CN1321995C - Total coptis alkaloid preparation method - Google Patents
Total coptis alkaloid preparation method Download PDFInfo
- Publication number
- CN1321995C CN1321995C CNB2005100443458A CN200510044345A CN1321995C CN 1321995 C CN1321995 C CN 1321995C CN B2005100443458 A CNB2005100443458 A CN B2005100443458A CN 200510044345 A CN200510044345 A CN 200510044345A CN 1321995 C CN1321995 C CN 1321995C
- Authority
- CN
- China
- Prior art keywords
- rhizoma coptidis
- coptis root
- preparation
- total alkaloids
- alkaloid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The present invention relates to a preparing method of coptis root total alkaloid, which uses novel styrene type macroporous resin to separate coptis root alkaloid. The preparing method has the advantages of simple and rapid technology, high impurity-removing efficiency, and great concentrating technology simplification of coptis root decoction. The preparing method comprises the following steps: weighing a proper quantity of pulverized coptis root medicinal materials to be decocted with water; controlling a flow speed, and adding the supernatant liquid of the decoction onto pretreated resin columns simultaneously; washing the resin columns with water; eluting the resin columns with aqueous ethanol; concentrating the eluent to separate a large amount of alkaloid sediment; drying the alkaloid sediment to obtain the coptis root total alkaloid. HPLC test shows that the content of the coptis root total alkaloid is from 25 to 100%. To the coptis root alkaloid, the resin has the characteristics of large sample-carrying quantity, strong adsorption capacity, easy elution from the resin, reusable utilization, etc. The preparing method is especially suitable for the mass production of medicinal extract products, simple recipes of Chinese medicine and new compound preparations containing coptis root in pharmaceutical factories and enterprises, and is also suitable for the quality testing process of the simple recipes of Chinese medicine and the new compound preparations containing the coptis root.
Description
Technical field
The present invention relates to the extraction and separation method of effective ingredient in Chinese, especially the method for extraction separation efficient part total alkaloids from the Chinese medicine coptis.
Background technology
The coptis (RHIZOMA COPTIDIS) is the dry rhizome that the ranunculaceae plant coptis, Coptis deltoidea C.Y.Cheng et Hsiao or cloud connect, record in one one of 2005 editions Chinese Pharmacopoeia, the effect of tool heat-clearing and damp-drying drug, eliminating fire and detoxication, treat the common drug of quench one's thirst (diabetes) for tcm clinical practice, mainly contain Protoberberine Alkoloids such as Berberine, palmatine, jateorhizine, alkaloids compositions such as coptisine.
Alkaloid is the big class basic nitrogen compound that occurring in nature extensively exists, be many medium-height grass the effective elements of the medicines, often exist under neutrality and the acidic conditions with cationic form, so generally can be with Zeo-karb separation and concentration from extracting solution, as having good antitumous effect gelsemium alkaloids, its cation exchange resin processes extraction process is: get exsiccant RADIX GELSEMII fragment 1g, add 0.3% aqueous sulfuric acid and soak 2d, filter filter residue, soak 1 time, merging filtrate transfers pH to 5.0 back by 0017 strong acid cation exchange resin column with sodium hydroxide again, HCl wash-out alkaloid with 2mol/L, elutriant is with among the NaOH and transfer pH to 11.0, and with chloroform extraction 2 times, concentrated extract is to doing again, total recovery is 1.07%, purity is greater than 96%[Xu Jian, Liang Chongzhen, Acta Pharmaceutica Sinica, 1988,23 (6): 341].Ion exchange resin separating bio alkali applied sample amount is little and step is loaded down with trivial details, and the macroporous resin separation is easy fast, applied sample amount is big, be easy to wash-out and regeneration and adopt, and the application in separating, analyze at middle pharmaceutically active ingredient in recent years increases gradually.Be mainly used in the processing of glycoside, flavones ingredient in the Chinese medicine sample at present, the document that is applied to the alkaloids component separating less (Ma Zhenshan. [J] used in the research of macroporous resin in pharmaceutical field. Chinese patent medicine, 1997,19 (12): 40).Find as yet to adopt styrene type macroporous resin to separate the bibliographical information for preparing Rhizoma Coptidis total alkaloids in a large number, this process using styrene type macroporous resin prepares Rhizoma Coptidis total alkaloids, has solved problems such as coptis decocting liquid is long-pending greatly, concentrated time-consuming, foreign matter content height.
