CN103940916A - Fingerprint analysis method of "Jinghua" capsule for treating stomach disease - Google Patents
Fingerprint analysis method of "Jinghua" capsule for treating stomach disease Download PDFInfo
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Abstract
The invention provides a fingerprint analysis method of a "Jinghua" capsule for treating stomach disease. The method comprises the following steps: preparing a reference solution and a test solution, and carrying out analysis through gas chromatography to obtain the fingerprint. The analysis method adopts gas chromatography to obtain the fingerprint of the capsule according to the characteristics of the capsule, finds the optimized chromatography conditions, thus the measurement result is precise, and the repeatability and the stability are good. The invention also provides a fingerprint of the "Jinghua" capsule for treating stomach disease.
Description
Technical field
The present invention relates to medical technical field, be specifically related to a kind of chaste tree Weikang capsule for curing gastropathy Gas Chromatography Fingerprint detection method.
Background technology
Chaste tree Weikang capsule for curing gastropathy is to be made up of chenopodium ambrosiodies, water body flower, has the effect of relieving haperacidity, analgesia, inhibition helicobacter pylori and protection gastric mucosa.This product has loose the trembling with fear of regulating the flow of vital energy, effect of heat clearing and blood stasis dispersing.Be applicable to epigastric distension and distress, pain, belch, return the disease such as acid, duodenal ulcer.
The formula of chaste tree Weikang capsule for curing gastropathy and preparation method are prior aries; evaluate effective control device of traditional Chinese medicine quality as the globality of multidimensional complicated components sample, traditional Chinese medicine fingerprint is can be a kind of method of the thoroughly evaluating traditional Chinese medicine quality pattern accepted extensively both at home and abroad at present.U.S. FDA allows declarer that the chromatographic fingerprinting data of product is provided in autonomic drug goods governing principle, German medicinal plant association, British Herbal Pharmacopoeia, India herbal medicine allusion quotation and Canada is medicinal and also one of content using finger-print as quality control standard all of fragrant plant association.Domestic scholars thank training mountain also think, traditional Chinese medicine quality needs comprehensive evaluation, fingerprint map analyzing is that Chinese medicine and preparation are carried out to one of feasible means of comprehensive macroanalysis.But have about the research of chaste tree Weikang capsule for curing gastropathy finger-print aspect and there is not yet report at home and abroad.
Summary of the invention
In order to control better the quality of chaste tree Weikang capsule for curing gastropathy, ensure security and the validity of clinical application, the invention provides a kind of chaste tree Weikang capsule for curing gastropathy fingerprint analysis method.
According to chaste tree Weikang capsule for curing gastropathy fingerprint analysis method of the present invention, comprise the following steps:
(1) preparation of reference substance solution: get reference substance appropriate, accurately weighed, solubilizer is mixed with solution, to obtain final product;
(2) preparation of need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate, accurately weighed, put in volumetric flask, solubilizer dissolves, and is settled to scale, to obtain final product;
(3) get described need testing solution, adopt gas chromatography to analyze, obtain finger-print.
Preferably, being prepared as of described reference substance solution: get p-cymene reference substance appropriate, accurately weighed, add ethyl acetate and make the solution of every 1mL containing the about 0.3-0.7mg of p-cymene, to obtain final product.
Experiment shows, p-cymene chromatographic peak accounts for the more than 20% of total peak area, therefore preferably taking p-cymene as reference substance.
Preferably, being prepared as of described need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate, take respectively about 10-50mg, accurately weighed, put in 5mL volumetric flask, add ethyl acetate and dissolve in right amount, and be settled to scale, to obtain final product.
According to one of embodiment of the present invention, the chromatographic condition of described gas chromatography is: chromatographic column: nonpolar or middle polarity chromatographic column; Column temperature: temperature programme; Injector temperature: 150-300 DEG C; Fid detector; Temperature: 200-300 DEG C; Carrier gas: nitrogen.
