CN102091283B - Method for detecting Xingnaojing injection - Google Patents
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Abstract
The invention relates to a method for detecting a traditional Chinese medicinal preparation, in particular to a method for detecting a traditional Chinese medicament, namely Xingnaojing injection. The detection method comprises the following steps of: observing characteristics; identifying contents; detecting the contents; comparing a finger-print; and measuring content of ingredients which the injection comprises.
Description
Technical field
The present invention relates to a kind of detection method of Chinese medicine preparation, be specifically related to a kind of detection method of Chinese medicine XINGNAOJING ZHUSHEYE.
Background technology
XINGNAOJING ZHUSHEYE comprises the effective constituent of Moschus, cape jasmine, root tuber of aromatic turmeric, borneol four traditional Chinese medicine material, because Chinese crude drug composition more complicated detects by existing quality standard, can not monitor the quality of finished product fully.
Existing product detection method influence factor is more, and reappearance is relatively poor as a result, can not the better controlled drug quality, thus can not guarantee the stable uniform of product quality well.
For guaranteeing its steady quality homogeneous, this just requires have a good method of quality control that it is carried out effective quality control to product, makes product accomplish " safe, effective, quality controllable ".
In order better to guarantee the quality of XINGNAOJING ZHUSHEYE finished product; So the method for employing finger-print is carried out quality control to the material of each link; The method that adopts than primary standard has more accurately, the characteristics of favorable reproducibility, thereby can accurately strictly control the quality and the homogeneity of product.
Summary of the invention
The present invention is to provide a kind of method of quality control to XINGNAOJING ZHUSHEYE; Can comprise following content: the observation of proterties, the discriminating of content, the inspection of content; Finger-print relatively; Composition to containing carries out assay, and therefore, its main content of method of quality control of the present invention is that the composition to XINGNAOJING ZHUSHEYE detects.This method can be held the quality of relevant medicine more accurately, reduces drug risk.
The present invention provides a kind of detection method of XINGNAOJING ZHUSHEYE, comprises that intermedium and the XINGNAOJING ZHUSHEYE to Moschus, root tuber of aromatic turmeric, borneol, cape jasmine, XINGNAOJING ZHUSHEYE carries out determining fingerprint pattern.
The present invention differentiates the drug ingedient in the medicine through determining fingerprint pattern, therefore the present invention relates to a kind of finger-print relative method.
Said finger-print relative method may further comprise the steps:
The finger-print of step 2, mensuration preparation;
Step 3, the finger-print of standard control finger-print and preparation is compared.
More available range estimation also can adopt software for calculation relatively, and test sample finger-print and standard control finger-print similarity are qualified greater than 0.80, and is preferred 0.90, and more preferably 0.95.
Said employing software for calculation is to adopt a kind of chromatographic fingerprints of Chinese materia medica similarity evaluation system software that is provided by Chinese Pharmacopoeia Commission relatively, belongs to the known operation method.
Method of the present invention, wherein various data are experiment and obtain, and in actual mechanical process, have error, this error ± 20% with interior all can, therefore the numerical value in the method for the present invention be on the numerical value basis that the present invention puts down in writing ± 20% in.
Anyone all drops in the scope of the invention with interior use numerical value of the present invention ± 20%.
Finger-print relative method concrete steps of the present invention are following:
1) mensuration of standard Moschus finger-print
A. chromatographic condition and system suitability test: WAX capillary column; 30m * 0.25mm * 0.25 μ m (thickness); Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 3: 1; Fid detector temperature: 270 ℃; Injector temperature: 270 ℃; Column temperature: 50 ℃ of 200 ℃ of 240 ℃ of (0min) 4 ℃/min of (5min) 10 ℃/min (30min);
B. the preparation of object of reference solution: get the 0.025g heptadecane and be settled in the 50ml volumetric flask, promptly get, as inner mark solution with normal hexane
C. the preparation of need testing solution: precision takes by weighing Moschus medicinal material 40mg, to 500ml round-bottomed flask flask, adds distilled water 200ml; Normal hexane 2ml,, in electric jacket, extract 4h respectively with the volatile oil extractor heating;, collect hexane solution to the 5ml volumetric flask, the accurate inner mark solution 1ml that adds; And be settled to scale with normal hexane, as need testing solution.
