CN105784915A - Thin-layer identification method for leonurus japonicus houtt. in Yixuean granules - Google Patents
Thin-layer identification method for leonurus japonicus houtt. in Yixuean granules Download PDFInfo
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- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a thin-layer identification method for leonurus japonicus houtt. in Yixuean granules. Stachydrine hydrochloride is adopted as a reference, and acetone, ethyl acetate and hydrochloric acid are adopted as developers. The method has good separation effects, and is high in reproducibility and easy to operate, leonurus japonicus houtt. can be rapidly and qualitatively analyzed, and effective control over the quality of the Yixuean granules is reliably guaranteed.
Description
Technical field
The present invention relates to drug tests, particularly the thin-layer identification method of Herba Leonuri in her blood peace granule a kind of.
Background technology
Her blood peace granule is a kind of Chinese patent medicine treating gynecologic blood diseases, and Main Ingredients and Appearance is Herba Blumeae Balsamiferae, Herba Leonuri, Rhizoma Corydalis, Radix Glycyrrhizae etc., has the effect such as promoting blood circulation and hemostasis, promoting the circulation of QI to relieve pain.Clinically for postpartum lochiorrhea, after artificial abortion, metrorrhagia is clean, differential diagnosis in tcm belongs to syndrome of blood stasis person.
Her ministerial drug of blood peace granule is Herba Leonuri, for the fresh or dry aerial parts of Labiatae mother wort plant Herba Leonuri [LeonurusjaponicusHoutt.]；Its acrid in the mouth, micro-hardship, cold nature, enter pericardium, Liver Channel, there is effect of promoting blood flow to regulate menstruation, inducing diuresis to remove edema.In Herba Leonuri, main chemical compositions is alkaloids, flavonoid, Diterpenes, phenylpropanol glycoside, fatty acid, volatile oil, ring-like polypeptide etc., and containing various trace elements such as zinc, copper, manganese, ferrum, selenium；Herba Leonuri, containing total alkaloids, wherein mainly has leonurine, stachydrine, Herba Leonuri pyridine and leonurinine etc..
By differentiating to carry out qualitative analysis to the thin layer of stachydrine hydrochloride in " Chinese Pharmacopoeia " version one in 2010, with acetone-dehydrated alcohol-hydrochloric acid for developing solvent, develop the color with rare bismuth potassium iodide test solution-ferric chloride test solution mixed solution.Assay aspect, with the content of stachydrine hydrochloride and hydrochloric acid leonurine in high effective liquid chromatography for measuring Herba Leonuri.Lot of documents shows, differentiates to realize to the many thin layers with stachydrine hydrochloride of qualitative analysis of Herba Leonuri.Assay, based on high performance liquid chromatography, is the content measuring stachydrine hydrochloride mostly.The patent of invention that notification number is CN102937635A discloses the thin-layer identification method of Herba Leonuri in her blood peace granule a kind of, the pre-treating method of her blood peace granule pacifies granule 15g for taking her blood of finished product, add cold dehydrated alcohol 100～300ml, 30min is extracted in jolting, filter, filtrate is evaporated, residue add dehydrated alcohol 2～4ml dissolve, then using volume ratio be the acetone of 6～8:4～6:1, the mixed solution of dehydrated alcohol, concentrated hydrochloric acid as developing solvent launch；The method pacifies, for her blood existing, the problem that granular mass standard is perfect not to the utmost, with acetone, dehydrated alcohol, concentrated hydrochloric acid mixed solution differentiate the Herba Leonuri in her blood peace granule for developing solvent, but in practical operation experiment, owing to stachydrine hydrochloride is unstable, thin layer discrimination test duration of run is longer and expansion effect is undesirable, occur that speckle separates the bad or unconspicuous phenomenon of speckle, and repeatability is undesirable, therefore, the qualitative rapid techniques of Herba Leonuri in a kind of her stable blood peace granule is lacked.