Preferably, described chromatographic column fixed phase is taking 14% cyanogen propyl group-phenyl 86% dimethyl polysiloxane as filler, and the condition of described temperature programme is:
Investigate the separating effect of opposed polarity capillary column, result shows: nonpolar capillary column separates the chromatographic peak number and the peak shape that obtain with middle polarity capillary column basically identical, wherein the chromatographic peak degree of separation of middle polarity chromatographic column is larger, therefore preferred middle polarity chromatographic column.
The present invention further provides a kind of chaste tree Weikang capsule for curing gastropathy finger-print obtaining by said method.
According to the present invention, described finger-print is made up of 11 total fingerprint peakses.
According to one of embodiment of the present invention, described 11 total peaks are respectively with respect to average relative retention time and the RSD of p-cymene:
No. 1 peak, average retention time is 0.649min, RSD is 0.02%;
No. 2 peaks, average retention time is 0.839min, RSD is 0.01%;
No. 3 peaks, average retention time is 0.919min, RSD is 0.01%;
No. 4 peaks, average retention time is 0.945min, RSD is 0.01%;
No. 5 peaks, average retention time is 1.000min, RSD is 0.00%;
No. 6 peaks, average retention time is 1.045min, RSD is 0.01%;
No. 7 peaks, average retention time is 1.473min, RSD is 0.01%;
No. 8 peaks, average retention time is 1.618min, RSD is 0.02%;
No. 9 peaks, average retention time is 1.743min, RSD is 0.01%;
No. 10 peaks, average retention time is 2.182min, RSD is 0.01%;
No. 11 peaks, average retention time is 2.865min, RSD is 0.01%.
Another embodiment according to the present invention, described 11 total peaks are respectively with respect to average relative peak area and the RSD of p-cymene:
No. 1 peak, average relative peak area is that 0.179, RSD is 40.17%;
No. 2 peaks, average relative peak area is that 0.043, RSD is 37.30%;
No. 3 peaks, average relative peak area is that 1.115, RSD is 3.50%;
No. 4 peaks, average relative peak area is that 0.034, RSD is 29.80%;
No. 5 peaks, average relative peak area is that 1.000, RSD is 0.00%;
No. 6 peaks, average relative peak area is that 0.015, RSD is 4.55%;
No. 7 peaks, average relative peak area is that 0.015, RSD is 3.85%;
No. 8 peaks, average relative peak area is that 0.134, RSD is 39.36%;
No. 9 peaks, average relative peak area is that 0.062, RSD is 33.37%;
No. 10 peaks, average relative peak area is that 0.785, RSD is 2.10%;
No. 11 peaks, average relative peak area is that 1.002, RSD is 2.44%.
According to the present invention, described in described 11 total peaks, No. 1 peak is australene; Described No. 2 peaks are phellandrene; Described No. 3 peaks are α-terpinene; Described No. 4 peaks are citrene; Described No. 5 peaks are p-cymene; Described No. 6 peaks are cyclohexadiene; Described No. 8 peaks are isocarveol; Described No. 10 peaks are terpinolene.
The present invention, according to chaste tree Weikang capsule for curing gastropathy own characteristic, adopts the finger-print of gas chromatography determination chaste tree Weikang capsule for curing gastropathy, has found the chromatographic condition of optimizing, and makes measurement result precision, reproducible, has good stability.
The present invention has good linearity, repeatability, reappearance and the recovery, contributes to control the quality of chaste tree Weikang capsule for curing gastropathy more comprehensively.
Brief description of the drawings
Fig. 1 HP-5 capillary chromatographic column chromatogram.
Fig. 2 DB-1701 capillary chromatographic column chromatogram.
2 times of analysis duration chromatograms of Fig. 3.
Fig. 4 10 batch sample comparison diagrams.
Fig. 5 chaste tree Weikang capsule for curing gastropathy reference fingerprint fitted figure.
110305 batches of chaste tree Weikang capsule for curing gastropathy sample mass spectrograms of Fig. 6.
