CN107860859B - Method for determining ten-ingredient Daoxiangwan as Tibetan medicine - Google Patents
Method for determining ten-ingredient Daoxiangwan as Tibetan medicine Download PDFInfo
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Abstract
The invention relates to a method for determining ten-ingredient milk flavor pills of a Tibetan medicine, which adopts a thin-layer chromatography to detect the pachaga in the ten-ingredient milk flavor pills and specifically comprises the following steps: grinding the drug to be detected, sieving, wetting, ultrasonic treating, filtering, dissolving, extracting, concentrating to dry, dissolving to obtain a test solution, preparing a control solution by the same preparation method as the test solution from a pachaga control drug, respectively dropping the two solutions on the same silica gel G thin layer plate, developing by using toluene-ethyl acetate-petroleum ether-diethylamine as a developing agent, taking out, drying in the air, spraying an improved bismuth potassium iodide solution, and blowing to the spot to develop the color clearly. The method fills the blank of detecting the Tibetan medicine Shiwei Ruxiang pill by using the pacha as a detection object, and the developing agent used by the method has the advantages of good reproducibility and stability, clear spot color development, good separation degree and the like.
Description
Technical Field
The invention relates to a detection method of a pharmaceutical composition preparation, in particular to a determination method of a Tibetan medicine Shiwei Ruxiang pill.
Background
Baxia ga, also known as ouxia ga, Dana Dong Chi, Dona Chi, etc., is one of the commonly used Tibetan herbs. Because the explanation of the Tibetan medicine sources is inconsistent in different Tibetan areas, the phenomenon of one medicine and multiple medicines is serious. The sources of the pachaga are mainly plants of the vasica, the veronica and the corydalis, and although the plants are different in species and form, the plants are widely used because the plants have curative effect in the clinical use process of Tibetan medicine.
The pachaga is mainly used for protecting liver, promoting urination, reducing blood pressure, removing sore and promoting growth, and has good pharmacological activity. Modern researches show that the Veronica plant has good antioxidant, antiinflammatory, antibacterial and anticancer activities, and in vitro blood coagulation and cough relieving effects. The pachaga contains various chemical components, such as iridoids, phenethyl alcohol, flavonoids, organic acids and the like, and known components mainly comprise aucubin, catalpol, protocatechuic acid, ferulic acid and the like.
The ten-ingredient milk fragrance pills are Tibetan medicines and are collected in a Tibetan medicine booklet of drug Standard of Ministry of health of the people's republic of China, and the standard number is WS 3-BC-0211-95; the prescription comprises 100g of frankincense, 150g of myrobalan, 80g of cassia seed, 100g of fructus terminaliae billericae, 80g of radix malvae, 120g of emblic leafflower fruit, 85g of costustoot, 100g of tinospora sinensis, 80g of pachaga and 50g of zhanjian ointment, and is mainly used for treating red swelling pain and eczema of limbs and joints caused by 'dry yellow water'. According to the prescription of the ten-flavor milk flavor pills, the pachaga is a medicinal material which plays a main medicinal effect in the ten-flavor milk flavor pills, and in order to better monitor the quality of the ten-flavor milk flavor pills, the pachaga in the ten-flavor milk flavor pills needs to be detected.
However, in the prior art, as disclosed in chinese publication No. CN102520110A entitled "method for detecting shiwei boswellia preparation", a method for detecting shiwei boswellia preparation by thin layer chromatography is disclosed, but the detection objects are limited to boswellia, aucklandia root and cassia seed in the preparation, and there is no reference to the detection of pachaga therein. And the applicant does not find the existing technology for detecting the pacha in the ten-flavor frankincense pill by using thin-layer chromatography.
Disclosure of Invention
Therefore, the invention aims to provide a method for detecting the pachaga in the ten-flavor frankincense balls by using a thin-layer chromatography, so as to realize the monitoring of the quality of the ten-flavor frankincense balls.