Summary of the invention
When the present invention is directed to medicinal material extract such as the coptis, decocting liquid long-pending big, concentrate problem such as time-consuming, foreign matter content height, adopt styrene type macroporous resin to prepare Rhizoma Coptidis total alkaloids, particular content is as follows:
Take by weighing the medicinal material through suitable pulverizing, with water extraction, decocting liquid filters or centrifugal settling, the control flow velocity adds to decocting liquid supernatant liquor on the good resin column of pre-treatment, and the aqueous ethanol wash-out is used in washing, the aqueous ethanol elutriant concentrated to separate out the large number of biological alkali precipitation, be drying to obtain; The extract total alkaloid content detects through HPLC, is reference substance with berberine hydrochloride, palmatine hydrochloride, Jatrorrhizine chloride and berberine sulfate alkali, Rhizoma Coptidis total alkaloids content 25～100%.
Preferably, medicinal material is the commercially available or fresh medicinal material through the suitable coptis of pulverizing, golden cypress, Radix Berberidis.
Preferably, the coptis medicinal material through suitably pulverizing decocts 2～3 times with 12～24 times of water gagings, and decocting liquid filters or centrifugal settling.
Preferred, macroporous resin that resin column is filled is a styrene type, and its maximal absorptive capacity is 50～300g coptis medicinal material/1000g resin.
Preferred, last sample and cleaning control flow velocity are 2～50mLmin
-1
Preferred, the aqueous ethanol that adopts is 10～50% aqueous ethanols.
Preferred, drying means can adopt oven dry, drying under reduced pressure or other drying means.
The total alkaloids that this method makes detects through HPLC, and with berberine hydrochloride, palmatine hydrochloride, Jatrorrhizine chloride, berberine sulfate alkali is reference substance, Rhizoma Coptidis total alkaloids content 25～100%.
This method also can be used for the alkaloidal a large amount of preparations of Berberine type in the medicinal materials such as golden cypress, Radix Berberidis.
The processing of macroporous resin and renovation process are: soak through aqueous ethanol before macroporous resin uses, can go up sample after the washing; Regeneration of resin can adopt aqueous ethanol to soak behind the wash-out, can enter next circulation after the washing.
The novel macroporous resin of this process using is applied to alkaloidal preparation in the medicinal materials such as the coptis, shorten concentration process greatly, removed impurity, have easy fast, applied sample amount is big, be easy to advantages such as wash-out and regeneration, is suitable for alkaloidal a large amount of preparations in the medicinal material such as the coptis.
Embodiment
Embodiment 1
Take by weighing coptis medicinal material 350g, decoct 2 times with 9,6 times of water gagings respectively through suitable pulverizing, the centrifugal settling of decocting liquid, last sample and cleaning control flow velocity are 2mLmin
-1, supernatant liquor is added on the good DS-401 resin column of pre-treatment (5.1 * 75cm glass column), washing, the aqueous ethanol wash-out with 20% can be separated out the large number of biological alkali precipitation with the aqueous ethanol elutriant is concentrated, and drying under reduced pressure promptly gets 23g.With berberine hydrochloride, palmatine hydrochloride, Jatrorrhizine chloride, berberine sulfate alkali is reference substance, and Rhizoma Coptidis total alkaloids HPLC measurement result sees Table 1, known organism alkali content 40.26% in the extract.