Embodiment
The selection of test example one chromatographic column
Chromatographic column: 1. non-polar column, fixing taking 5% phenyl 95% dimethyl polysiloxane as filler, Agilent HP-5(30m × 0.32mm × 0.25 μ is m);
2. middle polarity post, fixing taking 14% cyanogen propyl group-phenyl 86% dimethyl polysiloxane as filler, Agilent DB-1701(30m × 0.25mm × 0.25 μ m).
Investigate the separating effect of opposed polarity capillary column, 2 kinds of opposed polarity capillary columns separate the chromatographic peak number and the peak shape basically identical (seeing Fig. 1～2) that obtain as a result, wherein chromatographic column chromatographic peak degree of separation is 2. larger, therefore 2. preferred column carries out the investigation of temperature programme condition.
The selection of test example two temperature programme conditions
Use chromatographic column 2. temperature programme condition to be investigated to adjustments, ensureing out that peak is completely in situation, shortening analysis duration as far as possible.Result, under this temperature programme condition (in Table (1)), is isolated approximately 11 chromatographic peaks altogether, and analysis time, overall length was 46min, saw Fig. 2.
Table (1) temperature programme table
Detection method of the present invention, its chromatographic condition is learned checking through following methods, and proving effect is good.
Test example three methodology checkings
Instrument: U.S. Agilent7890A, ChemStation workstation.
Chromatographic column: fixing taking 14% cyanogen propyl group-phenyl 86% dimethyl polysiloxane as filler, Agilent DB-1701(30m × 0.25mm × 0.25 μ m).
Column temperature: temperature programme condition is in Table (1); Injector temperature: 250 DEG C; Detecting device: FID; Temperature: 250 DEG C;
Carrier gas: nitrogen; Split sampling; Split ratio: 15: 1; Sample size: 1 μ L.
Reagent: ethyl acetate (chromatographically pure, Tianjin Concord Technology Co., Ltd.).
Reference substance: p-cymene (Sigma company, lot number: MKBB0433, purity > 99%).
Sample: chaste tree Weikang capsule for curing gastropathy (Tianjin Tasly Pharmaceutical Co., Ltd, lot number: 100312,110309,110403,110406,, 110409,110410,110501,110502,110503,110507,2011E09,110606).
Replica test
Get with a collection of chaste tree Weikang capsule for curing gastropathy (lot number: 110606), 6 parts of test samples of parallel preparation, adopt above-mentioned chromatographic condition, analyze.
Taking the retention time of No. 5 peak p-cymenes and peak area as 1, calculate the ratio of relative retention time (R.Rt) and the relative peak area (R.A) of other each total fingerprint peaks.The results are shown in Table (2).Result repeatability is good.
Relative retention time, the relative peak area tables of data of table (2) replica test
Precision test
Get with a collection of chaste tree Weikang capsule for curing gastropathy (lot number: 110606), prepare 1 part of test sample continuous sample introduction 6 times, adopt above-mentioned chromatographic condition, analyze.
Taking the retention time of No. 5 peak p-cymenes and peak area as 1, calculate the ratio of relative retention time (R.Rt) and the relative peak area (R.A) of other each total fingerprint peaks.The results are shown in Table (3).Result precision is good.
Relative retention time, the relative peak area tables of data of table (3) precision test
Stability test
Get with a collection of chaste tree Weikang capsule for curing gastropathy (lot number: 110606), prepare 1 part of test sample in 0,2,4,8,11,14,19,24H sample introduction respectively, adopt above-mentioned chromatographic condition, analyze.
Taking the retention time of No. 5 peak p-cymenes and peak area as 1, calculate the ratio of relative retention time (R.Rt) and the relative peak area (R.A) of other each total fingerprint peaks.The results are shown in Table (4).In result 24H, sample stability is good.
