CN102706984A - Method for determining ephedrine hydrochloride content in lung-clearing inflammation pill by high-performance liquid phase - Google Patents
Method for determining ephedrine hydrochloride content in lung-clearing inflammation pill by high-performance liquid phase Download PDFInfo
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Abstract
The invention relates to a method for determining ephedrine hydrochloride content in a lung-clearing inflammation pill by a high-performance liquid phase, wherein the chromatographic condition mobile phase is acetonitrile and 0.02mol/L of monopotassium phosphate solution with pH2.7; the volume ratio is 4:96; the detection wavelength is 207nm; the flow speed is 1.0ml/min; the chromatographic column is Dikma 5mumC184.6*250mm, and the column temperature is 30 DEG C. The separating effect of ephedrine hydrochloride and pseudoephedrine hydrochloride peak is good under a flow phase condition; the quantity of the theoretical plates is 6976 according to the ephedrine hydrochloride peak, and 1g of the product contains ephedrine hydrochloride (C10H15NO.HCl) being not less than 0.65mg. According to the determination method disclosed by the invention, the controllability of content standard of the drug is improved; the internal content of the product is ensured, and the method has significance in the aspects of promoting product sales, increasing the market competitiveness of the product and ensuring the medication safety of a patient.
Description
Technical field
The invention belongs to the Chinese medicine preparation technical field, relate to the quality determining method of Chinese patent drug, a kind of method that adopts high performance liquid chromatogram to measure ephedrine hydrochloride content in the lung-clearing anti-inflammatory ball of more specifically saying so.
Background technology
In China, the science of identification of Chinese materia medica is a comparatively traditional Test on Traditional Chinese Medicine technology, follows the development of China's theory of traditional Chinese medical science and progressively ripe.Many identification methods are being brought into play its peculiar advantage gradually aspect the traditional Chinese medicine quality check.There were 59 kinds of medicinal materials and 50 kinds of clinical Chinese patent drugs to choose high performance liquid chromatography in 2000 in the middle of the version pharmacopeia in China and test, simultaneously the also increasing traditional Chinese medicine ingredients analysis field that is applied to of high performance liquid chromatography.In middle pharmacology, change identification method, the application of high performance liquid chromatography HPLC is relatively extensive.High performance liquid chromatography has rapidly, quick, the more high relatively many advantages of separation efficiency.When Chinese medicine is tested; After High performance liquid chromatography is separated the singularity composition; Through UV-detector or mass detector Chinese medicine is carried out the analysis of structure and related fields such as quantitative again, can make rational evaluation the quality of Chinese medicine.Adopt high-efficient liquid phase technique to be used for the drug safety of the quality testing of Chinese patent drug, with having very big practical application meaning to the guarantee people.
The lung-clearing anti-inflammatory ball is a kind of traditional Chinese medicines preparation, and it is made up of Chinese ephedra, gypsum, earthworm, great burdock achene, lepidium seed, calculus bovis factitius, semen armeniacae amarae (stir-fry), antelope's horn.Be mainly used in clearing lung and eliminating phlegm, relieving cough and asthma.Be used for pulmonary retention of phlegmopyrexia, cough and asthma, distending pain in the chest and hypochondrium, it is yellow thick to spit, the acute attack of the infection of the upper respiratory tract, acute bronchitis and chronic bronchitis, and the cough phlegm that pulmonary infection causes is thick, the illness such as out of breath of panting.In the version pharmacopeia in 2005, use wherein Determination of Ephedrine Hydrochloride of tlc scanning determination in the lung-clearing anti-inflammatory ball.But the reappearance of thin layer chromatography scanning is relatively poor relatively.