D. determination method: get each batch medicinal material need testing solution 2 μ l respectively, inject gas chromatograph, record 1h chromatogram.
2) standard root tuber of aromatic turmeric determining fingerprint pattern
A. chromatographic condition and system suitability test: WAX capillary column; 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 50 ℃ of 90 ℃ of 220 ℃ of (5min) 2 ℃/min of (5min) 4 ℃/min (6min); Sample size: 1 μ l.
B. the preparation of object of reference solution: get the 0.035g dodecane and be settled in the 500ml volumetric flask, promptly get, as inner mark solution with normal hexane.
C. the preparation of need testing solution: get the RADIX CURCUMAE sample and be ground into meal, 20.0 grams of taking a sample are respectively put in the round-bottomed flask; Add distilled water 200ml; Place after 12 hours, add the 3ml normal hexane, put in the electric jacket with volatile oil extractor heating and extracting 8 hours; Collect normal hexane and be settled in the 5ml volumetric flask the extremely clarification of adding anhydrous sodium sulfate dehydration.Precision is measured 1.00ml normal hexane sample solution, with 1.00ml inner mark solution mixing, as need testing solution.
D. determination method: get need testing solution 1 μ l, inject gas chromatograph writes down 1 hour chromatogram.
3) standard borneol determining fingerprint pattern
A. chromatographic column: WAX capillary column (30m * 0.25mm * 0.25 μ m); Injector temperature: 200 ℃; Fid detector temperature: 200 ℃; Carrier gas: high pure nitrogen; Flow velocity 1ml/min; Split ratio: 40: 1; Column temperature: 100 ℃ (5min) 7 ℃/min170 ℃; Internal standard compound: octadecane.
B. the preparation of standard solution
The accurate title, decided the camphor standard items, is dissolved in surely in the 5ml volumetric flask with normal hexane, is made into the standard solution that concentration is 2.5mg/ml; The accurate title, decided the isoborneol standard items, in the 5ml volumetric flask, is made into the standard solution that concentration is 2.5mg/ml with the normal hexane constant volume; The accurate title, decided the borneol standard items, in the 5ml volumetric flask, is made into the standard solution that concentration is 3.0mg/ml with the normal hexane constant volume.
C. the preparation of object of reference solution: precision takes by weighing pentadecane, is settled to 250ml with normal hexane, and getting concentration is the inner mark solution of 0.80mg/ml.
D. the preparation of need testing solution: the accurate random sample article of claiming, be dissolved in surely in the 5ml volumetric flask with normal hexane, be made into the standard solution that concentration is 1.0mg/ml.
E. get need testing solution 1 μ l, inject gas chromatograph writes down 1 hour chromatogram.
4) standard cape jasmine determining fingerprint pattern
A. chromatographic condition and system suitability test: chromatographic column: DB-5MS capillary column, 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1.0ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 50 ℃ (5min) 4 ℃/min240 ℃ (5min); Sample size: 1 μ l.
B. the preparation of object of reference solution: precision takes by weighing pentadecane 0.020g and is settled to 250ml with normal hexane, as inner mark solution.
C. the preparation of need testing solution: get the cape jasmine sample and be ground into meal, sampling 20.0 grams are put in the round-bottomed flask; Add distilled water 200ml; Place after 12 hours, add the 3ml normal hexane, in electric jacket with volatile oil extractor heating and extracting 8 hours; Collect the normal hexane sample solution and be settled to 5ml, add anhydrous sodium sulfate dehydration to clarification.Precision is measured cape jasmine normal hexane sample solution 1.00ml, adds inner mark solution 1.00ml, gets need testing solution.
D. determination method: the material need testing solution 1 μ l that gets it filled, inject gas chromatograph, record 1h chromatogram.
5) Xingnaojing injection intermedium determining fingerprint pattern:
A. chromatographic condition and system suitability test: WAX capillary column; 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 50 ℃ of 220 ℃ of (5min) 4 ℃/min (12min).