Relative retention time, the relative peak area tables of data of table (4) stability test
The foundation of test example four finger-prints
For determining the accuracy of finger-print of chaste tree Weikang capsule for curing gastropathy; need Criterion reference fingerprint; the foundation of standard control finger-print of the present invention is by the detection to many batch samples, in the situation that its chromatogram homogeneity is good, determines, process of establishing is as follows:
Choose at random 10 batches of chaste tree Weikang capsule for curing gastropathy, prepare need testing solution, adopt above-mentioned chromatographic condition, analyze.According to 10 batches of given correlation parameters of chaste tree Weikang capsule for curing gastropathy test sample GC collection of illustrative plates; the main chromatographic peak that chaste tree Weikang capsule for curing gastropathy is measured gained all occurred in 35 minutes; by the technical requirement of setting up finger-print; the need testing solution chromatogram that records 70 minutes 2 times of times shows not occur for 35 minutes chromatographic peak (see figure 3) later.
Relatively the chromatogram of 10 batch samples find that there is 11 chromatographic peaks be each batch total, the overlapping chromatogram (see figure 4) of 10 batch samples.Separately relative retention time and the relative peak area at 11 total peaks in 10 batch samples are analyzed, taking No. 5 peak p-cymenes as with reference to peak, the relative retention time and the peak area ratio that calculate other 10 total peaks, the relative retention time RSD of 10 batch samples is all in 0.1%; Unimodal area is greater than 10% relative peak area ratio R SD all in 5.0%, in Table (5), (6).
Table (5) 10 batch sample relative retention time tables of data
Table (6) 10 batch sample relative peak area ratio data tables
As total peak, utilize computer simulation similarity software for calculation (2004A version) taking 11 peaks in the finger-print of above-mentioned 10 batch samples, chaste tree Weikang capsule for curing gastropathy finger-print is determined in matching, sees Fig. 5.This collection of illustrative plates is chaste tree Weikang capsule for curing gastropathy standard control finger-print of the present invention.
Taking chaste tree Weikang capsule for curing gastropathy standard control finger-print as contrast; adopt computer simulation similarity software for calculation (2004B version); the similarity of precision, repeatability, stability test data in computing methodology checking, similarity all, more than 0.990, the results are shown in Table (7).
The similarity of table (7) precision, repeatability, stability test data
The GC-MS qualitative analysis at total peak
Precision takes 110305 crowdes of 30mg of chaste tree Weikang capsule for curing gastropathy; press test sample disposal methods sample; adopt Agilent HP-5MS capillary chromatographic column; carry out the analysis of gas chromatograph-mass spectrometer (GCMS) by chromatographic condition of the present invention, the model of gas chromatograph-mass spectrometer (GCMS) is: Agilent7890A-5975C.
The collection of illustrative plates of chaste tree Weikang capsule for curing gastropathy and corresponding gas chromatogram are basically identical, and only No. 4 peak separation are poor, see Fig. 6.
Each chromatographic peak in sample and NIST8.0 spectrum storehouse are compared, identify altogether 8 peaks in 11 total peaks, be respectively peak australene No. 1; No. 2 peak phellandrenes; No. 3 peak α-terpinene; No. 4 peak citrenes; No. 5 peak p-cymenes; No. 6 peak cyclohexadiene; No. 8 peak isocarveols; No. 10 peak 4-terpinolene.
Embodiment 1,
(1) preparation of reference substance solution: get p-cymene reference substance appropriate, accurately weighed, add ethyl acetate and make the solution of every 1mL containing the about 0.5mg of p-cymene, to obtain final product.
(2) preparation of need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate, take respectively about 30mg, accurately weighed, put in 5mL volumetric flask, add ethyl acetate and dissolve in right amount, and be settled to scale, to obtain final product.
(3) get described need testing solution, adopt gas chromatography to analyze, obtain finger-print.
Chromatographic condition:
Chromatographic column: fixing taking 14% cyanogen propyl group-phenyl 86% dimethyl polysiloxane as filler; Column temperature: temperature programme; Injector temperature: 250 DEG C; Fid detector; Temperature: 250 DEG C; Carrier gas: nitrogen.
The condition of temperature programme is:
Embodiment 2
(1) preparation of reference substance solution: get p-cymene reference substance appropriate, accurately weighed, add ethyl acetate and make the solution of every 1mL containing the about 0.3mg of p-cymene, to obtain final product.
(2) preparation of need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate, take respectively about 10mg, accurately weighed, put in 5mL volumetric flask, add ethyl acetate and dissolve in right amount, and be settled to scale, to obtain final product.
