CN105784915B - The thin-layer identification method of motherwort in her blood peace particle - Google Patents
The thin-layer identification method of motherwort in her blood peace particle Download PDFInfo
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- CN105784915B CN105784915B CN201610317109.7A CN201610317109A CN105784915B CN 105784915 B CN105784915 B CN 105784915B CN 201610317109 A CN201610317109 A CN 201610317109A CN 105784915 B CN105784915 B CN 105784915B
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention discloses a kind of thin-layer identification method of motherwort in her blood peace particle, using stachydrine hydrochloride as control, using acetone, ethyl acetate, hydrochloric acid as solvent, this method good separating effect, reproduction degree is high, and it is simple to operate, quick qualitative analysis can be carried out to motherwort, effectively to control her the quality of blood peace particle to provide Reliable guarantee.
Description
Technical field
The present invention relates to drug tests, her particularly a kind of blood pacifies the thin-layer identification method of motherwort in particle.
Background technology
Her blood peace particle is a kind of Chinese patent drug for treating gynecologic blood diseases, and Main Ingredients and Appearance is blumea riparia, motherwort, prolonged recklessly
Rope, radix glycyrrhizae etc., the effects such as with promoting blood circulation and hemostasis, promoting qi circulation and relieving pain.Clinically it is used for post partum lochiorrhea, uterus goes out after induced abortion
Blood is not net, differential diagnosis in tcm belongs to syndrome of blood stasis person.
Her ministerial drug of blood peace particle is motherwort, is Labiatae mother wort plant motherwort [Leonurus
Japonicus Houtt.] fresh or dry aerial parts；Its pungent, slight bitter, cold nature enters pericardium, Liver Channel, with promoting blood circulation
The effect of menstruation regulating, inducing diuresis to remove edema.In motherwort main chemical compositions be alkaloids, flavonoids, Diterpenes, phenylpropyl alcohol alcohol glycoside,
Fatty acid, volatile oil, ring-like polypeptide etc., and contain the various trace elements such as zinc, copper, manganese, iron, selenium；Motherwort is containing total raw
Alkaloids, wherein mainly having leonurine, stachydrine, motherwort pyridine and leonurinine etc..
《Chinese Pharmacopoeia》Differentiate to carry out qualitative analysis by the thin layer to stachydrine hydrochloride in version one in 2010, with third
Ketone-absolute ethyl alcohol-hydrochloric acid is solvent, is developed the color with dilute bismuth potassium iodide test solution-ferric trichloride test solution mixed solution.Containing measurement
Fixed aspect, with the content of stachydrine hydrochloride and hydrochloric acid leonurine in high effective liquid chromatography for measuring motherwort.Lot of documents table
It is bright, realized to being differentiated with the thin layer of stachydrine hydrochloride more than the qualitative analysis of motherwort.Assay is with high performance liquid chromatography
Based on, it is the content for determining stachydrine hydrochloride mostly.Notification number discloses her a kind of blood for CN102937635A patent of invention
Pacify the thin-layer identification method of motherwort in particle, the pre-treating method of her blood peace particle is to take her blood of finished product to pacify particle 15g, plus cold
30min is extracted in 100~300ml of absolute ethyl alcohol, shaking, and filtrate is evaporated by filtration, and residue adds 2~4ml of absolute ethyl alcohol to dissolve, so
Afterwards using volume ratio as 6~8:4~6:1 acetone, absolute ethyl alcohol, the mixed solution of concentrated hydrochloric acid deploy as solvent；This method
The problem of being improved not to the utmost for her existing blood peace granular mass standard, using the mixed solution of acetone, absolute ethyl alcohol, concentrated hydrochloric acid to open up
Agent is opened to differentiate the motherwort in her blood peace particle, but in practical operation experiment, because stachydrine hydrochloride is unstable, thin layer mirror
Not Shi Yan duration of run it is longer and expansion effect is undesirable, there is the spot separation unconspicuous phenomenon of bad or spot, and again
Renaturation is undesirable, therefore, lacks the qualitative rapid techniques of motherwort in a kind of her blood peace particle of stabilization.
The content of the invention
, can be fast and accurately to her blood the invention provides a kind of thin-layer identification method of motherwort in her blood peace particle
The motherwort pacified in particle carries out qualitative analysis.