B. the preparation of object of reference solution is got the 0.0050g dodecane and is settled in the 50ml volumetric flask with normal hexane, promptly gets, as inner mark solution
C. the accurate Xingnaojing injection intermedium sample 10ml that draws of the preparation of need testing solution puts in the round-bottomed flask, adds distilled water 200ml; Zeolite a little, normal hexane 2ml, in electric jacket with volatile oil extractor heating and extracting 5 hours; Collect normal hexane and be settled to 5ml, add anhydrous sodium sulfate dehydration to clarification, extracting sample solution 1.00ml adds dodecane inner mark solution 1.00ml; Mixing promptly gets.
D. determination method: get need testing solution 1 μ l, inject gas chromatograph, record 1h chromatogram.
6) Xingnaojing injection determining fingerprint pattern:
A. chromatographic condition and system suitability test: WAX capillary column; 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 50 ℃ of 220 ℃ of (5min) 4 ℃/min (12min).
B. the preparation of object of reference solution: get the 0.0050g dodecane and be settled in the 50ml volumetric flask, promptly get, as inner mark solution with normal hexane.
C. the preparation of need testing solution: the accurate Xingnaojing injection sample 10ml that draws, put in the round-bottomed flask, add distilled water 200ml; Zeolite a little, normal hexane 2ml, in electric jacket with volatile oil extractor heating and extracting 5 hours; Collect normal hexane and be settled to 5ml, add anhydrous sodium sulfate dehydration to clarification, extracting sample solution 1.00ml adds dodecane inner mark solution 1.00ml; Mixing promptly gets.
D. determination method: get need testing solution 1 μ l, inject gas chromatograph, record 1h chromatogram.
At last the finger-print of intermedium and finished product and the finger-print of standard items are compared, the person of meeting is specification product, and the person of not meeting is a substandard product.
Advantage of the present invention is: method of quality control precision, sensitivity, stability are all good, guarantee " safety, the homogeneous, stable, effective, controlled " of product quality.Make this drug manufacture standardization, reach determined curative effect, steady quality, the advanced reasonably purpose of technology.
Below in conjunction with accompanying drawing and embodiment the present invention is done further narration; So that the public has more deep understanding to summary of the invention; Be not limitation of the present invention, all any this areas of carrying out according to the disclosure of invention are equal to replacement, all belong to protection scope of the present invention.
Description of drawings
Fig. 1 is a standard Moschus finger-print
Fig. 2 is a standard root tuber of aromatic turmeric finger-print
Fig. 3 is a standard borneol finger-print
Fig. 4 is a standard cape jasmine finger-print
Embodiment
Below in conjunction with embodiment the present invention is done explanation further, so that the present invention is done understanding in more detail.The following stated is merely in order to explain the preferred embodiments of the present invention, is not according to this present invention to be done any pro forma restriction, so every any form of on creation spirit of the present invention basis, being done is modified or change, all should belong to protection category of the present invention.
1.1 instrument and reagent
Gas chromatograph island Tianjin GC15-A, the C-R4A integraph.
Normal hexane (analyzing pure), anhydrous sodium sulfate (analyzing pure), volatile oil extractor (Beijing Glass Implement Factory).Dodecane: chromatographically pure, the chemical company limited of Chinese-foreign joint green Specific, lot number: 950824.
Ten a collection of different places of production RADIX CURCUMAEs: provided by mountain, Wuxi City, Jiangsu Province standing grain medicine company, gather the date: be that Yan Yuning professor identify by this school crude drug in January, 2003.
The preparation of inner mark solution: get the 0.03267g dodecane and be settled in the 50ml volumetric flask, promptly get, as inner mark solution with normal hexane.