Known composition percentage composition measurement result in table 1 Rhizoma Coptidis total alkaloids
| Sample | Content of berberine hydrochloride (%) | Palmatine hydrochloride content (%) | Hydrochloric acid coptisine content (%) | Jatrorrhizine chloride content (%) | Known composition percentage composition (%) |
| Rhizoma Coptidis total alkaloids 1 | 30.01 | 7.42 | 1.15 | 1.68 | 40.26 |
Embodiment 2
Take by weighing coptis medicinal material 500g, decoct 3 times with 9,6,6 times of water gagings respectively through suitable pulverizing, the centrifugal settling of decocting liquid, last sample and cleaning control flow velocity are 10mLmin
-1, the control flow velocity adds to supernatant liquor on the good DA-201 resin column of pre-treatment (8.0 * 96em glass column), washing, and the aqueous ethanol wash-out with 30% concentrates the aqueous ethanol elutriant and can separate out the large number of biological alkali precipitation, dries and promptly gets 35.421g.The extract total alkaloid content sees Table 2.
Known composition percentage composition measurement result in table 2 Rhizoma Coptidis total alkaloids
| Sample | Content of berberine hydrochloride (%) | Palmatine hydrochloride content (%) | Hydrochloric acid coptisine content (%) | Jatrorrhizine chloride content (%) | Known composition percentage composition (%) |
| Rhizoma Coptidis total alkaloids 2 | 28.29 | 5.71 | 1.08 | 1.69 | 36.77 |
Embodiment 3
Take by weighing the golden cypress medicinal material through suitable pulverizing, decoct 2 times with 9,6 times of water gagings respectively, decocting liquid filters, and last sample and cleaning control flow velocity are 15mLmin
-1, the control flow velocity adds to supernatant liquor on the good resin column that the D-101-I type is housed of pre-treatment (8.0 * 96cm glass column), washing, and the aqueous ethanol wash-out with 30% can be separated out the large number of biological alkali precipitation with the aqueous ethanol elutriant is concentrated, and drying under reduced pressure is promptly.The extract total alkaloid content sees Table 3.
Known composition percentage composition measurement result in table 3 Rhizoma Coptidis total alkaloids
| Sample | Content of berberine hydrochloride (%) | Palmatine hydrochloride content (%) | Hydrochloric acid coptisine content (%) | Jatrorrhizine chloride content (%) | Known composition percentage composition (%) |
| Total alkaloids 3 | 32.11 | 12.60 | - | - | 44.71 |
Embodiment 4
Take by weighing Radix Berberidis medicinal material, decoct 2 times with 9,6 times of water gagings respectively through suitable pulverizing, centrifugal settling, last sample and cleaning control flow velocity are 30mLmin
-1, the control flow velocity adds to supernatant liquor on the good DM-301 resin column of pre-treatment (8.0 * 96cm glass column), washing, and the aqueous ethanol aqueous ethanol wash-out with 410% concentrates the aqueous ethanol elutriant and can separate out the large number of biological alkali precipitation, dries promptly.The extract total alkaloid content sees Table 4.
Known composition percentage composition measurement result in table 4 Rhizoma Coptidis total alkaloids
| Sample | Content of berberine hydrochloride (%) | Palmatine hydrochloride content (%) | Hydrochloric acid coptisine content (%) | Jatrorrhizine chloride content (%) | Known composition percentage composition (%) |
| Total alkaloids 4 | 33.42 | 5.29 | - | 1.04 | 40.75 |
Embodiment 5
The HPLC of Rhizoma Coptidis total alkaloids detects
1. instrument, reagent and medicine:
SHIMADZU high performance liquid chromatograph (LC-10AT pump, LC-10 UV-detector) (Japan), N2000 chromatographic working station (Zhejiang University's intelligent information Graduate School of Engineering).Berberine hydrochloride, palmatine hydrochloride, Jatrorrhizine chloride are all identified institute available from Chinese pharmaceutical biological product, and berberine sulfate alkali provides (purity＞99%) by doctor Zhou Honglei.
2. chromatographic condition
Chromatographic column: Kromasil C
18(250mm * 4.6mm, 5 μ m); Moving phase: acetonitrile-water (48: 52, every 1L phosphoric acid potassium dihydrogen 3.4g, sodium lauryl sulphate 1.7g); Flow velocity is 1.0mLmin
-1The detection wavelength is 345nm, sample size 20 μ l.