To achieve the above object, the technical scheme is that：
The thin-layer identification method of motherwort, comprises the following steps in her a kind of blood peace particle：
(1) preparation of need testing solution：Her blood peace particle, plus absolute ethyl alcohol are taken, shaking is extracted, filtration, the filter obtained
Liquid is evaporated, and residue adds absolute ethyl alcohol dissolving, is used as need testing solution；
(2) reference substance solution：Stachydrine hydrochloride reference substance adds absolute ethyl alcohol that reference substance solution is made；
(3) above-mentioned need testing solution, reference substance solution are taken, is put on same silica gel thin-layer plate, using volume ratio as 5~7:5
~7:1 acetone, ethyl acetate, hydrochloric acid mixed solution are solvent expansion, take out, dry, and are sprayed to improve bismuth potassium iodide test solution,
Heating makes spot development clear, and need testing solution chromatogram shows same color on position corresponding with reference substance solution chromatogram
Spot.
It is preferred that, in the solvent, acetone, ethyl acetate, the volume ratio of hydrochloric acid are 6:6:1.
It is preferred that, the concrete operation method of the step (1) is：Her blood peace particle 15g is taken, absolute ethyl alcohol 50ml is added,
Shaking is extracted 20~60 minutes, and filtration, filtrate is evaporated, and residue adds absolute ethyl alcohol 1ml to make dissolving, is used as need testing solution.It is more excellent
Choosing, her the blood peace particle is first ground to 100~300 mesh before absolute ethyl alcohol is added.
It is preferred that, the time that shaking is extracted is 30 minutes.
It is preferred that, in the step (2), reference substance solution be by every 1ml absolute ethyl alcohols dissolving stachydrine hydrochloride 0.1~
0.3mg is made.
It is preferred that, in the step (3), need testing solution, reference substance solution respectively take 10~20 μ L points thin in same silica gel
On laminate.
Techniques discussed above scheme, the solvent used thin-layer identification method has carried out emphasis optimization, with acetone, second
Acetoacetic ester, hydrochloric acid mixed solution are as solvent, and duration of run is shorter, and spot separation is preferable, and reproduction degree is high, in addition, our
Method also has simple to operate, qualitative accurate advantage, effectively to control her the quality of blood peace particle to provide Reliable guarantee.
Brief description of the drawings
Fig. 1 is the thin-layer chromatogram that embodiment 1 is obtained.
Fig. 2 is the chromatogram obtained according to notification number for the method in CN102937635A patent of invention.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited to following reality
Apply example：Embodiment 1
The preparation of need testing solution：Take her blood of three different lot numbers to pacify each 15g of particle, be ground to 100~300 mesh, plus
Enter absolute ethyl alcohol 50ml, shaking is extracted 30 minutes, and filtration, filtrate is evaporated, and residue adds absolute ethyl alcohol 1ml to make dissolving, as trying
Product solution.
The preparation of reference substance solution：It is made per 1ml absolute ethyl alcohols dissolving stachydrine hydrochloride 0.1mg.
The preparation of negative control sample solution：Her blood for lacking motherwort pacifies particle, according to the preparation method of need testing solution
Prepared.
According to thin-layered chromatography (one annex VI B of Chinese Pharmacopoeia version in 2010) experiment, above-mentioned need testing solution is drawn, right
According to each 10 μ L of product solution, put respectively on the same silica GF254 lamellae using sodium carboxymethylcellulose as binder, with volume
Than for 6:6:1 acetone, ethyl acetate, hydrochloric acid mixed solution are solvent, are placed in the pre-saturated expansion cylinder of solvent, are opened up
Open, take out, dry, spray to improve bismuth potassium iodide test solution, be heated to spot development clear.Need testing solution chromatogram with reference substance
On the corresponding position of solution chromatogram, show the spot of same color.
This method development rate is fast, it is only necessary to 20min, and as shown in figure 1,1,2,3 be she of three batches of the present embodiment
Blood pacifies particle need testing solution, and 4 be the stachydrine hydrochloride reference substance solution of the present embodiment, and 5 be the negative control sample of the present embodiment
Product solution, this method good separating effect, spot shows that clearly method reproduction degree is high.
Embodiment 2
The preparation of need testing solution：Her blood peace particle 15g is taken, 100~300 mesh is ground to, adds absolute ethyl alcohol 50ml, shake
Extraction 30 minutes is shaken, filtration, filtrate is evaporated, and residue adds absolute ethyl alcohol 1ml to make dissolving, is used as need testing solution.