1.2 the investigation of analysis condition
Get the RADIX CURCUMAE sample and be ground into meal, 20.0 grams of taking a sample are respectively put in the round-bottomed flask; Add distilled water 200ml; Place after 12 hours, add the 3ml normal hexane, in electric jacket, extracted respectively 2,4,6,8,10 hours with the volatile oil extractor heating; Collect hexane solution and be settled in the 5ml volumetric flask the extremely clarification of adding anhydrous sodium sulfate dehydration.Precision is measured 1.00ml normal hexane sample solution, with 1.00ml inner mark solution mixing, and as need testing solution, sample introduction 1 μ l.With maximum peak area in the chromatogram is index, and experimental result shows that extraction time should be 6 hours and gets final product.
Constant temperature continued one hour after temperature programme rose to 220 ℃, in 60 minutes, did not see other peaks.Experimental result shows that this heating schedule can make all compositions in the RADIX CURCUMAE volatile oil flow out pillar, can be used for the analysis of RADIX CURCUMAE volatile oil composition.
1.3GC analysis condition
GC analysis condition: chromatographic column: ALLTECH-WAX capillary column; 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 50 ℃ of 90 ℃ of 220 ℃ of (5min) 2 ℃/min of (5min) 4 ℃/min (6min); Sample introduction: 1 μ l.
1.4 specimen preparation
11 batches in RADIX CURCUMAE sample is got the RADIX CURCUMAE sample and is ground into meal, 20.0 grams of taking a sample respectively; Put in the round-bottomed flask, add distilled water 200ml, place after 12 hours; Add the 3ml normal hexane; Put in the electric jacket with volatile oil extractor heating and extracting 6 hours, collect normal hexane and also be settled in the 5ml volumetric flask, add anhydrous sodium sulfate dehydration to clarification.Precision is measured the 1.00ml normal hexane, with 1.00ml inner mark solution mixing, and as need testing solution, sample introduction 1 μ l.
According to the fingerprint image of ten different places of production RADIX CURCUMAEs, find 20 total peaks.
With these 20 total peaks as standard root tuber of aromatic turmeric finger-print.
The discriminating of root tuber of aromatic turmeric in the Xingnaojing injection intermedium:
A. chromatographic condition and system suitability test: WAX capillary column; 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 50 ℃ of 220 ℃ of (5min) 4 ℃/min (12min).
B. the preparation of object of reference solution is got the 0.0050g dodecane and is settled in the 50ml volumetric flask with normal hexane, promptly gets, as inner mark solution
C. the accurate Xingnaojing injection intermedium sample 10ml that draws of the preparation of need testing solution puts in the round-bottomed flask, adds distilled water 200ml; Zeolite a little, normal hexane 2ml, in electric jacket with volatile oil extractor heating and extracting 5 hours; Collect normal hexane and be settled to 5ml, add anhydrous sodium sulfate dehydration to clarification, extracting sample solution 1.00ml adds dodecane inner mark solution 1.00ml; Mixing promptly gets.
D. determination method: get need testing solution 1 μ l, inject gas chromatograph, record 1h chromatogram.
The employing software for calculation compares, and test sample finger-print and standard root tuber of aromatic turmeric finger-print similarity are greater than 0.95.
The discriminating of root tuber of aromatic turmeric in the Xingnaojing injection
A. chromatographic condition and system suitability test: WAX capillary column; 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 50 ℃ of 220 ℃ of (5min) 4 ℃/min (12min).
B. the preparation of object of reference solution: get the 0.0050g dodecane and be settled in the 50ml volumetric flask, promptly get, as inner mark solution with normal hexane.
C. the preparation of need testing solution: the accurate Xingnaojing injection sample 10ml that draws, put in the round-bottomed flask, add distilled water 200ml; Zeolite a little, normal hexane 2ml, in electric jacket with volatile oil extractor heating and extracting 5 hours; Collect normal hexane and be settled to 5ml, add anhydrous sodium sulfate dehydration to clarification, extracting sample solution 1.00ml adds dodecane inner mark solution 1.00ml; Mixing promptly gets.
D. determination method: get need testing solution 1 μ l, inject gas chromatograph, record 1h chromatogram.
The employing software for calculation compares, and test sample finger-print and standard root tuber of aromatic turmeric finger-print similarity are greater than 0.95.