Summary of the invention
The shortcoming that the objective of the invention is to overcome prior art is with not enough; A kind of method that adopts high performance liquid chromatogram to measure ephedrine hydrochloride content in the lung-clearing anti-inflammatory ball is provided; Wherein the lung-clearing anti-inflammatory ball is made up of Chinese ephedra 250g, gypsum 750g, earthworm 750g, great burdock achene 250g, lepidium seed 250g, calculus bovis factitius 100g, semen armeniacae amarae (stir-fry) 60g, antelope's horn 30g eight flavor medicines, by following step Determination of Ephedrine Hydrochloride is measured:
(1) preparation of testing liquid:
1) preparation of reference substance solution: it is an amount of to get the ephedrine hydrochloride reference substance, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 15 μ g, promptly gets;
2) preparation of need testing solution: get these article, porphyrize is got about 2g; The accurate title, decide, and adds 5mol/L sodium hydroxide solution 120ml, sodium chloride 7.5g, sonicated 10 minutes; Keep little distillation down of boiling, collect distillate 90-98ml, be preferably near 95ml with filling 0.5mol/L hydrochloric acid solution 5ml measuring bottle in advance; Add water to scale, shake up, promptly get;
3) preparation of negative controls: do not contain the sample of Chinese ephedra by prescription and prepared, press the test sample preparation method and prepare;
(2) chromatographic condition
Moving phase: the potassium dihydrogen phosphate of acetonitrile-0.02mol/L pH2.7, its volume ratio are 4:96;
The detection wavelength is: 207nm;
Flow velocity is: 1.0ml/min
Chromatographic column is: enlightening horse 5 μ mC
184.6 * 250mm;
Column temperature is: 35 ℃;
Theoretical cam curve is calculated as 3000 by the ephedrine hydrochloride peak; Hydrochloric ephedrine (the C of the every 1g of these article
10H
15NO.HCl), must not be less than 0.65mg; Wherein said article refer to: the lung-clearing anti-inflammatory ball.
Assay method of the present invention can detect the lung-clearing anti-inflammatory ball.
The high-efficient liquid phase determining method that the present invention adopts is found out suitable chromatographic condition through test, makes ephedrine hydrochloride and pseudoephedrine hydrochloride peak good separating effect in the lung-clearing anti-inflammatory ball, and theoretical cam curve is calculated as 3000 by the ephedrine hydrochloride peak.The hydrochloric ephedrine of the every 1g of these article (C10H15NO.HCl) must not be less than 0.65mg.
The more detailed assay method of the present invention:
1. assay:
The lung-clearing anti-inflammatory ball is made up of Chinese ephedra, gypsum, earthworm, great burdock achene, lepidium seed, calculus bovis factitius, semen armeniacae amarae (stir-fry), antelope's horn eight flavor medicines, and its epheday intermedia is monarch drug in a prescription.Ephedrine is the effective constituent in the Chinese ephedra, " Chinese ephedra " assay of version pharmacopeia in 2005 item down income just be to use the high effective liquid chromatography for measuring Determination of Ephedrine Hydrochloride.Use wherein Determination of Ephedrine Hydrochloride of tlc scanning determination in the lung-clearing anti-inflammatory ball statutory standards.Because the reappearance of thin layer chromatography scanning is relatively poor relatively, use Determination of Ephedrine Hydrochloride in the high effective liquid chromatography for measuring lung-clearing anti-inflammatory ball so intend.The row method of going forward side by side is learned research and checking.
1.1 the preparation of testing liquid
The preparation of reference substance solution:It is an amount of to get the ephedrine hydrochloride reference substance, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 15 μ g, promptly gets.
The preparation of need testing solution:These article of getting, porphyrize is got about 2g, and accurate the title, decide; Add 5mol/L sodium hydroxide solution 120ml, sodium chloride 7.5g, sonicated 10 minutes, distillation (keeping little boiling) is collected the nearly 95ml of distillate with the 100ml measuring bottle that fills 0.5mol/L hydrochloric acid solution 5ml in advance; Add water to scale, shake up, promptly get.
The preparation of negative controls: do not contain the sample of Chinese ephedra by prescription and prepared, press the test sample preparation method and prepare.
1.2 chromatographic condition
Moving phase: acetonitrile-0.02mol/L potassium dihydrogen phosphate (phosphoric acid adjust pH to 2.7) (4:96)
Detect wavelength: 207nm
Flow velocity: 1.0ml/min
Chromatographic column: enlightening horse 5 μ mC
184.6 * 250mm
Column temperature: 35 ℃
1.3 confirming of chromatographic condition
1.3.1 the selection of moving phase
Grope to choose acetonitrile-0.02mol/L potassium dihydrogen phosphate (phosphoric acid adjust pH to 2.7) through experiment and (4:96) be the mobile condition of these article assay item.Under this moving phase condition, ephedrine hydrochloride and pseudoephedrine hydrochloride peak good separating effect, theoretical cam curve is calculated as 3000 by the ephedrine hydrochloride peak.Hydrochloric ephedrine (the C of the every 1g of these article
10H
15NO.HCl), must not be less than 0.65mg.