Aiming at the purposes, the technical scheme of the invention is as follows:
the invention provides a method for determining ten-ingredient Dacron pills of a Tibetan medicine, which is characterized by comprising the following steps: the method detects pachaga by thin layer chromatography.
The method specifically comprises the steps of taking 2-3G of a drug to be detected, grinding the drug to be detected, sieving the drug with a 100-mesh sieve, adding 2-3 m of ammonia water to L, wetting the drug with methanol, carrying out ultrasonic treatment, filtering, volatilizing the methanol from filtrate, dissolving the filtrate with an acetic acid solution, extracting the dissolved solution with butyl acetate, concentrating the solution to dryness, dissolving the solution with ethanol to 1m L to serve as a test solution, taking 1mg of a pachaga control drug, preparing a pachaga control drug solution by using the same preparation method as the test solution, sucking the two solutions with the diameter of 20-30 mu L respectively, dropping the two solutions on the same silica gel G thin layer plate, taking toluene-ethyl acetate-petroleum ether-diethylamine as a developing agent, developing, taking out, airing, spraying an improved potassium iodide solution, and inspecting the spots with the same color in a sample chromatogram at positions corresponding to the chromatogram of the control drug chromatogram.
Preferably, the mass percentage concentration of the acetic acid solution is 5-7%.
Preferably, the volume ratio of toluene to ethyl acetate to petroleum ether to diethylamine in the developing agent is: 3-8: 0.2-4: 5-10: 1-2.
Preferably, the volume ratio of toluene to ethyl acetate to petroleum ether to diethylamine in the developing agent is: 5:1.5:6.5: 1.2.
Compared with the prior art, the determination method has the advantages that:
the invention carries out thin-layer chromatography detection research on the pachaga in the prescription of the Tibetan medicine ten-flavor milk flavor pills, and a method for monitoring the ten-flavor milk flavor pills by taking the pachaga as a detection object does not exist in the prior art, so that the invention fills the gap of monitoring the Tibetan medicine ten-flavor milk flavor pills by taking the pachaga as the detection object. The invention adopts toluene-ethyl acetate-petroleum ether-diethylamine as developing solvent, and has the advantages of good reproducibility and stability, clear spot color development, good separation degree and the like.
Detailed Description
Example 1:
taking 2G of a drug to be detected, grinding the drug to be detected, sieving the drug to be detected by a 100-mesh sieve, adding 2m L of ammonia water, carrying out ultrasonic treatment by using methanol, filtering the drug, volatilizing the methanol from filtrate, dissolving the methanol in an acetic acid solution with the mass percentage concentration of 5%, extracting the dissolved solution by using butyl acetate, concentrating the solution to be dried, dissolving the solution in ethanol to 1m L of the solution to be used as a test solution, taking 1mg of a pachaga control drug, preparing a pachaga control drug solution by using the same preparation method as the test solution, sucking the two solutions with the volume of 20 mu L respectively on the same silica gel G thin layer plate, taking toluene-ethyl acetate-petroleum ether-diethylamine (the volume ratio is 5:1.5:6.5: 1.2) as a developing agent, developing, taking out, airing the solution, spraying the modified bismuth potassium iodide solution, inspecting the solution, and displaying spots with the same color on the positions corresponding to the control drug in a sample chromatogram.
Example 2:
taking 2G of a drug to be detected, grinding the drug to be detected, sieving the drug to be detected by a 100-mesh sieve, adding 2.5m L of ammonia water, carrying out ultrasonic treatment by using methanol, filtering the drug, volatilizing the methanol from filtrate, dissolving the methanol in an acetic acid solution with the mass percentage concentration of 6%, extracting the dissolved solution by using butyl acetate, concentrating the solution to be dry, dissolving the solution in ethanol to be 1m L to be used as a test solution, taking 1mg of a pachaga control drug, preparing a pachaga control drug solution by using the same preparation method as the test solution, sucking the two solutions with the volume of 20 mu L respectively, dropping the two solutions on the same silica gel G thin-layer plate, taking toluene-ethyl acetate-petroleum ether-diethylamine (the volume ratio is 3: 1: 6: 1) as a developing agent, taking out the solution, airing the solution, spraying the improved bismuth potassium iodide solution, and inspecting spots with the same color in positions corresponding to the control drug chromatogram.
