CN101810654B - Vinegar-prepared radix bupleuri solvent extract is preparing the application in anticholesteremic agent - Google Patents
Vinegar-prepared radix bupleuri solvent extract is preparing the application in anticholesteremic agent Download PDFInfo
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- CN101810654B CN101810654B CN200910046593.4A CN200910046593A CN101810654B CN 101810654 B CN101810654 B CN 101810654B CN 200910046593 A CN200910046593 A CN 200910046593A CN 101810654 B CN101810654 B CN 101810654B
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Abstract
The invention discloses vinegar-prepared radix bupleuri solvent extract and preparing the application in anticholesteremic agent, described solvent is water, ethanol, methanol or its mixture.Described vinegar-prepared radix bupleuri solvent extract can be refined by resin method after alcohol extraction or decoction and alcohol sedimentation technique further.The Radix Bupleuri (processed with vinegar) extract obtained by the present invention has obvious effect in cholesterol reducing.
Description
Technical field
The present invention relates to field of natural medicinal chemistry, specifically, relate to vinegar-prepared radix bupleuri solvent extract and preparing the application in anticholesteremic agent.
Background technology
Radix Bupleuri is the dry root of umbelliferae bupleurum BupleurumchinenseDC. or Radix Bupeuri Scorzonerfolii. BupleurumscorzonerifoliumWild., and bitter in the mouth, is slightly cold, return liver, gallbladder meridian, there is evacuation bring down a fever, the effect of soothing liver-QI, yang invigorating, be listed in top grade in book on Chinese herbal medicine.Be monarch drug mainly with Radix Bupleuri in the hepatopathy medication of history tree and modern Chinese medicine.But the different processed product treatment disease emphasis of Radix Bupleuri differ, when being used for the treatment of hepatopathy, its vinegar goods conventional, compared with the raw product of Radix Bupleuri are used for inducing sweat and bring down a fever, vinegar goods can relax and rise loose property, contribute to priming and enter liver, strengthen the effect of dispersing the depressed liver-QI for alleviating pain, be applicable to the cards such as the hypochondriac pain of stagnation of QI due to depression of the liver, stomachache and menoxenia.The preparation method of Radix Bupleuri (processed with vinegar), according to the Pharmacopoeia of the People's Republic of China 2005 editions annex IID stir-baking with vinegar, is namely got the clean medical material of Radix Bupleuri, is mixed thoroughly with vinegar, vexed, puts in pot, when frying the degree to regulation, takes out, cools.
The extracting method that Chinese patent 200710039351.3 discloses a kind of Radix Bupleuri (processed with vinegar) active site traditional is as follows: Radix Bupleuri (processed with vinegar) alcohol percolation, by alcohol evaporate to dryness, obtains fluid extract; Gained fluid extract ethanol or water are diluted to suspension, and described suspension extracts by organic solvent petroleum ether, chloroform and ethyl acetate successively respectively, by ethyl acetate layer evaporate to dryness, obtains Radix Bupleuri ethyl acetate extract; Or described suspension uses organic solvent petroleum ether, chloroform, ethyl acetate and n-butanol extraction successively respectively, by n-butanol layer evaporate to dryness, obtain Radix Bupleuri n-butanol extract.The Radix Bupleuri (processed with vinegar) extract that extraction like this obtains is proved the effect with certain secretion of bile.
Disclose injection of Radix Bupleuri in paper " the injection of Radix Bupleuri lipid-lowering effect preliminary observation " literary composition that the people such as the Li Huantang of Guilin hospital of air force deliver and there is the effect reducing serum triglycerides, but then fail to support to the effect reducing cholesterol.
Therefore, document is not yet had to disclose the effect of vinegar-prepared radix bupleuri solvent extract in cholesterol reducing up to now.
Summary of the invention
For solving the problems of the technologies described above, the present inventor improves the extracting method of traditional Radix Bupleuri (processed with vinegar) active site, obtains the Radix Bupleuri (processed with vinegar) extract having obvious effect in cholesterol reducing.