1.3.2 confirming of pre-treating method
The ephedrine hydrochloride maximum absorption wavelength is less, in compound preparation, disturbs more.Utilize free ephedrine to have the advantages that to be prone to distillation, adopt the way of distillation that sample is handled, the test sample that obtains is measured noiseless, the good separating effect of ephedrine hydrochloride.
Add 5mol/L sodium hydroxide solution 80ml, 120m, 140ml respectively, investigate the ephedrine hydrochloride rate of transform, the result sees table 1.
Table 1 adds the different volumes sodium hydroxide solution and extracts Determination of Ephedrine Hydrochloride
| Sodium hydroxide solution volume (ml) | 80 | 120 | 140 |
| Ephedrine hydrochloride content (g) | 0.837 | 0.857 | 0.817 |
Visible by table 1, when the sodium hydroxide solution volume is 120ml, the extraction ratio of the extraction ratio of ephedrine hydrochloride ephedrine hydrochloride during a little more than 80ml, 140ml.So the sodium hydroxide solution optimum addition is 120ml.
1.4 specificity test
Get reference substance solution 10 μ l, inject liquid chromatograph, measure according to above-mentioned chromatographic condition, the record chromatogram, the result sees Fig. 1.
Get need testing solution 10 μ l, inject liquid chromatograph, measure according to above-mentioned chromatographic condition, the record chromatogram, the result sees Fig. 2.
Get negative sample solution 10 μ l, inject liquid chromatograph, measure according to above-mentioned chromatographic condition, the record chromatogram, the result sees Fig. 3.
The result shows, in the test sample chromatogram with the reference substance chromatogram on identical retention time corresponding chromatographic peak is arranged, peak shape is good.According to formula n=5.54 (t
R/ W
H/2)
2Calculate, the theoretical cam curve of chromatographic column is 6976.
According to formula R=2 (t
R2--t
R1)/(W
1+ W
2) calculate, degree of separation is 2.0.
In the negative sample chromatogram, do not have chromatographic peak, explain that this method specificity is good in identical retention time, negative noiseless.
1.5 linear test
Precision takes by weighing ephedrine hydrochloride reference substance 20.80mg, puts in the 25ml measuring bottle, adds methyl alcohol to scale, shakes up, and obtains the reference substance storing solution of 0.8320mg/ml.Precision pipettes the reference substance storing solution and is diluted to the reference substance solution that concentration is 3.798 μ g/ml, 7.956 μ g/ml, 15.912 μ g/ml, 31.824 μ g/ml, 63.648 μ g/ml, 79.56 μ g/ml respectively.With reference substance storing solution and reference substance solution difference sample introduction 10 μ l, measure peak area according to the chromatographic condition of working out, the result sees table 2.
The linear result that investigates of table 2
| Sample size (μ g) | Peak area | Average peak area |
| 0.03798 | 81568 | 82254.5 |
| ? | 82941 | ? |
| 0.07956 | 184013 | 183095.5 |
| ? | 182178 | ? |
| 0.15912 | 381569 | 381762 |
| ? | 381955 | ? |
| 0.31824 | 768556 | 767877.5 |
| ? | 767199 | ? |
| 0.63648 | 1512918 | 1517812 |
| ? | 1522706 | ? |
| 0.7956 | 1874063 | 1877379.5 |
| ? | 1880696 | ? |
Ephedrine hydrochloride peak area and sample size are carried out linear regression processing, get regression equation:
y?=?2373449.6?x?-125.66 r?=0.9999
With the sample size is that the corresponding peak area of horizontal ordinate is an ordinate, drawing standard curve such as Fig. 4.
The result shows that ephedrine hydrochloride is good linear relationship between sample size 0.03798 μ g ~ 0.7956 μ g.
1.6 repeatability
These article of getting (lot number I0001) porphyrize is got about 2g, and accurate the title decides, and presses a need testing solution preparation preparation down, gets need testing solution 10 μ l injecting chromatographs, presses above-mentioned chromatographic condition and measures 6 times, and the result sees table 3.
Table 3 replica test result
Calculate according to test findings, RSD is 0.29%, meets the requirements, and shows that chromatograph repeatability under this condition is good.
