783 A CN201010111783 A CN 201010111783A CN 201010111783 A CN201010111783 A CN 201010111783A CN 101775049 A CN101775049 A CN 101775049A
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Abstract
The invention relates to a method for extracting and purifying salidroside from glossy privet fruit, which comprises the following steps: taking the glossy privet fruit as a raw material; stewing the material in ethanol with the concentration of 15-50%, and drying; dispersing an obtained crude product in cold water which is 5-8 times (V/W)of the amount of the crude product; adding ethyl acetate for extraction, wherein the amount of the ethyl acetate is 3-5 times of that of the product obtained from the last step; aqueous phase filtering, decontaminating by using a nanofiltration membrane with the cut-off molecular weight of 300-500, reducing the pressure of permeate and concentrating to 1/10-1/15 of the original volume; standing and crystallizing; saturating and dissolving in methanol with the concentration of 90-95%; and recrystallizating for 3 times to obtain the product. The method has high raw material utilization efficient of products, small dosage of solvent, low cost, high yield and purity.
Description
Technical field:
The present invention relates to a kind of method of extracting purifying salidroside from Glossy Privet Fruit, especially a kind of ethanol that adopts is stewed the method that system, membrane sepn and recrystallization prepare rhodioside.
Background technology:
Rhodioside (Salidroside) has another name called salidroside, Salidroside.
Chemical name: p-hydroxyphenylethanol glucopyranoside
Molecular formula: C
14H
20O
7
Molecular weight: 300.31
Character: white crystalline powder.Fusing point 165.5-166.5 ℃, water-soluble, ethanol, methyl alcohol, butanols are insoluble in ether, chloroform, ethyl acetate.
Rhodioside is the main active ingredient of Tibetan medicine Root of Kirilow Rhodiola (Rhadolia rasea L.), also is that it adapts to the necessary composition of high mountain severe environment.Studies show that rhodioside has expansion resistance vessel and capacity vessel, resist myocardial ischemia, multiple pharmacological effect such as anti-hepatic fibrosis that rhodioside obtains Application and Development widely as medicine and protective foods.
The general preparation method of rhodioside is chemosynthesis and extracts from Root of Kirilow Rhodiola.Rhodiola plant grows in the highlands, natural resources shortage and costing an arm and a leg.The Chinese medicine Glossy Privet Fruit is the dry mature fruit of Oleaceae plant glossy privet ligustrum lucidum Ait., contains the various active composition, comprises the rhodioside that content is considerable.China Glossy Privet Fruit plant is widely distributed, aboundresources and cheap.
Summary of the invention:
The contriver tests through process optimization, has invented a kind of method of extracting purifying salidroside from Glossy Privet Fruit.This technology is simple to operation, the product yield height, and production cost is low.
The present invention realizes by the following technical solutions:
1) the stewed system of ethanol: get clean Glossy Privet Fruit, put in the reactor, the aqueous ethanolic solution that adds material quantity 1/4-1/5 is mixed thoroughly, sealing, and vexed profit 4-6h uses steam heating, stewes system 12-24h, dries in the baking oven, gets crude product;
2) membrane sepn: above-mentioned crude product is scattered in the cold water, filters, use ethyl acetate extraction, the nanofiltration membrane of molecular weight cut-off 300-500 is crossed in water intaking mutually, sees through liquid and concentrates, and leaves standstill crystallization;
3) recrystallization: coarse crystallization is leached the saturated dissolving of heating in 90-95% methyl alcohol, leave standstill crystallization, leach crystallisate, repeat 2 times, place crystallization, leach cryodrying and promptly get product.
Above-mentioned preparation method is characterized in that described 1) the stewed system condition of middle ethanol: the concentration of aqueous ethanolic solution is 15-50%.
Above-mentioned preparation method is characterized in that described 2) in the cold water consumption be that the 5-8 of crude product doubly measures (V/W), the ethyl acetate consumption is that the 3-5 of crude product doubly measures (V/W).