(3) get described need testing solution, adopt gas chromatography to analyze, obtain finger-print.
Chromatographic condition:
Chromatographic column: fixing taking 5% phenyl 95% dimethyl polysiloxane as filler, Agilent HP-5(30m × 0.32mm × 0.25 μ m); Column temperature: temperature programme; Injector temperature: 150 DEG C; Fid detector; Temperature: 300 DEG C; Carrier gas: nitrogen.
The condition of temperature programme is:
Embodiment 3
(1) preparation of reference substance solution: get p-cymene reference substance appropriate, accurately weighed, add ethyl acetate and make the solution of every 1mL containing the about 0.7mg of p-cymene, to obtain final product.
(2) preparation of need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate, take respectively about 50mg, accurately weighed, put in 5mL volumetric flask, add ethyl acetate and dissolve in right amount, and be settled to scale, to obtain final product.
(3) get described need testing solution, adopt gas chromatography to analyze, obtain finger-print.
Chromatographic condition:
Chromatographic column: crosslinked 50% phenyl-methyl polysiloxane be fixing phase capillary column (column length is 30m, and internal diameter is 0.32mm, film thickness be 0.25 μ m); Column temperature: temperature programme; Injector temperature: 200 DEG C; Fid detector; Temperature: 300 DEG C; Carrier gas: nitrogen.
The condition of temperature programme is:
Embodiment 4
(1) preparation of reference substance solution: get p-cymene reference substance appropriate, accurately weighed, add ethyl acetate and make the solution of every 1mL containing the about 0.6mg of p-cymene, to obtain final product.
(2) preparation of need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate, take respectively about 40mg, accurately weighed, put in 5mL volumetric flask, add ethyl acetate and dissolve in right amount, and be settled to scale, to obtain final product.
(3) get described need testing solution, adopt gas chromatography to analyze, obtain finger-print.
Chromatographic condition:
Chromatographic column: fixing taking 14% cyanogen propyl group-phenyl 86% dimethyl polysiloxane as filler; Column temperature: temperature programme; Injector temperature: 250 DEG C; Fid detector; Temperature: 250 DEG C; Carrier gas: nitrogen.
The condition of temperature programme is:
Embodiment 5
(1) preparation of reference substance solution: get p-cymene reference substance appropriate, accurately weighed, add ethyl acetate and make the solution of every 1mL containing the about 0.5mg of p-cymene, to obtain final product.
(2) preparation of need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate, take respectively about 30mg, accurately weighed, put in 5mL volumetric flask, add ethyl acetate and dissolve in right amount, and be settled to scale, to obtain final product.
(3) get described need testing solution, adopt gas chromatography to analyze, obtain finger-print.
Chromatographic condition:
Chromatographic column: crosslinked 50% phenyl-methyl polysiloxane be fixing phase capillary column (column length is 30m, and internal diameter is 0.32mm, film thickness be 0.25 μ m); Column temperature: temperature programme; Injector temperature: 200 DEG C; Fid detector; Temperature: 200 DEG C; Carrier gas: nitrogen.
The condition of temperature programme is:
Embodiment 6
(1) preparation of reference substance solution: get p-cymene reference substance appropriate, accurately weighed, add ethyl acetate and make the solution of every 1mL containing the about 0.5mg of p-cymene, to obtain final product.
(2) preparation of need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate, take respectively about 30mg, accurately weighed, put in 5mL volumetric flask, add ethyl acetate and dissolve in right amount, and be settled to scale, to obtain final product.
(3) get described need testing solution, adopt gas chromatography to analyze, obtain finger-print.
Chromatographic condition:
Chromatographic column: fixing taking 14% cyanogen propyl group-phenyl 86% dimethyl polysiloxane as filler; Column temperature: temperature programme; Injector temperature: 250 DEG C; Fid detector; Temperature: 300 DEG C; Carrier gas: nitrogen.