1.7 reappearance test
These article of getting (lot number I0001) porphyrize is got about 2g, and accurate the title decides, and presses a need testing solution preparation preparation down, parallel 6 parts.Measure by the condition determination sample introduction of drafting 10 μ l, calculate relative standard deviation.The result sees table 4.
Table 4 reproducible test results
The result shows: the average content of sample ephedrine hydrochloride is 0.8526mg/g
,Relative standard deviation is 1.46%, meets the requirements.
1.8 accuracy test
These article of getting (lot number I0001, average content 0.8526mg/g), porphyrize; Get about 1g, the accurate title, decide, accurate respectively ephedrine hydrochloride reference substance methanol solution (0.7956mg/ml) 1ml that adds; Parallel 6 parts, press a need testing solution preparation preparation down, measure by the condition determination of drafting; Calculate recovery rate and relative standard deviation, the result sees table 5.
Table 5 accuracy test result
Test findings shows that the average recovery rate of this method is 99.24%, and relative standard deviation is 0.96%, proves that this method accuracy is good.
1.9 stability test
These article of getting (lot number I0001) porphyrize is got about 2g, and accurate the title decides; Press a need testing solution preparation preparation down; Measure the ephedrine hydrochloride peak area at the 0th, 1,2,4,6,8,10,12 hour sample introduction 10 μ l respectively by the condition determination of drafting, calculate relative standard deviation, the result sees table 6.
Table 6 stability test result
Test findings shows that need testing solution is good at 12 hours internal stabilities.
1.10 serviceability test
These article of getting (lot number I0001) porphyrize is got about 2g, and accurate the title decides, and presses a need testing solution preparation preparation down, uses the chromatographic column of different octadecylsilane chemically bonded silicas as filling agent respectively by the condition determination of drafting, and the result sees table 7.
Table 7 serviceability test result
Visible by test findings, use the chromatographic column of different octadecylsilane chemically bonded silicas as filling agent, peak type and degree of separation are good, and it is unaffected basically to measure the result, this method good tolerance.
1.11 Determination of Ephedrine Hydrochloride is measured in the sample
According to said method, measure Determination of Ephedrine Hydrochloride in the 3 lot sample article.The result sees table 8.
Table 83 lot sample article assay results
1.12 the formulation of content limit
According to ephedrine hydrochloride content in the Chinese ephedra medicinal material, calculate the finished product content limit.
1, ephedrine hydrochloride content situation analysis in the Chinese ephedra medicinal material
The content assaying method that adopts the lung-clearing anti-inflammatory ball to draft is measured ten batches of Chinese ephedra medicinal materials, and the result sees table 9.
Table 9 Chinese ephedra medicinal material assay result
| Sequence number | Ephedrine hydrochloride (%) | Pseudoephedrine hydrochloride (%) | Fiber crops+puppet fiber crops (%) | Fiber crops: pseudo-fiber crops |
| 1 | 1.08 | 0.4 | 1.48 | 2.70 |
| 2 | 0.91 | 0.38 | 1.29 | 2.39 |
| 3 | 0.87 | 0.36 | 1.23 | 2.42 |
| 4 | 0.94 | 0.32 | 1.26 | 2.94 |
| 5 | 1.18 | 0.37 | 1.55 | 3.19 |
| 6 | 1.52 | 0.45 | 1.97 | 3.38 |
| 7 | 0.93 | 0.35 | 1.28 | 2.66 |
| 8 | 0.93 | 0.38 | 1.31 | 2.45 |
| 9 | 0.92 | 0.37 | 1.29 | 2.49 |
| 10 | 0.94 | 0.34 | 1.28 | 2.77 |
| On average | 1.02 | 0.37 | 1.39 | 2.74 |
The assay result shows that the ratio of ephedrine hydrochloride and pseudoephedrine hydrochloride is 2.39 ~ 3.38; With reference to a Chinese ephedra medicinal material of version pharmacopeia in 2005 content limit was 1.0% (ephedrine hydrochloride and pseudoephedrine hydrochloride add up to), and then ephedrine hydrochloride content is 0.71% ~ 0.77% in the Chinese ephedra medicinal material.
2, the confirming of ephedrine hydrochloride in the lung-clearing anti-inflammatory ball
Prescription epheday intermedia accounts for 10.2% of total preparation prescription amount, because the lung-clearing anti-inflammatory ball is that former powder is used as medicine, the rate of transform is calculated by 90%, and it is tentative for the hydrochloric ephedrine of the every 1g of these article (C10H15NO.HCl) with its content limit, must not be less than 0.65mg.
