CN103446214B - A kind of preparation method of Radix Berberidis kunmingensis extract - Google Patents
A kind of preparation method of Radix Berberidis kunmingensis extract Download PDFInfo
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- CN103446214B CN103446214B CN201310363150.4A CN201310363150A CN103446214B CN 103446214 B CN103446214 B CN 103446214B CN 201310363150 A CN201310363150 A CN 201310363150A CN 103446214 B CN103446214 B CN 103446214B
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Abstract
The invention belongs to technical field of extraction of Chinese traditional medicine, be specifically related to a kind of preparation method of Radix Berberidis kunmingensis extract.The method comprises the following steps: a, Radix Berberidis wall breaking pulverization, extracts at least twice, each 30-40 minute in boiling water, filters; B, merging filtrate, filtrate simmer down to extractum; C, extract dry obtain crude extract; D, crude extract macroporous resin chromatographic column carry out purification, first use soda lye wash remove impurity during purification, then with ethanol to chromatographic column eluting, collect ethanol elution, ethanol elution concentrate, the Radix Berberidis kunmingensis extract of dry content of berberine hydrochloride >=80%.The extraction and isolation that can realize berberine hydrochloride in Radix Berberidis of the present invention, and technique is simple, and energy consumption is little, and the time is short, implements easily, and low to equipment configratioin requirement, extraction efficiency is high simultaneously, and purity is good.
Description
Technical field
The invention belongs to technical field of extraction of Chinese traditional medicine, be specifically related to a kind of preparation method of Radix Berberidis kunmingensis extract.
Background technology
Radix Berberidis has another name called berberis poiretii, pin passeris montani saturati, copper acupuncture, Radix Berberidis soulieanae, is Berberidaceae, being commonly called as of Berberis class plant, machaka.The extract of Radix Berberidis is with its natural sex, become one of antibiotic succedaneum without advantages such as Drug resistance, multifunctionality and toxic and side effects are less.
The main active of Radix Berberidis kunmingensis extract is berberine, also known as berberine, Chang Zuowei broad ectrum antibiotic uses clinically, in recent years, research find berberine also have many novelty teabag, particularly Cardiological, oncology, organ transplantation aspect research application have new discovery (Song Jun, berberine clinical practice and New research progress, the modern medicine health 24 volume ll phases in 2008,1652-1654).
Consider that berberine has above-mentioned special efficacy in Radix Berberidis, be necessary to carry out extraction and isolation.And the domestic research of the extraction and isolation to Radix Berberidis active substance is less, the main method adopting acid-soluble alkali deposited to saltout is extracted, as follows: to get Radix Berberidis root, section, add 8 times of water gagings, add sulphuric acid adjust ph to 1 ~ 2, flood 2 times, each 24 hours, filter, filtrate merges, by lime cream adjust ph to 12, leave standstill 12 hours, filter, filtrate adds 3 times amount 8% sodium chloride solutions, with salt acid for adjusting pH value to 8 ~ 9, leave standstill 12 hours, filter, get precipitation, dry, obtain semifinished product.Semifinished product is added 15 times of water gagings, be heated to 80 DEG C and be stirred to dissolve, filter, filtrate salt adding acid for adjusting pH value to 1 ~ 2, leave standstill 24 hours, filter, precipitation washes unnecessary hydrochloric acid with water, dry below 80 DEG C, to obtain final product.Someone is by the concentration of Orthogonal Method to extracting solution, the soak extraction time, salinity 4 factors of pH value when saltouing and liquid of saltouing are optimized (Zhao Yongsheng, Hu great Ze, the optimized choice of Radix Berberidis extraction process, China National folk medicine magazine total 64th phase in 2003,299-300), this process cycle is long, generally need 3-4 days, yield is low, and equipment must be acidproof, requires high.
Summary of the invention
The present invention relates to the preparation method of short Radix Berberidis kunmingensis extract of a kind of extraction time.