3. sample determination
Get 0.645mgmL respectively
-1Berberine hydrochloride solution 0.5mL, 0.285mgmL
-1Palmatine Hydrochloride solution 1mL, 0.125mgmL
-1Berberine sulfate alkali 2mL, 0.502mgmL
-1Jateorhizine solution 0.5mL in the 10mL volumetric flask, methanol constant volume is as mixing reference substance solution.Precision takes by weighing the Rhizoma Coptidis total alkaloids 10.0mg that makes, and dissolve with methanol also is settled to 100mL, as need testing solution.Filtering with microporous membrane, sample introduction is measured under above-mentioned chromatographic condition, and one point external standard method calculates content.
Claims (8)
1, a kind of preparation method of Rhizoma Coptidis total alkaloids, it is characterized in that: take by weighing medicinal material through suitable pulverizing, with water extraction, decocting liquid filters or centrifugal settling, the control flow velocity adds to decocting liquid supernatant liquor on the good macroporous adsorptive resins of pre-treatment, and the aqueous ethanol wash-out is used in washing, the aqueous ethanol elutriant concentrated to separate out the large number of biological alkali precipitation, be drying to obtain; The extract total alkaloid content detects through HPLC, is reference substance with berberine hydrochloride, palmatine hydrochloride, Jatrorrhizine chloride and berberine sulfate alkali, Rhizoma Coptidis total alkaloids content 25～100%.
2, according to the preparation method of claims 1 described Rhizoma Coptidis total alkaloids, it is characterized in that; Medicinal material is the commercially available or fresh medicinal material through the coptis of suitably pulverizing, golden cypress, Radix Berberidis.
3, according to the preparation method of claims 1 described Rhizoma Coptidis total alkaloids, it is characterized in that: the coptis medicinal material through suitably pulverizing, boil 2～3 times with decocting, decocting liquid filters or centrifugal settling.
4, according to the preparation method of claims 1 described Rhizoma Coptidis total alkaloids, it is characterized in that: macroporous adsorbent resin that macroporous adsorptive resins is filled is a styrene type, and its maximal absorptive capacity is 50～300g coptis medicinal material/1000g resin.
5, according to the preparation method of claims 1 described Rhizoma Coptidis total alkaloids, it is characterized in that: going up sample and cleaning control flow velocity is 2～50mLmin
-1
6, according to the preparation method of claims 1 described Rhizoma Coptidis total alkaloids, it is characterized in that: the aqueous ethanol that adopts is 10～50% aqueous ethanols.
7, according to the preparation method of claims 1 described Rhizoma Coptidis total alkaloids, it is characterized in that: drying means can adopt oven dry, drying under reduced pressure or other drying means.
8, according to the preparation method of claims 2 described Rhizoma Coptidis total alkaloidss, it is characterized in that: this method also can be used for the alkaloidal a large amount of preparations of Berberine type in the medicinal materials such as golden cypress, Radix Berberidis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100443458A CN1321995C (en) | 2005-08-02 | 2005-08-02 | Total coptis alkaloid preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100443458A CN1321995C (en) | 2005-08-02 | 2005-08-02 | Total coptis alkaloid preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1730480A CN1730480A (en) | 2006-02-08 |
| CN1321995C true CN1321995C (en) | 2007-06-20 |
Family
ID=35962905
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100443458A Expired - Fee Related CN1321995C (en) | 2005-08-02 | 2005-08-02 | Total coptis alkaloid preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1321995C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101874834A (en) * | 2009-04-30 | 2010-11-03 | 成都中医药大学 | New application of processed products of Chinese goldthread stir-fried with rice vinegar |
| CN103446214B (en) * | 2013-08-20 | 2015-08-05 | 遂成药业股份有限公司 | A kind of preparation method of Radix Berberidis kunmingensis extract |
| CN104887793B (en) * | 2015-05-15 | 2018-06-26 | 宁玉梅 | A kind of coptis chinensis total alkaloid vaginal plug |