Description of drawings:
Fig. 1 is an ephedrine hydrochloride reference substance chromatogram;
Fig. 2 is lung-clearing anti-inflammatory ball sample chromatogram figure;
Fig. 3 is a Chinese ephedra negative sample chromatogram;
Fig. 4 is a canonical plotting.
Below in conjunction with embodiment, the present invention is further specified, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.All Chinese crude drugs and reference substance all have commercially available.
Embodiment 1
Prescription:
750 parts of 750 parts of earthworms of 250 parts of gypsum of Chinese ephedra
100 parts of 250 parts of cow-bezoars of great burdock achene 250 lepidium seeds
30 parts of 60 parts of antelope's horns of semen armeniacae amarae (stir-fry)
The preparation method:
More than eight the flavor, except that calculus bovis factitius, Cornu Saigae Tataricae powder is broken into impalpable powder, Six-elements such as all the other Chinese ephedras are ground into fine powder, with above-mentioned antelope's horn and calculus bovis factitius powder facing-up, mixing sieves.Every 100g powder adds an amount of water pill with refined honey 60 ~ 80g, processes water-honeyed pill; Or use water pill, and making the water-bindered pill, drying promptly gets.
Embodiment 2
(1) preparation of testing liquid:
1) preparation of reference substance solution: it is an amount of to get the ephedrine hydrochloride reference substance, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 30 μ g, promptly gets;
2) preparation of need testing solution: get the lung-clearing anti-inflammatory ball, porphyrize is got about 2g; The accurate title, decide, and adds 5mol/L sodium hydroxide solution 120ml, sodium chloride 7.5g, sonicated 10 minutes; Keep little distillation down of boiling, collect distillate 90-98ml, add water to scale with filling 0.5mol/L hydrochloric acid solution 5ml measuring bottle in advance; Shake up, promptly get;
3) preparation of negative controls: do not contain the sample of Chinese ephedra by prescription and prepared, press the test sample preparation method and prepare;
(2) chromatographic condition
Moving phase: the potassium dihydrogen phosphate of acetonitrile-0.02mol/L pH2.7, its volume ratio are 4:96;
The detection wavelength is: 207nm;
Flow velocity is: 1.0ml/min
Chromatographic column is: enlightening horse 5 μ mC
184.6 * 250mm;
Column temperature is: 35 ℃; Theoretical cam curve is calculated as 3000 by the ephedrine hydrochloride peak; The hydrochloric ephedrine of the every 1g of these article (C10H15NO.HCl) 0.65mg.
Embodiment 3
(1) preparation of testing liquid:
1) preparation of reference substance solution: it is an amount of to get the ephedrine hydrochloride reference substance, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 30 μ g, promptly gets;
2) preparation of need testing solution: get the lung-clearing anti-inflammatory ball, porphyrize is got about 2g; The accurate title, decide, and adds 5mol/L sodium hydroxide solution 80ml, sodium chloride 7.5g, sonicated 10 minutes; Keep little distillation down of boiling, collect distillate 90-98ml, add water to scale with filling 0.5mol/L hydrochloric acid solution 5ml measuring bottle in advance; Shake up, filter, promptly get through 0.45 μ m miillpore filter;
3) preparation of negative controls: do not contain the sample of Chinese ephedra by prescription and prepared, press the test sample preparation method and prepare;
(2) chromatographic condition
Moving phase: the potassium dihydrogen phosphate of acetonitrile-0.02mol/L pH2.7, its volume ratio are 4:96;
The detection wavelength is: 207nm;
Flow velocity is: 1.0ml/min
Chromatographic column is: enlightening horse 5 μ mC
184.6 * 250mm;
Column temperature is: 35 ℃; Theoretical cam curve is calculated as 3000 by the ephedrine hydrochloride peak; The hydrochloric ephedrine of the every 1g of these article (C10H15NO.HCl), 0.68mg.