Example 3:
taking 3G of a drug to be detected, grinding, sieving by a 100-mesh sieve, adding 3m L of ammonia water, carrying out ultrasonic treatment by using methanol, filtering, volatilizing the methanol from filtrate, dissolving the filtrate by using an acetic acid solution with the mass percentage concentration of 7%, extracting the dissolved solution by using butyl acetate, concentrating the solution to be dry, dissolving the solution by using ethanol to 1m L to serve as a test solution, taking 1mg of a pachaga control drug, preparing a pachaga control drug solution by using the same preparation method as the test solution, sucking 30 mu L of the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, taking toluene-ethyl acetate-petroleum ether-diethylamine (the volume ratio is 5: 2: 7: 1) as a developing agent, unfolding, taking out, airing, spraying an improved bismuth iodide solution, and inspecting spots with the same color in a sample chromatogram at positions corresponding to the control drug chromatogram.
Example 4:
taking 3G of a drug to be detected, grinding, sieving by a 100-mesh sieve, adding 3m L of ammonia water, carrying out ultrasonic treatment by using methanol, filtering, volatilizing the methanol from filtrate, dissolving by using an acetic acid solution with the mass percentage concentration of 6%, extracting the dissolved solution by using butyl acetate, concentrating to be dry, dissolving by using ethanol to be 1m L to serve as a test solution, taking 1mg of a pachaga control drug, preparing a pachaga control drug solution by using the same preparation method as the test solution, sucking the two solutions, respectively dropping 25 mu L on the same silica gel G thin layer plate, taking toluene-ethyl acetate-petroleum ether-diethylamine (the volume ratio is 5: 2: 8: 1.5) as a developing agent, unfolding, taking out, airing, spraying an improved bismuth potassium iodide solution, and inspecting spots with the same color in a sample chromatogram at positions corresponding to the control drug chromatogram.
Example 5:
taking 2.5G of a drug to be detected, grinding, sieving by a 100-mesh sieve, adding 2.5m of ammonia water to L, wetting, performing ultrasonic treatment by methanol, filtering, volatilizing methanol from filtrate, dissolving by using an acetic acid solution with the mass percentage concentration of 7%, extracting the dissolved solution by using butyl acetate, concentrating to dryness, dissolving by using ethanol to 1m L to serve as a test solution, taking 1mg of a pachaga control drug, preparing a pachaga control drug solution by using the same preparation method as the test solution, sucking the two solutions with the thickness of 30 mu L respectively, dropping the two solutions on the same silica gel G thin layer plate, taking toluene-ethyl acetate-petroleum ether-diethylamine (the volume ratio is 4: 3: 7: 2) as a developing agent, unfolding, taking out, drying in the air, spraying an improved bismuth potassium iodide solution, inspecting, and inspecting spots with the same color in positions corresponding to the control drug chromatogram.
Example 6:
taking 3G of a drug to be detected, grinding, sieving by a 100-mesh sieve, adding 3m L of ammonia water, carrying out ultrasonic treatment by using methanol, filtering, volatilizing the methanol from filtrate, dissolving by using an acetic acid solution with the mass percentage concentration of 6.5%, extracting the dissolved solution by using butyl acetate, concentrating to dryness, dissolving by using ethanol to 1m L to serve as a test solution, taking 1mg of a pachaga control drug, preparing a pachaga control drug solution by using the same preparation method as the test solution, sucking the two solutions with the thickness of 25 mu L respectively, dropping the two solutions on the same silica gel G thin layer plate, taking toluene-ethyl acetate-petroleum ether-diethylamine (the volume ratio is 8: 4: 10: 2) as a developing agent, unfolding, taking out, airing, spraying an improved bismuth potassium iodide solution, and inspecting spots with the same color in a sample chromatogram at positions corresponding to the control drug chromatogram.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, and those skilled in the art may make modifications and variations within the spirit of the present invention, and all modifications, equivalents and modifications of the above embodiments according to the technical spirit of the present invention are within the scope of the present invention.