| CN104922235B (en) * | 2015-05-15 | 2018-05-04 | 浙江中医药大学 | A kind of coptis chinensis total alkaloid vaginal gel |
| CN108593634A (en) * | 2018-05-09 | 2018-09-28 | 江西德上制药股份有限公司 | The detection method of alkaloid in Chinese medicinal ingredients |
| CN109999074A (en) * | 2019-04-16 | 2019-07-12 | 信阳农林学院 | The preparation method and its usage of Chinese mahonia total alkaloid extract |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450074A (en) * | 2002-04-05 | 2003-10-22 | 北京康思瞄医药技术开发有限公司 | Process for extracting coptis total alkaloid and new use thereof |
-
2005
- 2005-08-02 CN CNB2005100443458A patent/CN1321995C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450074A (en) * | 2002-04-05 | 2003-10-22 | 北京康思瞄医药技术开发有限公司 | Process for extracting coptis total alkaloid and new use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1730480A (en) | 2006-02-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1321995C (en) | Total coptis alkaloid preparation method | |
| CN105111255A (en) | Extraction and separation method for echinacoside and verbascoside in cistanche | |
| CN104415573B (en) | Method for classifying and preparing tertiary amine alkaloid and quaternary ammonium alkaloid from corydalis extract | |
| CN101028388B (en) | Quality inspection of Chinese-medicinal preparation for treating shortsighness and asthenopia | |
| CN101647828B (en) | Method for separating total alkaloid from sophora flavescens ait by using ion exchange resin | |
| CN102579612A (en) | Method for extracting total alkaloid of aconitum soongaricum | |
| CN107383144A (en) | A kind of extraction for preparing Panaxsaponin composition and conversion coupling technique | |
| CN102423329A (en) | Decolorization method of panax notoginsenoside extract | |
| CN106290599B (en) | Content determination method of traditional Chinese medicine composition | |
| CN106995425A (en) | The extraction process and its isolation and purification method of a kind of Rhizoma Belamcandae flavone aglycone | |
| CN102631414A (en) | SepHaniadelavayi Diels total alkaloid extraction and purification technology | |
| CN103592391B (en) | The content assaying method of Specnuezhenide in Zhenqi Fuzheng prepn | |
| CN104829474B (en) | Method for preparing glycine betaine chemical reference substances from boxthorn leaves | |
| CN104725450A (en) | Method for extracting high-purity oleuropein from jasminum grandiflorum | |
| CN102998375B (en) | A kind of method simultaneously detecting forulic acid and paeoniflorin content in blood-nourishing and brain-refreshing granules | |
| CN103323558A (en) | Ginkgo biloba preparation analysis sample rapid preparation method based on solid phase extraction technology | |
| CN104610401A (en) | Method for simultaneously extracting baicalin, baicalein and wogonin from scutellaria baicalensis | |
| CN102372750A (en) | Method for simultaneously preparing albiflorin and paeoniflorin | |
| CN101658598B (en) | Method for extracting and enriching alisma total triterpenic ketone alcohol components from alisma | |
| CN108519450B (en) | Rhizoma corydalis reference extract and preparation method and application thereof | |
| CN103083392B (en) | A kind of method at tool isoamylene radical chromocor position in separation and concentration Radix Sophorae Tonkinensis | |
| CN109776515A (en) | The method of mangiferin is extracted from myrica rubra leaf | |
| CN111001189A (en) | Method for capturing and separating effective components in liquorice by using mixed-mode agarose gel medium | |
| CN101210039B (en) | Method for separating and preparing madecassoside chemical reference substance | |
| CN101703669A (en) | Smilax china effective fractions and extraction as well as purification process thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C57 | Notification of unclear or unknown address | ||
| DD01 | Delivery of document by public notice |
Addressee: Wei Yingqin Document name: Written notice of preliminary examination of application for patent for invention |
|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| DD01 | Delivery of document by public notice |
Addressee: Wei Yingqin Document name: Notification of Termination of Patent Right |
|
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070620 Termination date: 20100802 |