The object of this invention is to provide vinegar-prepared radix bupleuri solvent extract and preparing the application in anticholesteremic agent, described solvent is water, ethanol, methanol or its mixture.
After alcohol extraction, resin method or decoction and alcohol sedimentation technique are generally used for refining extract.General step is the solution after alcohol extraction or water extract-alcohol precipitation, concentrated, obtains the concentrated night of certain density, through macroporous resin column chromatography, with the ethanol eluting successively of water and variable concentrations, finally obtains extract.Alcohol used is generally methanol, ethanol, isopropyl alcohol or its mixture, and selects suitable resin according to the character of extract.
After alcohol extraction of the present invention, the concrete operation step of resin method is as follows: the methanol of Radix Bupleuri (processed with vinegar) 50%-100% concentration or alcoholic solution heating and refluxing extraction, extracting solution merging is concentrated into low concentration, concentrated solution macroporous resin column chromatography, with the ethanol eluting successively of water and variable concentrations, obtain vinegar-prepared radix bupleuri solvent extract.
Wherein, it is 20-40% that extracting solution heating and refluxing extraction obtained is concentrated into concentration, and preferably extracting solution being concentrated into concentration is 30%.
Described macroporous resin is nonpolar macroporous adsorption resin, is preferably 860021 types.
The ethanol of described variable concentrations is preferably the ethanol of 30-95%, is more preferably the ethanol of 30%, 50%, 70% or 95%.
The concrete operation step of decoction and alcohol sedimentation technique of the present invention is as follows: Radix Bupleuri (processed with vinegar) water heating extraction, and extracting solution merging is concentrated into low-density, adds ethanol and generation is precipitated, and make mixed liquor be concentrated into high concentration, abundant ultrasonic rear standing, obtains Radix Bupleuri (processed with vinegar) extract.
Wherein, preferably by merging with the extracting solution after water heating extraction, to be concentrated into density be 1.1-1.2; Adding ethanol makes generation precipitate, and wherein the concentration of ethanol is 70%-100%; It is 60-80% that mixed liquor is concentrated into concentration, is preferably 70%.
The Radix Bupleuri (processed with vinegar) extract that above-mentioned steps obtains can be refined further: again filter gained Radix Bupleuri (processed with vinegar) extract, concentrated filtrate, macroporous resin on concentrated solution, with the ethanol eluting successively of water and variable concentrations, obtains refining vinegar-prepared radix bupleuri solvent extract.
Wherein, described macroporous resin is nonpolar macroporous adsorption resin, is preferably 860021 types.
The ethanol of described variable concentrations is preferably the ethanol of 30-95%, is more preferably the ethanol of 30%, 50%, 70% or 95%.
The method that the present invention obtains extract from Radix Bupleuri (processed with vinegar) is simple, and this extract has obvious effect in cholesterol reducing.
Detailed description of the invention
Embodiment 1
Radix Bupleuri (processed with vinegar) 1000g, by 8 times amount 75% alcoholic solution heating and refluxing extraction 2 times for several times, extracting solution merging is concentrated into 30% concentration, macroporous resin on concentrated solution, wash liquid, 30% ethanol, 50% ethanol, 70% ethanol and 95% ethanol elution successively with water, obtain 30% ethanol elution (No. 4 extracts), 50% ethanol elution (No. 3 extracts), 70% ethanol elution (No. 2 extracts), 95% ethanol elution (No. 1 extract) respectively.
Embodiment 2
Radix Bupleuri (processed with vinegar) 500g, micro-extraction 2 times of boiling is heated to water, it is 1.1 that extracting solution merging is concentrated into density, adding 3 times amount 95% ethanol makes generation precipitate, and about making final mixed liquid concentration to 70%, abundant ultrasonic standing a period of time, filter, be divided into precipitation (No. 5 extracts) and filtrate (No. 6 extracts).