Summary of the invention
The invention provides the thin-layer identification method of Herba Leonuri in her blood peace granule a kind of, fast and accurately the Herba Leonuri in her blood peace granule can be carried out qualitative analysis.
For achieving the above object, the technical scheme is that
The thin-layer identification method of Herba Leonuri in her blood peace granule a kind of, comprises the following steps:
(1) preparation of need testing solution: taking her blood peace granule, add dehydrated alcohol, jolting is extracted, and filters, and the filtrate obtained is evaporated, and residue adds anhydrous alcohol solution, as need testing solution；
(2) reference substance solution: stachydrine hydrochloride reference substance adds dehydrated alcohol and makes reference substance solution；
(3) take above-mentioned need testing solution, reference substance solution, put on same silica gel thin-layer plate, with volume ratio be the acetone of 5～7:5～7:1, ethyl acetate, hydrochloric acid mixed solution for developing solvent launch, take out, dry, spray is to improve bismuth potassium iodide test solution, heating makes spot development clear, and need testing solution chromatograph, on position corresponding with reference substance solution chromatograph, shows the speckle of same color.
Preferably, in described developing solvent, acetone, ethyl acetate, hydrochloric acid volume ratio be 6:6:1.
Preferably, the concrete operation method of described step (1) is: taking her blood peace granule 15g, add dehydrated alcohol 50ml, jolting is extracted 20～60 minutes, filters, and filtrate is evaporated, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.It is furthermore preferred that her blood peace granule described is first ground to 100～300 orders before adding dehydrated alcohol.
Preferably, the time that jolting is extracted is 30 minutes.
Preferably, in described step (2), reference substance solution is made up of every 1ml anhydrous alcohol solution stachydrine hydrochloride 0.1～0.3mg.
Preferably, in described step (3), need testing solution, reference substance solution respectively take 10～20 μ L points on same silica gel thin-layer plate.
Techniques discussed above scheme, the developing solvent that thin-layer identification method is used has carried out emphasis optimization, using acetone, ethyl acetate, hydrochloric acid mixed solution as developing solvent, duration of run is shorter, and speckle separates better, reproduction degree is high, additionally, this method also has advantage accurately simple to operate, qualitative, provides Reliable guarantee for effectively controlling her quality of blood peace granule.
Accompanying drawing explanation
Fig. 1 is the thin-layer chromatogram that embodiment 1 obtains.
Fig. 2 is the chromatogram obtained according to the method in the patent of invention that notification number is CN102937635A.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited to following example: embodiment 1
The preparation of need testing solution: her blood taking three different lot numbers pacifies each 15g of granule, is ground to 100～300 orders, adds dehydrated alcohol 50ml, and jolting is extracted 30 minutes, filters, and filtrate is evaporated, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.
The preparation of reference substance solution: every 1ml anhydrous alcohol solution stachydrine hydrochloride 0.1mg makes.
The preparation of negative control sample solution: her blood lacking Herba Leonuri pacifies granule, is prepared according to the preparation method of need testing solution.
Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VIB of version in 2010), draw above-mentioned need testing solution, each 10 μ L of reference substance solution, put respectively in same with on the silica GF254 lamellae that sodium carboxymethyl cellulose is adhesive, with volume ratio be 6:6:1 acetone, ethyl acetate, hydrochloric acid mixed solution for developing solvent, be placed in the pre-saturated expansion cylinder of developing solvent, launch, take out, drying, spray is to improve bismuth potassium iodide test solution, and it is clear to spot development to heat.Need testing solution chromatograph, on position corresponding with reference substance solution chromatograph, shows the speckle of same color.
This method development rate is fast, only need 20min, and as shown in Figure 1,1,2,3 is her blood peace granule need testing solution of three batches of the present embodiment, 4 is the stachydrine hydrochloride reference substance solution of the present embodiment, and 5 is the negative control sample solution of the present embodiment, this method good separating effect, speckle shows clearly, and method reproduction degree is high.