The present invention is by the following technical solutions:
A preparation method for Radix Berberidis kunmingensis extract, comprises the following steps: a, Radix Berberidis wall breaking pulverization, extracts at least twice, each 30-40 minute in boiling water, filters; B, merging filtrate, filtrate simmer down to extractum; C, extract dry obtain crude extract; D, crude extract macroporous resin chromatographic column carry out purification, first use soda lye wash remove impurity during purification, then with ethanol to chromatographic column eluting, collect ethanol elution, ethanol elution concentrate, the Radix Berberidis kunmingensis extract of dry content of berberine hydrochloride >=80%.
Refining further, the Radix Berberidis kunmingensis extract that steps d obtains also can continue to adopt C18 reverse phase silica gel filler chromatographic column to be further purified, with 85-95%(v/v) ethanol mobile phase eluting, collection eluent, eluent concentrates, the dry Radix Berberidis kunmingensis extract obtaining content of berberine hydrochloride >=95%.
In step a, boiling water consumption is 8-15 times of Radix Berberidis quality.
In steps d, aqueous alkali is the sodium hydroxide solution of concentration 0.5mol/L, and the consumption of aqueous alkali is 10-15 times of chromatographic column packing volume, and ethanol contend concentration is 85-95%.
Filler in steps d in macroporous resin chromatographic column is HP600 macroporous resin.
Super micron mill is adopted during wall breaking pulverization in step a.
The extraction and isolation that can realize berberine hydrochloride in Radix Berberidis of the present invention, and technique is simple, and energy consumption is little, and the time is short, only needs about 24h, implements easily, and low to equipment configratioin requirement, extraction efficiency is high simultaneously, and purity is good.
Detailed description of the invention
Embodiment 1:
A, take 10kg Radix Berberidis decoction pieces, carry out breaking cellular wall by super micron mill and smash; In the purified water of 8 times of quality, steam boils, dynamic agitation, 30 minutes time, crosses 100 eye mesh screens, extracts 2 times;
B, by filtrate merge, vacuum concentration is extractum;
C, extractum spraying dry obtain crude extract;
D, crude extract HP600 macroporous resin chromatographic column carry out purification, first use the sodium hydroxide solution washing impurity-removing of the 0.5mol/L of chromatographic column packing volume 10 times, use 90%(v/v again) ethanol elution, collect ethanol elution, ethanol elution vacuum concentration becomes extractum, extractum spraying dry obtains extract, and wherein the content of berberine hydrochloride reaches 80.9%;
E, polishing purification, carry out reverse phase silica gel chromatographic isolation by said extracted thing, and immobile phase is C18 reverse phase silica gel, elution flow phase 90%(v/v) ethanol, collect eluent, eluent concentrate, dry purity reach 96.1% Radix Berberidis kunmingensis extract.
Embodiment 2:
A, take 10kg Radix Berberidis decoction pieces, carry out breaking cellular wall by super micron mill and smash; In the purified water of 12 times of quality, steam boils, dynamic agitation, 30 minutes time, crosses 100 eye mesh screens, extracts 2 times;
B, by filtrate merge, vacuum concentration is extractum;
C, extractum spraying dry obtain crude extract;
D, crude extract HP600 macroporous resin chromatographic column carry out purification, first use the sodium hydroxide solution washing impurity-removing of the 0.5mol/L of chromatographic column packing volume 12 times, use 95%(v/v again) ethanol elution, collect ethanol elution, ethanol elution vacuum concentration becomes extractum, extractum spraying dry obtains extract, and wherein the content of berberine hydrochloride reaches 81.6%;
E, polishing purification, carry out reverse phase silica gel chromatographic isolation by said extracted thing, and immobile phase is C18 reverse phase silica gel, elution flow phase 95%(v/v) ethanol, collect eluent, eluent concentrate, dry purity reach 97.3% Radix Berberidis kunmingensis extract.