Embodiment 3
Radix Bupleuri (processed with vinegar) 500g, is heated to micro-extraction 2 times of boiling with water, and it is 1.1 that extracting solution merging is concentrated into density, adding 3 times amount 95% ethanol makes generation precipitate, and about making final mixed liquid concentration to 70%, abundant ultrasonic standing a period of time, filter, be divided into precipitation and filtrate, the concentrated suitable quantity of water that adds of filtrate produces precipitation, filter, be divided into precipitation and filtrate, filtrate concentrates, upper macroporous resin, use water and 70% ethanol elution successively, obtain water lotion and 70% ethanol elution (No. 7 extracts).
Radix Bupleuri (processed with vinegar) used in embodiment 1 is that Shanghai Leiyunshang Chinese Traditional Medicine Crude Slices Factory produces; Lot number: criticize 3; Date of manufacture: 2006.12.7;
Radix Bupleuri (processed with vinegar) used in embodiment 2,3 is that Shanghai Leiyunshang Chinese Traditional Medicine Crude Slices Factory produces; Lot number: criticize 2; Date of manufacture: 2006.12.7;
Macroporous resin used in above embodiment is 860021 types that resin subsidiary factory of Lukang Medical Co., Ltd., Shandong produces;
The ultrasonic KQ2200 type ultrasonic cleaner for Kunshan Ultrasonic Instruments Co., Ltd.'s production used in above embodiment.
Pharmacodynamic result:
Test example 1: gained Radix Bupleuri (processed with vinegar) extract of the present invention is on the impact of biliary cholesterol
1. laboratory animal
SD rat, ♂, about 250 grams.
2. test dose
High and low two dosage groups established by each sample, low dose group: 300mg/kg;
High dose group: 1g/kg.
3. experimental technique
Experimental technique is with reference to " herbal pharmacology experimental methodology (second edition) " 472-474 page
Rat random packet, is divided into blank group, No. 1-6 6 samples, 12 groups, often organizes 6 rats.Rat, through the anesthesia of lumbar injection 3% secobarbital, opens abdominal cavity after anesthesia, is separated common bile duct, draws bile with self-control plastic straw.Different lot number, dose drug after 30 minutes (0-30 minute), are respectively injected stomach with No. 9 pins at collection bile by each rat.By 0-30 minute, 30-60 minute before administration, 60-90 minute, 90-120 minute, 120-150 minute, 5 time points collect bile, and statistics secretion quantity, analyzes the content of bile cholesterol.This experiment point completes for several days, has some dosage group rats to occur dead in experimentation.The results are shown in following table 1.
Table 1
Compare with matched group:
*p < 0.05;
*p < 0.01
Compare with before organizing administration:
#p < 0.05;
##p < 0.01
Conclusion: as shown in Table 1, No. 1, No. 2, No. 3, No. 5, No. 6 samples compare with matched group, all have the effect reducing cholesterol; No. 4 samples compare the effect that has and reduce cholesterol with matched group and there were significant differences, comparing, showing certain dosage effect with organizing various dose.
Gained Radix Bupleuri (processed with vinegar) extract of the present invention all has the effect reducing biliary cholesterol, and No. 4 sample activity are remarkable.
Test example 2: gained Radix Bupleuri (processed with vinegar) extract of the present invention is on the impact of biliary cholesterol
1. laboratory animal
SD rat, ♂, about 250 grams.
2. test dose
High and low two the dosage groups of each sample, low dose group: 50mg/kg;
High dose group: 300mg/kg.
High and low two the dosage groups of positive drug, low dose group: 50mg/kg;
High dose group: 150mg/kg.
3. experimental technique:
Experimental technique is with reference to " herbal pharmacology experimental methodology (second edition) " 472-474 page.
The pharmacological action of the ursodesoxycholic acid of use reference " pharmacology's (third edition) Zhu Xinying edits " 255 pages of positive drug (ursodesoxycholic acid).