Embodiment 2
The preparation of need testing solution: taking her blood peace granule 15g, be ground to 100～300 orders, add dehydrated alcohol 50ml, jolting is extracted 30 minutes, filters, and filtrate is evaporated, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.
The preparation of reference substance solution: every 1ml anhydrous alcohol solution stachydrine hydrochloride 0.1mg makes.
Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VIB of version in 2010), draw above-mentioned need testing solution, each 10 μ L of reference substance solution, put respectively in same with on the silica GF254 lamellae that sodium carboxymethyl cellulose is adhesive, with volume ratio be 5:7:1 acetone, ethyl acetate, hydrochloric acid mixed solution for developing solvent, be placed in the pre-saturated expansion cylinder of developing solvent, launch, take out, drying, spray is to improve bismuth potassium iodide test solution, and it is clear to spot development to heat.Need testing solution chromatograph, on position corresponding with reference substance solution chromatograph, shows the speckle of same color.
This method development rate is fast, it is only necessary to 22min, and separating effect is better, and speckle shows clearly, and method reproduction degree is high.
Embodiment 3
The preparation of need testing solution: taking her blood peace granule 15g, be ground to 100～300 orders, add dehydrated alcohol 50ml, jolting is extracted 30 minutes, filters, and filtrate is evaporated, and residue adds dehydrated alcohol 1ml makes dissolving, as need testing solution.
The preparation of reference substance solution: every 1ml anhydrous alcohol solution stachydrine hydrochloride 0.1mg makes.
Test according to thin layer chromatography (Chinese Pharmacopoeia one annex VIB of version in 2010), draw above-mentioned need testing solution, each 10 μ L of reference substance solution, put respectively in same with on the silica GF254 lamellae that sodium carboxymethyl cellulose is adhesive, with volume ratio be 5:7:1 acetone, ethyl acetate, hydrochloric acid mixed solution for developing solvent, be placed in the pre-saturated expansion cylinder of developing solvent, launch, take out, drying, spray is to improve bismuth potassium iodide test solution, and it is clear to spot development to heat.Need testing solution chromatograph, on position corresponding with reference substance solution chromatograph, shows the speckle of same color.
This method development rate is fast, it is only necessary to 25min, and separating effect is better, and speckle shows clearly, and method reproduction degree is high.
Embodiment 4
Notification number is the method in the patent of invention of CN102937635A:
Her blood of finished product taking three different lot numbers pacifies each 15g of granule, adds cold dehydrated alcohol 300ml, and 30min is extracted in jolting, filters, filtrate is evaporated, and residue adds dehydrated alcohol 4ml and dissolves, as need testing solution；
Take stachydrine hydrochloride reference substance appropriate, add dehydrated alcohol and make every 1ml solution containing 0.1mg as reference substance solution；
Her blood taking scarce Herba Leonuri pacifies granule and Herba Leonuri control medicinal material, prepares negative control sample solution and Herba Leonuri control medicinal material solution respectively according to the preparation method of need testing solution.
Thin layer chromatography according to one annex VIB of " Chinese Pharmacopoeia " version in 2010 is tested, draw need testing solution and each 10 μ L of reference substance solution respectively, put respectively on same silica gel g thin-layer plate, with volume ratio be 6:6:1 acetone, dehydrated alcohol, concentrated hydrochloric acid mixed solution for developing solvent launch, take out, dry, spray is to improve bismuth potassium iodide developer, heating makes spot development clear, in test sample chromatograph on position corresponding with reference substance chromatograph, and the speckle of aobvious same color.
This method development rate is slower, need 30min, and as shown in Figure 2,6,7,8 is her blood peace granule need testing solution of three batches of the present embodiment, 9 is the stachydrine hydrochloride reference substance solution of the present embodiment, 10 is the negative control sample solution of the present embodiment, and 11 is Herba Leonuri control medicinal material solution, and method reproduction degree is low.