Claims (1)
1. the detection method of an XINGNAOJING ZHUSHEYE comprises following content: the observation of proterties, and the discriminating of content, the inspection of content, finger-print relatively carries out assay to the composition that contains,
Wherein, said finger-print relatively may further comprise the steps:
1) the mensuration a. chromatographic condition and the system suitability test of standard Moschus finger-print: WAX capillary column; Thickness 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 3: 1; Fid detector temperature: 270 ℃; Injector temperature: 270 ℃; Column temperature: 240 ℃ of 30min of 4 ℃/min of 200 ℃ of 0min of 10 ℃/min of 50 ℃ of 5min; B. the preparation of object of reference solution: get the 0.025g heptadecane and be settled in the 50ml volumetric flask, promptly get, as inner mark solution with normal hexane; C. the preparation of need testing solution: precision takes by weighing Moschus medicinal material 40mg, to 500ml round-bottomed flask flask, adds distilled water 200ml; Normal hexane 2ml,, in electric jacket, extract 4h respectively with the volatile oil extractor heating;, collect hexane solution to the 5ml volumetric flask, the accurate inner mark solution 1ml that adds; And be settled to scale with normal hexane, as need testing solution; D. determination method: get each batch medicinal material need testing solution 2 μ l respectively, inject gas chromatograph, record 1h chromatogram;
2) standard root tuber of aromatic turmeric determining fingerprint pattern a. chromatographic condition and system suitability test: WAX capillary column; 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 220 ℃ of 6min of 2 ℃/min of 90 ℃ of 5min of 4 ℃/min of 50 ℃ of 5min; Sample size: 1 μ l; B. the preparation of object of reference solution: get the 0.035g dodecane and be settled in the 500ml volumetric flask, promptly get, as inner mark solution with normal hexane; C. the preparation of need testing solution: get the RADIX CURCUMAE sample and be ground into meal, 20.0 grams of taking a sample are respectively put in the round-bottomed flask; Add distilled water 200ml, place after 12 hours, add the 3ml normal hexane; Put in the electric jacket with volatile oil extractor heating and extracting 8 hours, collect normal hexane and also be settled in the 5ml volumetric flask, add anhydrous sodium sulfate dehydration to clarification; Precision is measured 1.00ml normal hexane sample solution, with 1.00ml inner mark solution mixing, as need testing solution; D. determination method: get need testing solution 1 μ l, inject gas chromatograph writes down 1 hour chromatogram;
3) standard borneol determining fingerprint pattern a. chromatographic column: WAX capillary column 30m * 0.25mm * 0.25 μ m; Injector temperature: 200 ℃; Fid detector temperature: 200 ℃; Carrier gas: high pure nitrogen; Flow velocity 1ml/min; Split ratio: 40: 1; Column temperature: 170 ℃ of 7 ℃/min of 100 ℃ of 5min; Internal standard compound: octadecane; B. the camphor standard items decided in the accurate title of the preparation of standard solution, is dissolved in surely in the 5ml volumetric flask with normal hexane, is made into the standard solution that concentration is 2.5mg/ml; The accurate title, decided the isoborneol standard items, in the 5ml volumetric flask, is made into the standard solution that concentration is 2.5mg/ml with the normal hexane constant volume; The accurate title, decided the borneol standard items, in the 5ml volumetric flask, is made into the standard solution that concentration is 3.0mg/ml with the normal hexane constant volume; C. the preparation of object of reference solution: precision takes by weighing pentadecane, is settled to 250ml with normal hexane, and getting concentration is the inner mark solution of 0.80mg/ml; D. the preparation of need testing solution: the accurate random sample article of claiming, be dissolved in surely in the 5ml volumetric flask with normal hexane, be made into the standard solution that concentration is 1.0mg/ml; E. get need testing solution 1 μ l, inject gas chromatograph writes down 1 hour chromatogram;