Rat random packet, is divided into blank group, positive drug (ursodesoxycholic acid), 4, No. 6 samples.Rat, through the anesthesia of lumbar injection 3% secobarbital, opens abdominal cavity after anesthesia, is separated common bile duct, draws bile with self-control plastic straw.Different lot number, dose drug after 30 minutes (0-30 minute), are respectively injected stomach with No. 9 pins at collection bile by each rat.By 0-30 minute, 30-60 minute before administration, 60-90 minute, 90-120 minute, 120-150 minute, 5 time points collect bile, and statistics secretion quantity, analyzes the content of bile cholesterol.The results are shown in following table 2.
Table 2
Divide with 0-30 and compare
*p < 0.05;
*p < 0.05.
Conclusion: as shown in Table 2, No. 4, No. 7 samples compare the effect that has and reduce cholesterol with matched group and there were significant differences, compare, show the advantage of certain pharmacologically active with positive drug.
The further screening of the present invention's No. 4, No. 7 Radix Bupleuri (processed with vinegar) extracts shows it all good pharmacologically active, reduces the effect highly significant of biliary cholesterol.
Claims (6)
1. vinegar-prepared radix bupleuri solvent extract reduces the application in biliary cholesterol medicine in preparation, wherein said solvent is water, ethanol, methanol or its mixture, described vinegar-prepared radix bupleuri solvent extract is prepared according to the following steps: the methanol of Radix Bupleuri (processed with vinegar) 50%-100% concentration or alcoholic solution heating and refluxing extraction, extracting solution merging is concentrated into low concentration, macroporous resin on concentrated solution, with the ethanol eluting successively of water and variable concentrations, obtain vinegar-prepared radix bupleuri solvent extract; Or Radix Bupleuri (processed with vinegar) water heating extraction, it is 1.1-1.2 that extracting solution merging is concentrated into density, adds 70%-100% ethanol and generation is precipitated, and make mixed liquor be concentrated into 60-80%, abundant ultrasonic rear standing, obtain vinegar-prepared radix bupleuri solvent extract, filter described Radix Bupleuri (processed with vinegar) extract further, concentrated filtrate, macroporous resin on concentrated solution, with the ethanol eluting successively of water and variable concentrations, obtain refining Radix Bupleuri (processed with vinegar) extract, the ethanol of wherein said variable concentrations is the ethanol of 30-70%.
2. application according to claim 1, is characterized in that, described low concentration is 20-40%.
3. application according to claim 2, is characterized in that, described low concentration is 30%.
4. application according to claim 1, is characterized in that, described macroporous resin is nonpolar macroporous adsorption resin.
5. application according to claim 4, is characterized in that, described macroporous resin is 860021 types.
6. application according to claim 1, is characterized in that, the ethanol of described variable concentrations is the ethanol of 30%, 50% or 70%.
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| CN102526144B (en) * | 2010-12-14 | 2014-07-30 | 上海医药工业研究院 | Vinegar-processed Chinese thorowax root extract, its preparation method and application in preparation of antilipemic medicament |
| CN108210532A (en) * | 2018-02-26 | 2018-06-29 | 广州中医药大学(广州中医药研究院) | Bupleurum extract is preparing the application in adjusting the drug of metabolism and fat reducing health products |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1714811A (en) * | 2004-06-30 | 2006-01-04 | 天津天士力制药股份有限公司 | Radix bupleuri dripping pill and its preparing method |
| CN101062071A (en) * | 2007-06-18 | 2007-10-31 | 石任兵 | Total saponins from radix bupleuri extract and the preparing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1714811A (en) * | 2004-06-30 | 2006-01-04 | 天津天士力制药股份有限公司 | Radix bupleuri dripping pill and its preparing method |
| CN101062071A (en) * | 2007-06-18 | 2007-10-31 | 石任兵 | Total saponins from radix bupleuri extract and the preparing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 吴静.炮制对柴胡有效成分与临床运用的影响.《湖北中医杂志》.2008,第30卷(第9期),第60-61页. * |
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