The preparation of reference substance solution：It is made per 1ml absolute ethyl alcohols dissolving stachydrine hydrochloride 0.1mg.
According to thin-layered chromatography (one annex VI B of Chinese Pharmacopoeia version in 2010) experiment, above-mentioned need testing solution is drawn, right
According to each 10 μ L of product solution, put respectively on the same silica GF254 lamellae using sodium carboxymethylcellulose as binder, with volume
Than for 5:7:1 acetone, ethyl acetate, hydrochloric acid mixed solution are solvent, are placed in the pre-saturated expansion cylinder of solvent, are opened up
Open, take out, dry, spray to improve bismuth potassium iodide test solution, be heated to spot development clear.Need testing solution chromatogram with reference substance
On the corresponding position of solution chromatogram, show the spot of same color.
This method development rate is fast, it is only necessary to 22min, and separating effect is preferably, and spot is shown clearly, and method reproduction degree is high.
Embodiment 3
The preparation of need testing solution：Her blood peace particle 15g is taken, 100~300 mesh is ground to, adds absolute ethyl alcohol 50ml, shake
Extraction 30 minutes is shaken, filtration, filtrate is evaporated, and residue adds absolute ethyl alcohol 1ml to make dissolving, is used as need testing solution.
The preparation of reference substance solution：It is made per 1ml absolute ethyl alcohols dissolving stachydrine hydrochloride 0.1mg.
According to thin-layered chromatography (one annex VI B of Chinese Pharmacopoeia version in 2010) experiment, above-mentioned need testing solution is drawn, right
According to each 10 μ L of product solution, put respectively on the same silica GF254 lamellae using sodium carboxymethylcellulose as binder, with volume
Than for 5:7:1 acetone, ethyl acetate, hydrochloric acid mixed solution are solvent, are placed in the pre-saturated expansion cylinder of solvent, are opened up
Open, take out, dry, spray to improve bismuth potassium iodide test solution, be heated to spot development clear.Need testing solution chromatogram with reference substance
On the corresponding position of solution chromatogram, show the spot of same color.
This method development rate is fast, it is only necessary to 25min, and separating effect is preferably, and spot is shown clearly, and method reproduction degree is high.
Embodiment 4
Notification number is the method in CN102937635A patent of invention：
Her blood of the finished product of three different lot numbers is taken to pacify each 15g of particle, plus cold absolute ethyl alcohol 300ml, 30min is extracted in shaking,
Filtration, filtrate is evaporated, and residue adds absolute ethyl alcohol 4ml to dissolve, and is used as need testing solution；
Take stachydrine hydrochloride reference substance appropriate, plus that solution of every 1ml containing 0.1mg is made is molten as reference substance for absolute ethyl alcohol
Liquid；
Her blood of scarce motherwort is taken to pacify particle and motherwort control medicinal material, it is accurate respectively according to the preparation method of need testing solution
Standby negative control sample solution and motherwort control medicinal material solution.
According to《Chinese Pharmacopoeia》The one annex VIB of version in 2010 thin-layered chromatography experiment, respectively draw need testing solution and
Each 10 μ L of reference substance solution, put on same silica gel g thin-layer plate, using volume ratio as 6 respectively:6:It is 1 acetone, absolute ethyl alcohol, dense
The mixed solution of hydrochloric acid deploys for solvent, takes out, dries, and spray is to improve bismuth potassium iodide developer, and heating makes spot development clear
It is clear, in test sample chromatogram on position corresponding with reference substance chromatogram, show the spot of same color.
This method development rate is slower, needs 30min, and as shown in Fig. 26,7,8 be she of three batches of the present embodiment
Blood pacifies particle need testing solution, and 9 be the stachydrine hydrochloride reference substance solution of the present embodiment, and 10 be the negative control sample of the present embodiment
Product solution, 11 be motherwort control medicinal material solution, and method reproduction degree is low.
From Fig. 1 and Fig. 2 chromatogram relatively, notification number for CN102937635A patent of invention in method obtain
Chromatogram spot it is small, unintelligible, reappearance is bad, expansion effect it is undesirable.The chromatogram that the method for the present invention is obtained, reappears
Property good, clear spot, good separating effect.