From the chromatogram of Fig. 1 and Fig. 2 relatively, notification number is that the chromatogram speckle that the method in the patent of invention of CN102937635A obtains is little, and unintelligible, repeatability is bad, launches effect undesirable.The chromatogram that the method for the present invention obtains, favorable reproducibility, clear spot, good separating effect.
Claims (7)
1. the thin-layer identification method of Herba Leonuri in her a blood peace granule, it is characterised in that comprise the following steps:
(1) preparation of need testing solution: taking her blood peace granule, add dehydrated alcohol, jolting is extracted, and filters, and the filtrate obtained is evaporated, and residue adds anhydrous alcohol solution, as need testing solution；
(2) reference substance solution: stachydrine hydrochloride reference substance adds dehydrated alcohol and makes reference substance solution；
(3) take above-mentioned need testing solution, reference substance solution, put on same silica gel thin-layer plate, with volume ratio be the acetone of 5～7:5～7:1, ethyl acetate, hydrochloric acid mixed solution for developing solvent launch, take out, dry, spray is to improve bismuth potassium iodide test solution, heating makes spot development clear, and need testing solution chromatograph, on position corresponding with reference substance solution chromatograph, shows the speckle of same color.
2. the thin-layer identification method of Herba Leonuri in her blood peace granule according to claim 1, it is characterised in that:
In described developing solvent, acetone, ethyl acetate, hydrochloric acid volume ratio be 6:6:1.
3. the thin-layer identification method of Herba Leonuri in her blood peace granule according to claim 1, it is characterised in that:
The concrete operation method of described step (1) is: taking her blood peace granule 15g, add dehydrated alcohol 50ml, jolting is extracted 20～60 minutes, filters, and filtrate is evaporated, and residue adds dehydrated alcohol 1～3ml makes dissolving, as need testing solution.
4. the thin-layer identification method of Herba Leonuri in her blood peace granule according to claim 3, it is characterised in that:
Her blood peace granule described is first ground to 100～300 orders before adding dehydrated alcohol.
5. the thin-layer identification method of Herba Leonuri in her blood peace granule according to claim 3, it is characterised in that:
The time that jolting is extracted is 30 minutes.
6. the thin-layer identification method of Herba Leonuri in her blood peace granule according to claim 1, it is characterised in that:
In described step (2), reference substance solution is made up of every 1ml anhydrous alcohol solution stachydrine hydrochloride 0.1～0.3mg.
7. the thin-layer identification method of Herba Leonuri in her blood peace granule according to claim 1, it is characterised in that:
In described step (3), need testing solution, reference substance solution respectively take 10～20 μ L points on same silica gel thin-layer plate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111024879A (en) * | 2020-01-08 | 2020-04-17 | 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 (4)
| 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 |
| JP2016013991A (en) * | 2014-07-03 | 2016-01-28 | 康力生技股▲分▼有限公司 | Chinese medical herb synthetic for anti-uterine fibroid, and application of extract thereof |
-
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- 2016-05-12 CN CN201610317109.7A patent/CN105784915B/en active Active
Patent Citations (4)
| 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 |
| JP2016013991A (en) * | 2014-07-03 | 2016-01-28 | 康力生技股▲分▼有限公司 | Chinese medical herb synthetic for anti-uterine fibroid, and application of extract thereof |
Non-Patent Citations (3)
| Title |
|---|
| 国家药典委员会: "《中华人民共和国药典 2010年版 一部》", 31 January 2010 * |
| 罗毅等: "肾宁颗粒的薄层色谱鉴别", 《中药新药与临床药理》 * |
| 陆爱武等: "益母草中水苏碱TLC鉴别方法研究", 《实用中西医结合临床》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111024879A (en) * | 2020-01-08 | 2020-04-17 | 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 |
| 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 |
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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 |