Above-mentioned preparation method is characterized in that described 2) middle crystallization condition: see through the 1/10-1/15 that liquid is concentrated into its volume, crystallization time 2-3h.
Above-mentioned preparation method is characterized in that described recrystallization condition: crystallization time 2-3h.
In sum, there is following advantage in the present invention: a lot of unsettled iridoid glycosides that contains in the Glossy Privet Fruit all has the rhodioside parent nucleus, can hydrolysis generate the secondary glycoside rhodioside through the system of stewing, and has improved raw material availability; Rhodioside is insoluble in ethyl acetate, therefore can remove a part of non-water soluble substance by extraction; The rhodioside molecular weight is lower, is similar to the minimum molecular weight cut-off of nanofiltration membrane, and transmitance is very high, plays good refining effect.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
The assay of rhodioside adopts high performance liquid chromatography (with reference to " extracting the technical study of rhodioside from Glossy Privet Fruit " documents such as wangdans) among the following embodiment, and concrete grammar is as follows:
High-efficient liquid phase chromatogram condition:
Chromatographic column: Hypersil-C
18Analyze chromatographic column (4.6mm * 150mm, 5 μ m);
Moving phase: methyl alcohol: water (20: 80);
Flow velocity: 0.4mL/min;
Detect wavelength: 220nm;
Sample size: 20 μ L;
Sensitivity: 0.010AUFs
Embodiment 1:
Get Glossy Privet Fruit raw material 10kg, place reactor, add 2L 50% ethanol, vexed profit 4h, steam heating is stewed system 12h, dries in baking oven, gets the 35.8g crude product.Dissolving crude product in 160ml cold water, is removed by filter insolubles, and filtrate adds the 120ml ethyl acetate extraction, is evaporated to 20ml after the nanofiltration membrane removal of impurities of water by molecular weight cut-off 300-500, leaves standstill the 2h crystallization, gets coarse crystallization 26.1g.Coarse crystallization heats saturated dissolving with 90% methyl alcohol, puts cold 2h crystallization, and recrystallization is 2 times again, leaches crystallization, leaches cryodrying, gets product 18.5g, content 96.1%.
Embodiment 2:
Get Glossy Privet Fruit raw material 10kg, place reactor, add 2.5L 35% ethanol, vexed profit 5h, steam heating is stewed system 16h, dries in baking oven, gets the 34.3g crude product.Dissolving crude product in 210ml cold water, is removed by filter insolubles, and filtrate adds the 140ml ethyl acetate extraction, is evaporated to 16ml after the nanofiltration membrane removal of impurities of water by molecular weight cut-off 300-500, leaves standstill the 2.5h crystallization, gets coarse crystallization 28.4g.Coarse crystallization heats saturated dissolving with 92% methyl alcohol, puts cold 2.5h crystallization, and recrystallization is 2 times again, leaches crystallization, leaches cryodrying, gets product 20.4g, content 95.7%.
Embodiment 3:
Get Glossy Privet Fruit raw material 10kg, place reactor, add 2.3L 35% ethanol, vexed profit 6h, steam heating is stewed system 20h, dries in baking oven, gets the 36.5g crude product.Dissolving crude product in 250ml cold water, is removed by filter insolubles, and filtrate adds the 150ml ethyl acetate extraction, is evaporated to 20ml after the nanofiltration membrane removal of impurities of water by molecular weight cut-off 300-500, leaves standstill the 3h crystallization, gets coarse crystallization 29.6g.Coarse crystallization heats saturated dissolving with 95% methyl alcohol, puts cold 3h crystallization, and recrystallization is 2 times again, leaches crystallization, leaches cryodrying, gets product 23.8g, content 96.4%.
Embodiment 4:
Get Glossy Privet Fruit raw material 10kg, place reactor, add 3L 15% ethanol, vexed profit 6h, steam heating is stewed system 24h, dries in baking oven, gets the 35.5g crude product.Dissolving crude product in 240ml cold water, is removed by filter insolubles, and filtrate adds the 180ml ethyl acetate extraction, is evaporated to 16ml after the nanofiltration membrane removal of impurities of water by molecular weight cut-off 300-500, leaves standstill the 3h crystallization, gets coarse crystallization 28.5g.Coarse crystallization heats saturated dissolving with 95% methyl alcohol, puts cold 2h crystallization, and recrystallization is 2 times again, leaches crystallization, leaches cryodrying, gets product 22.9g, content 96.7%.