Embodiment 3:
A, take 10kg Radix Berberidis decoction pieces, carry out breaking cellular wall by super micron mill and smash; In the purified water of 15 times of quality, steam boils, dynamic agitation, 30 minutes time, crosses 100 eye mesh screens, extracts 2 times;
B, by filtrate merge, vacuum concentration is extractum;
C, extractum spraying dry obtain crude extract;
D, crude extract HP600 macroporous resin chromatographic column carry out purification, first use the sodium hydroxide solution washing impurity-removing of the 0.5mol/L of chromatographic column packing volume 15 times, use 85%(v/v again) ethanol elution, collect ethanol elution, ethanol elution vacuum concentration becomes extractum, extractum spraying dry obtains extract, and wherein the content of berberine hydrochloride reaches 82.1%;
E, polishing purification, carry out reverse phase silica gel chromatographic isolation by said extracted thing, and immobile phase is C18 reverse phase silica gel, elution flow phase 85%(v/v) ethanol, collect eluent, eluent concentrate, dry purity reach 96.9% Radix Berberidis kunmingensis extract.
Claims (4)
1. a preparation method for Radix Berberidis kunmingensis extract, is characterized in that comprising the following steps: a, Radix Berberidis wall breaking pulverization, extracts at least twice, each 30-40 minute in boiling water, filters; B, merging filtrate, filtrate simmer down to extractum; C, extract dry obtain crude extract; D, crude extract macroporous resin chromatographic column carry out purification, filler in macroporous resin chromatographic column is HP600 macroporous resin, the sodium hydroxide solution washing impurity-removing of concentration 0.5mol/L is first used during purification, the consumption of aqueous alkali is 10-15 times of chromatographic column packing volume, then be that the ethanol of 85-95% is to chromatographic column eluting by volumetric concentration, collection ethanol elution, ethanol elution concentrates, the dry Radix Berberidis kunmingensis extract obtaining content of berberine hydrochloride >=80%.
2. the preparation method of Radix Berberidis kunmingensis extract as claimed in claim 1, it is characterized in that, the Radix Berberidis kunmingensis extract that steps d obtains adopts C18 reverse phase silica gel filler chromatographic column to be further purified, with 85-95% ethanol mobile phase eluting, collection eluent, eluent concentrates, the dry Radix Berberidis kunmingensis extract obtaining content of berberine hydrochloride >=95%.
3. the preparation method of Radix Berberidis kunmingensis extract as claimed in claim 1 or 2, is characterized in that, in step a, boiling water consumption is 8-15 times of Radix Berberidis quality.
4. the preparation method of Radix Berberidis kunmingensis extract as claimed in claim 1 or 2, is characterized in that, adopts super micron mill in step a during wall breaking pulverization.
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Address after: 462000 No. 6 Renmin Middle Road, Zhengzhou, Henan, Xinzheng Applicant after: Suicheng Pharmaceutical Co., Ltd. Address before: 462000 No. 6 Renmin Middle Road, Zhengzhou, Henan, Xinzheng Applicant before: Tianjin Pharmaceutical Group Xinzheng Co., Ltd. |
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| CB03 | Change of inventor or designer information |
Inventor after: He Shengli Inventor after: Cheng Yongke Inventor after: Liu Zhenmin Inventor after: Li Junxia Inventor after: Bai Yanhe Inventor before: He Shengli Inventor before: Cheng Yongke Inventor before: Li Junxia Inventor before: Bai Yanhe |
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Free format text: CORRECT: INVENTOR; FROM: HE SHENGLI CHENG YONGKE LI JUNXIA BAI YANHE TO: HE SHENGLI CHENG YONGKE LIU ZHENMIN LI JUNXIA BAI YANHE Free format text: CORRECT: APPLICANT; FROM: TIANJIN PHARMACEUTICAL GROUP XINZHENG CO., LTD. TO: SUICHENG PHARMACEUTICAL CO., LTD. |
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