The condition of temperature programme is:
Claims (10)
1. a chaste tree Weikang capsule for curing gastropathy fingerprint analysis method, is characterized in that, said method comprising the steps of:
(1) preparation of reference substance solution: get reference substance appropriate, accurately weighed, solubilizer is mixed with solution, to obtain final product;
(2) preparation of need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate, accurately weighed, put in volumetric flask, solubilizer dissolves, and is settled to scale, to obtain final product;
(3) get described need testing solution, adopt gas chromatography to analyze, obtain finger-print.
2. the method for claim 1, is characterized in that, being prepared as of described reference substance solution: get p-cymene reference substance appropriate, and accurately weighed, add ethyl acetate and make the solution of every 1mL containing the about 0.3-0.7mg of p-cymene, to obtain final product.
3. the method for claim 1, is characterized in that, being prepared as of described need testing solution: get chaste tree Weikang capsule for curing gastropathy content appropriate; take respectively about 10-50mg, accurately weighed, put in 5mL volumetric flask; add ethyl acetate and dissolve in right amount, and be settled to scale, to obtain final product.
4. the method for claim 1, is characterized in that, the chromatographic condition of described gas chromatography is: chromatographic column: nonpolar or middle polarity chromatographic column; Column temperature: temperature programme; Injector temperature: 150-300 DEG C; Fid detector; Temperature: 200-300 DEG C; Carrier gas: nitrogen.
5. method as claimed in claim 4, is characterized in that, described chromatographic column fixed phase is taking 14% cyanogen propyl group-phenyl 86% dimethyl polysiloxane as filler, and the condition of described temperature programme is:
6. the chaste tree Weikang capsule for curing gastropathy finger-print obtaining by claim 1-5 any one.
7. finger-print as claimed in claim 6, is characterized in that, described finger-print is made up of 11 total fingerprint peakses.
8. finger-print as claimed in claim 7, is characterized in that, described 11 total peaks are respectively with respect to average relative retention time and the RSD of p-cymene:
No. 1 peak, average retention time is 0.649min, RSD is 0.02%;
No. 2 peaks, average retention time is 0.839min, RSD is 0.01%;
No. 3 peaks, average retention time is 0.919min, RSD is 0.01%;
No. 4 peaks, average retention time is 0.945min, RSD is 0.01%;
No. 5 peaks, average retention time is 1.000min, RSD is 0.00%;
No. 6 peaks, average retention time is 1.045min, RSD is 0.01%;
No. 7 peaks, average retention time is 1.473min, RSD is 0.01%;
No. 8 peaks, average retention time is 1.618min, RSD is 0.02%;
No. 9 peaks, average retention time is 1.743min, RSD is 0.01%;
No. 10 peaks, average retention time is 2.182min, RSD is 0.01%;
No. 11 peaks, average retention time is 2.865min, RSD is 0.01%.
9. finger-print as claimed in claim 7, is characterized in that, described 11 total peaks are respectively with respect to average relative peak area and the RSD of p-cymene:
No. 1 peak, average relative peak area is that 0.179, RSD is 40.17%;
No. 2 peaks, average relative peak area is that 0.043, RSD is 37.30%;
No. 3 peaks, average relative peak area is that 1.115, RSD is 3.50%;
No. 4 peaks, average relative peak area is that 0.034, RSD is 29.80%;
No. 5 peaks, average relative peak area is that 1.000, RSD is 0.00%;
No. 6 peaks, average relative peak area is that 0.015, RSD is 4.55%;
No. 7 peaks, average relative peak area is that 0.015, RSD is 3.85%;
No. 8 peaks, average relative peak area is that 0.134, RSD is 39.36%;
No. 9 peaks, average relative peak area is that 0.062, RSD is 33.37%;
No. 10 peaks, average relative peak area is that 0.785, RSD is 2.10%;
No. 11 peaks, average relative peak area is that 1.002, RSD is 2.44%.