Claims (5)
1. method of extracting purifying salidroside from Glossy Privet Fruit is characterized in that comprising following steps:
1) the stewed system of ethanol: get clean Glossy Privet Fruit, put in the reactor, the aqueous ethanolic solution that adds material quantity 1/4-1/5 is mixed thoroughly, sealing, and vexed profit 4-6h uses steam heating, stewes system 12-24h, dries in the baking oven, gets crude product;
2) membrane sepn: above-mentioned crude product is scattered in the cold water, filters, use ethyl acetate extraction, the nanofiltration membrane of molecular weight cut-off 300-500 is crossed in water intaking mutually, sees through liquid and concentrates, and leaves standstill crystallization;
3) recrystallization: coarse crystallization is leached the saturated dissolving of heating in 90-95% methyl alcohol, leave standstill crystallization, leach crystallisate, repeat 2 times, place crystallization, leach cryodrying and promptly get product.
2. preparation method as claimed in claim 1 is characterized in that described 1) the stewed system condition of middle ethanol: the concentration of aqueous ethanolic solution is 15-50%.
3. preparation method as claimed in claim 1 is characterized in that described 2) in the cold water consumption be that the 5-8 of crude product doubly measures (V/W), the ethyl acetate consumption is that the 3-5 of crude product doubly measures (V/W).
4. preparation method as claimed in claim 1 is characterized in that described 2) middle crystallization condition: see through the 1/10-1/15 that liquid is concentrated into its volume, crystallization time 2-3h.
5. preparation method as claimed in claim 1 is characterized in that described 3) middle recrystallization condition: crystallization time 2-3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010111783A CN101775049A (en) | 2010-02-08 | 2010-02-08 | Method for extracting and purifying salidroside from glossy privet fruit |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010111783A CN101775049A (en) | 2010-02-08 | 2010-02-08 | Method for extracting and purifying salidroside from glossy privet fruit |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321127A (en) * | 2011-07-05 | 2012-01-18 | 石任兵 | Novel method for preparing salidroside from glossy privet fruit |
| CN102492003A (en) * | 2011-11-30 | 2012-06-13 | 四川浩源生物科技有限公司 | Technique for extracting and separating salidroside from glossy privet fruit |
| CN102603819A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Preparation method of rosavin |
| CN103351416A (en) * | 2013-08-02 | 2013-10-16 | 福建中医药大学 | New crystal form A of salidroside and preparation method thereof |
| CN104017036A (en) * | 2014-06-11 | 2014-09-03 | 福建中医药大学 | Novel crystal form of rhodioloside and preparation method of novel crystal form |
-
2010
- 2010-02-08 CN CN201010111783A patent/CN101775049A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603819A (en) * | 2011-01-25 | 2012-07-25 | 苏州宝泽堂医药科技有限公司 | Preparation method of rosavin |
| CN102321127A (en) * | 2011-07-05 | 2012-01-18 | 石任兵 | Novel method for preparing salidroside from glossy privet fruit |
| CN102492003A (en) * | 2011-11-30 | 2012-06-13 | 四川浩源生物科技有限公司 | Technique for extracting and separating salidroside from glossy privet fruit |
| CN102492003B (en) * | 2011-11-30 | 2014-05-07 | 四川浩源生物科技有限公司 | Technique for extracting and separating salidroside from glossy privet fruit |
| CN103351416A (en) * | 2013-08-02 | 2013-10-16 | 福建中医药大学 | New crystal form A of salidroside and preparation method thereof |
| CN104017036A (en) * | 2014-06-11 | 2014-09-03 | 福建中医药大学 | Novel crystal form of rhodioloside and preparation method of novel crystal form |
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Application publication date: 20100714 |