Claims (3)
1. A method for determining Tibetan medicine Shiwei Ruxiang pills is characterized in that the method detects the pachaga therein through thin-layer chromatography, and specifically comprises the steps of taking 2-3G of a medicine to be detected, grinding the medicine to be detected, sieving the medicine to be detected by a 100-mesh sieve, adding 2-3 m L of ammonia water for wetting, carrying out ultrasonic treatment by using methanol, filtering, volatilizing the methanol from filtrate, dissolving the filtrate by using an acetic acid solution, extracting the dissolved solution by using butyl acetate, concentrating the solution to be dry, dissolving the solution to be 1m L by using ethanol to serve as a test solution, taking 1mg of a pachaga control medicinal material, preparing a pachaga control medicinal material solution by using the same preparation method as the test solution, sucking the two solutions with the diameters of 20-30 mu L respectively, dropping the two solutions on the same silica gel G thin-layer plate, taking toluene-ethyl acetate-petroleum ether-diethylamine as a developing agent, developing, taking out, airing, spraying the solution with improved potassium iodide, and inspecting spots with the same color in the sample chromatogram on the positions corresponding to the control medicinal material chromatogram;
wherein the volume ratio of toluene to ethyl acetate to petroleum ether to diethylamine in the developing agent is as follows: 3-8: 0.2-4: 5-10: 1-2.
2. The method for measuring the ten-ingredient Tibetan frankincense pill as claimed in claim 1, which is characterized in that: the mass percentage concentration of the acetic acid solution is 5-7%.
3. The method for measuring the ten-ingredient Tibetan frankincense pill as claimed in claim 2, which is characterized in that: the volume ratio of toluene to ethyl acetate to petroleum ether to diethylamine in the developing agent is as follows: 5:1.5:6.5:1.2.
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| CN102520113B (en) * | 2011-12-16 | 2014-05-07 | 西藏奇正藏药股份有限公司 | Detection method for fifteen Rupeng preparation |
| CN102520110B (en) * | 2011-12-16 | 2014-04-23 | 西藏奇正藏药股份有限公司 | Method for detecting ten-flavour rankincense preparation |
| CN102419357B (en) * | 2011-12-26 | 2014-11-12 | 西藏奇正藏药股份有限公司 | Method for detecting eighteen-component codonopsis pilosula preparation |
| CN102749401B (en) * | 2012-07-30 | 2013-12-18 | 山东阿如拉药物研究开发有限公司 | Inspection method of traditional Chinese medicine composition twenty-five-ingredient lung disease preparation |
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Effective date of registration: 20200616 Address after: 311404 No. 6, Shengfeng Road, Xindeng Town, Fuyang District, Hangzhou City, Zhejiang Province Applicant after: Hangzhou Fuchun Industry Co.,Ltd. Address before: 237000 east side of jingsan Road, Lu'an economic and Technological Development Zone, Anhui Province (502 science and technology entrepreneurship center) Applicant before: LU'AN SANJIANG BIOTECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20211215 Address after: 276000 No. 30, Xiangyu Road, economic and Technological Development Zone, Linyi City, Shandong Province Patentee after: XIANGYU PHARMACEUTICAL Co.,Ltd. Address before: No.6 Shengfeng Road, Xindeng Town, Fuyang District, Hangzhou City, Zhejiang Province Patentee before: Hangzhou Fuchun Industry Co.,Ltd. |