Claims (6)
1. the thin-layer identification method of motherwort in her a kind of blood peace particle, it is characterised in that comprise the following steps：
（1）The preparation of need testing solution：Her blood peace particle, plus absolute ethyl alcohol are taken, shaking is extracted, and filtration, the filtrate obtained is steamed
Dry, residue adds absolute ethyl alcohol dissolving, is used as need testing solution；
（2）Reference substance solution：Stachydrine hydrochloride reference substance adds absolute ethyl alcohol that reference substance solution is made；
（3）Above-mentioned need testing solution, reference substance solution point are taken on same silica gel thin-layer plate, using volume ratio as 6:6:1 acetone,
Ethyl acetate, hydrochloric acid mixed solution deploy for solvent, take out, dry, and spray is to improve bismuth potassium iodide test solution, and heating shows spot
Color is clear, and need testing solution chromatogram shows the spot of same color on position corresponding with reference substance solution chromatogram.
2. the thin-layer identification method of motherwort in her blood peace particle according to claim 1, it is characterised in that：
The step（1）Concrete operation method be：Her blood peace particle 15g is taken, absolute ethyl alcohol 50ml is added, shaking extracts 20 ~
60 minutes, filtration, filtrate was evaporated, and residue adds 1 ~ 3ml of absolute ethyl alcohol to make dissolving, is used as need testing solution.
3. the thin-layer identification method of motherwort in her blood peace particle according to claim 2, it is characterised in that：
Her the blood peace particle is first ground to 100 ~ 300 mesh before absolute ethyl alcohol is added.
4. the thin-layer identification method of motherwort in her blood peace particle according to claim 2, it is characterised in that：
The time that shaking is extracted is 30 minutes.
5. the thin-layer identification method of motherwort in her blood peace particle according to claim 1, it is characterised in that：
The step（2）In, reference substance solution is made up of every 1ml absolute ethyl alcohols dissolving 0.1 ~ 0.3mg of stachydrine hydrochloride.
6. the thin-layer identification method of motherwort in her blood peace particle according to claim 1, it is characterised in that：
The step（3）In, need testing solution, reference substance solution respectively take 10 ~ 20 μ L points on same silica gel thin-layer plate.
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| CN111024879B (en) * | 2020-01-08 | 2021-08-31 | 河北中医学院 | Rapid multi-information thin-layer identification method for fresh motherwort herb freeze-dried powder, particles and standard decoction dry powder |
Citations (3)
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| CN101306081A (en) * | 2008-06-26 | 2008-11-19 | 广州奇星药业有限公司 | Xinshuning tablets quality control method |
| CN102539588A (en) * | 2011-11-11 | 2012-07-04 | 云南良方制药有限公司 | Method for preparing test solution for quality detection of safe stagnation removing preparation |
| CN102937635A (en) * | 2012-11-27 | 2013-02-20 | 广西万寿堂药业有限公司 | Thin-layer identification method of leonurus in Yi Xue An particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP6034834B2 (en) * | 2014-07-03 | 2016-11-30 | 康力生技股▲分▼有限公司 | Kampo herbal composition for anti-uterine myoma and method for producing anti-uterine fibroid drug produced by herbal herbal extract |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306081A (en) * | 2008-06-26 | 2008-11-19 | 广州奇星药业有限公司 | Xinshuning tablets quality control method |
| CN102539588A (en) * | 2011-11-11 | 2012-07-04 | 云南良方制药有限公司 | Method for preparing test solution for quality detection of safe stagnation removing preparation |
| CN102937635A (en) * | 2012-11-27 | 2013-02-20 | 广西万寿堂药业有限公司 | Thin-layer identification method of leonurus in Yi Xue An particles |
Non-Patent Citations (2)
| Title |
|---|
| 益母草中水苏碱TLC鉴别方法研究;陆爱武等;《实用中西医结合临床》;20020831;第2卷(第4期);第54～55页 * |
| 肾宁颗粒的薄层色谱鉴别;罗毅等;《中药新药与临床药理》;20050228;第16卷(第2期);第135～136页 * |
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Denomination of invention: Thin-layer identification method of leonurus in Yi Xue An particles Effective date of registration: 20190428 Granted publication date: 20170929 Pledgee: Bank of Communications Ltd the Guangxi Zhuang Autonomous Region branch Pledgor: Guangxi Medictop Pharmaceutical Co., Ltd. Registration number: 2019450000016 |
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Date of cancellation: 20210604 Granted publication date: 20170929 Pledgee: Bank of Communications Ltd. the Guangxi Zhuang Autonomous Region branch Pledgor: GUANGXI MEDICTOP PHARMACEUTICAL Co.,Ltd. Registration number: 2019450000016 |