4) standard cape jasmine determining fingerprint pattern a. chromatographic condition and system suitability test: chromatographic column: DB-5MS capillary column, 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1.0ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 50 ℃ 5min4 ℃/min240 ℃ 5min; Sample size: 1 μ l; B. the preparation of object of reference solution: precision takes by weighing pentadecane 0.020g and is settled to 250ml with normal hexane, as inner mark solution; C. the preparation of need testing solution: get the cape jasmine sample and be ground into meal, sampling 20.0 grams are put in the round-bottomed flask; Add distilled water 200ml, place after 12 hours, add the 3ml normal hexane; In electric jacket,, collect the normal hexane sample solution and also be settled to 5ml, add anhydrous sodium sulfate dehydration to clarification with volatile oil extractor heating and extracting 8 hours; Precision is measured cape jasmine normal hexane sample solution 1.00ml, adds inner mark solution 1.00ml, gets need testing solution; D. determination method: the material need testing solution 1 μ l that gets it filled, inject gas chromatograph, record 1h chromatogram;
5) Xingnaojing injection intermedium determining fingerprint pattern: a. chromatographic condition and system suitability test: WAX capillary column; 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 220 ℃ of 12min of 4 ℃/min of 50 ℃ of 5min; B. the preparation of object of reference solution is got the 0.0050g dodecane and is settled in the 50ml volumetric flask with normal hexane, promptly gets, as inner mark solution; C. the accurate Xingnaojing injection intermedium sample 10ml that draws of the preparation of need testing solution puts in the round-bottomed flask, adds distilled water 200ml; Zeolite a little, normal hexane 2ml, in electric jacket with volatile oil extractor heating and extracting 5 hours; Collect normal hexane and be settled to 5ml, add anhydrous sodium sulfate dehydration to clarification, extracting sample solution 1.00ml adds dodecane inner mark solution 1.00ml; Mixing promptly gets; D. determination method: get need testing solution 1 μ l, inject gas chromatograph, record 1h chromatogram;
6) Xingnaojing injection determining fingerprint pattern: a. chromatographic condition and system suitability test: WAX capillary column; 30m * 0.25mm * 0.25 μ m; Carrier gas: high pure nitrogen; Flow velocity: 1ml/min; Split ratio: 20: 1; Fid detector temperature: 250 ℃; Injector temperature: 250 ℃; Column temperature: 220 ℃ of 12min of 4 ℃/min of 50 ℃ of 5min; B. the preparation of object of reference solution: get the 0.0050g dodecane and be settled in the 50ml volumetric flask, promptly get, as inner mark solution with normal hexane; C. the preparation of need testing solution: the accurate Xingnaojing injection sample 10ml that draws, put in the round-bottomed flask, add distilled water 200ml; Zeolite a little, normal hexane 2ml, in electric jacket with volatile oil extractor heating and extracting 5 hours; Collect normal hexane and be settled to 5ml, add anhydrous sodium sulfate dehydration to clarification, extracting sample solution 1.00ml adds dodecane inner mark solution 1.00ml; Mixing promptly gets; D. determination method: get need testing solution 1 μ l, inject gas chromatograph, record 1h chromatogram.
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| CN105548385B (en) * | 2015-12-09 | 2017-12-05 | 无锡济民可信山禾药业股份有限公司 | The assay method and its standard finger-print of XINGNAOJING ZHUSHEYE liquid-phase fingerprint |
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| CN107688072B (en) * | 2016-08-05 | 2021-06-29 | 河南天地药业股份有限公司 | Detection method of Xingnaojing injection |
| CN107091893B (en) * | 2017-05-26 | 2019-06-11 | 浙江中医药大学 | The measuring method of multi-target ingredient content in a kind of XINGNAOJING ZHUSHEYE or in which mesosome |
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| CN107907611B (en) * | 2017-11-14 | 2019-11-05 | 大理药业股份有限公司 | A kind of cape jasmine quality evaluating method for XINGNAOJING ZHUSHEYE |
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| CN109239249B (en) * | 2018-09-27 | 2020-09-25 | 无锡济民可信山禾药业股份有限公司 | Method for measuring gas-phase fingerprint of Xingnaojing injection and standard gas-phase fingerprint thereof |
| CN109212102B (en) * | 2018-11-12 | 2021-07-30 | 福建省粮油质量监测所 | Method for identifying gardenia oil based on characteristic component gas chromatography-mass spectrum fingerprint |
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