Claims (3)
1. method that adopts high performance liquid chromatogram to measure ephedrine hydrochloride content in the lung-clearing anti-inflammatory ball; It is made up of Chinese ephedra 250g, gypsum 750g, earthworm 750g, great burdock achene 250g, lepidium seed 250g, calculus bovis factitius 100g, stir-fry semen armeniacae amarae 60g, antelope's horn 30g eight flavor medicines, it is characterized in that its assay method is undertaken by following step:
(1) preparation of testing liquid:
1) preparation of reference substance solution: it is an amount of to get the ephedrine hydrochloride reference substance, and accurate the title decides, and adds methyl alcohol and processes the solution that every 1ml contains 15 μ g, promptly gets;
2) preparation of need testing solution: get these article, porphyrize is got about 2g; The accurate title, decide, and adds 5mol/L sodium hydroxide solution 80-140ml, sodium chloride 7.5g, sonicated 10 minutes; Distillation is collected distillate 90-98ml with the 100ml measuring bottle that fills 0.5mol/L hydrochloric acid solution 5ml in advance, adds water to scale; Shake up, promptly get;
3) preparation of negative controls: do not contain the sample of Chinese ephedra by prescription and prepared, press the test sample preparation method and prepare;
(2) chromatographic condition
Moving phase: the potassium dihydrogen phosphate of acetonitrile-0.02mol/L pH2.7, its volume ratio are 4:96;
The detection wavelength is: 207nm;
Flow velocity is: 1.0ml/min
Chromatographic column is: enlightening horse 5 μ mC
184.6 * 250mm;
Column temperature is: 35 ℃;
Theoretical cam curve is calculated as 3000 by the ephedrine hydrochloride peak; Hydrochloric ephedrine (the C of the every 1g of these article
10H
15NO.HCl), must not be less than 0.65mg; Wherein said article refer to: the lung-clearing anti-inflammatory ball.
2. the described assay method of claim 1, wherein the distillate collected of measuring bottle is 95ml.
3. the described assay method of claim 1, the amount that wherein adds the 5mol/L sodium hydroxide solution in the need testing solution is 120ml.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954086A (en) * | 2016-04-20 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for extracting ephedrine hydrochloride in lung regulating pill |
| CN106950292A (en) * | 2017-01-17 | 2017-07-14 | 天津中新药业集团股份有限公司达仁堂制药厂 | A kind of lung-clearing anti-inflammatory ball quality standard detecting method |
| CN110095458A (en) * | 2019-06-05 | 2019-08-06 | 公安部禁毒情报技术中心 | The preparation method of crystal methamphetamine urine detection kit quality control test panel |
| CN111830172A (en) * | 2020-07-27 | 2020-10-27 | 广州白云山潘高寿药业股份有限公司 | Quality control method of pinellia ternata syrup |
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| CN1366894A (en) * | 2001-01-22 | 2002-09-04 | 杨孟君 | Nano lung-clearing anti-inflammatory preparation medicine and preparation method thereof |
| CN1554407A (en) * | 2003-12-23 | 2004-12-15 | 天津中新药业集团股份有限公司达仁堂 | Medicine for clearing away lung-heat, eliminating phaegn, reliveing cough and asthma and its preparing method |
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| CN1366894A (en) * | 2001-01-22 | 2002-09-04 | 杨孟君 | Nano lung-clearing anti-inflammatory preparation medicine and preparation method thereof |
| CN1554407A (en) * | 2003-12-23 | 2004-12-15 | 天津中新药业集团股份有限公司达仁堂 | Medicine for clearing away lung-heat, eliminating phaegn, reliveing cough and asthma and its preparing method |
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| 罗辉 等: "HPLC法测定清肺消炎丸中盐酸麻黄碱的含量", 《世界科学技术（中医药现代化）》, vol. 11, no. 3, 31 March 2009 (2009-03-31), pages 461 - 464 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954086A (en) * | 2016-04-20 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for extracting ephedrine hydrochloride in lung regulating pill |
| CN106950292A (en) * | 2017-01-17 | 2017-07-14 | 天津中新药业集团股份有限公司达仁堂制药厂 | A kind of lung-clearing anti-inflammatory ball quality standard detecting method |
| CN110095458A (en) * | 2019-06-05 | 2019-08-06 | 公安部禁毒情报技术中心 | The preparation method of crystal methamphetamine urine detection kit quality control test panel |
| CN111830172A (en) * | 2020-07-27 | 2020-10-27 | 广州白云山潘高寿药业股份有限公司 | Quality control method of pinellia ternata syrup |
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Application publication date: 20121003 |