10. the finger-print as described in claim 8 or 9 any one, is characterized in that, described No. 1 peak is australene; Described No. 2 peaks are phellandrene; Described No. 3 peaks are α-terpinene; Described No. 4 peaks are citrene; Described No. 5 peaks are p-cymene; Described No. 6 peaks are cyclohexadiene; Described No. 8 peaks are isocarveol; Described No. 10 peaks are terpinolene.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104897837A (en) * | 2015-06-08 | 2015-09-09 | 辽宁华润本溪三药有限公司 | Detection method of pharmaceutical preparation for curing stomach pain caused by qi stagnation |
| CN111366672A (en) * | 2020-04-24 | 2020-07-03 | 劲牌有限公司 | Detection method of health wine fingerprint |
| CN113984917A (en) * | 2021-03-01 | 2022-01-28 | 天津中医药大学 | Method for detecting volatile chemical components in Weichang' an pills |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6344219B1 (en) * | 1995-03-23 | 2002-02-05 | Yongchuan Zhang | Chinese drug composition for treatment of peptic ulcer and preparation thereof |
| CN101183089A (en) * | 2006-11-13 | 2008-05-21 | 天津天士力制药股份有限公司 | Method for measuring content of p-Cymene |
| CN101194946A (en) * | 2006-12-08 | 2008-06-11 | 天津天士力制药股份有限公司 | Medicament for treating gastric cavity ache and method for preparing the same |
| CN102478551A (en) * | 2010-11-23 | 2012-05-30 | 天津天士力制药股份有限公司 | Method for determining effective component content in chenopodium ambrosioides volatile oil |
-
2013
- 2013-01-17 CN CN201310016847.4A patent/CN103940916B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6344219B1 (en) * | 1995-03-23 | 2002-02-05 | Yongchuan Zhang | Chinese drug composition for treatment of peptic ulcer and preparation thereof |
| CN101183089A (en) * | 2006-11-13 | 2008-05-21 | 天津天士力制药股份有限公司 | Method for measuring content of p-Cymene |
| CN101194946A (en) * | 2006-12-08 | 2008-06-11 | 天津天士力制药股份有限公司 | Medicament for treating gastric cavity ache and method for preparing the same |
| CN102478551A (en) * | 2010-11-23 | 2012-05-30 | 天津天士力制药股份有限公司 | Method for determining effective component content in chenopodium ambrosioides volatile oil |
Non-Patent Citations (5)
| Title |
|---|
| CAROLINA MARANGON JARDIM 等: "Composition and Antifungal Activity of the Essential Oil of the Brazilian Chenopodium ambrosioides L.", 《J CHEM ECOL》 * |
| 朱永宏 等: "气相色谱法同时测定荆花胃康胶丸中驱蛔素、对伞花烃、α-松油烯的含量", 《中国新药杂志》 * |
| 李意: "RP-HPLC法分离和测定荆花胃康原料药和胶丸中的对-异丙基甲苯和α-萜品烯", 《分析实验室》 * |
| 聂小妮 等: "不同产地土荆芥挥发油GC指纹图谱研究", 《西北植物学报》 * |
| 陈强: "荆花胃康胶丸的GC指纹图谱研究", 《海峡药学》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104897837A (en) * | 2015-06-08 | 2015-09-09 | 辽宁华润本溪三药有限公司 | Detection method of pharmaceutical preparation for curing stomach pain caused by qi stagnation |
| CN111366672A (en) * | 2020-04-24 | 2020-07-03 | 劲牌有限公司 | Detection method of health wine fingerprint |
| CN111366672B (en) * | 2020-04-24 | 2021-06-22 | 劲牌有限公司 | Detection method of health wine fingerprint |
| CN113984917A (en) * | 2021-03-01 | 2022-01-28 | 天津中医药大学 | Method for detecting volatile chemical components in Weichang' an pills |
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Address after: 300410 Tianjin city Beichen District Huaihe road and road intersection Dingjiang tianzhijiao Park forensic Center for Intellectual Property Department Patentee after: Tasly Pharmaceutical Group Limited by Share Ltd Address before: 300410 Tianjin city Beichen District Huaihe road and road intersection Dingjiang tianzhijiao Park forensic Center for Intellectual Property Department Patentee before: Tasly Pharmaceutical Group Co., Ltd. |