CN101112424A - Quality control method of asthma tablets - Google Patents
Quality control method of asthma tablets Download PDFInfo
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- CN101112424A CN101112424A CNA2007100778766A CN200710077876A CN101112424A CN 101112424 A CN101112424 A CN 101112424A CN A2007100778766 A CNA2007100778766 A CN A2007100778766A CN 200710077876 A CN200710077876 A CN 200710077876A CN 101112424 A CN101112424 A CN 101112424A
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- ephedrine hydrochloride
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Abstract
The present invention discloses a quality control method of asthma tablets, which includes the flowing steps: (1) chromatography conditions and system suitability experiment; (2) preparation of control solution; (3) preparation of test solution is as following: taking the product, removing the coating, porphyrizing, taking about 1g, placing into a 50ml volumetric flask, adding 1ml of ammonia test solution and 25ml of chloroform precisely, weighing the weight, carrying out the ultrasonic treatment with the power of 260w and the frequency of 40KHz for 30 minutes, cooling, weighing the weight, using the chloroform to supplement the loss weight, shaking evenly, filtering, sucking 5ml of filtrate precisely, adding 2ml of 2 percent hydrochloric ethanol anhydrous, shaking evenly, drying up by evaporation in a water bath, adding 10ml of 0.1percent hydrochloric acid in the residual slag, full dissolving by ultrasound, filtering, and taking the subsequent filtrate; (4) weigh and suck the control solution and the test solution precisely and respectively to inject to an HPLC instrument for determination. The method adopts the HPLC to carry out the content determination of morphine, codeine phosphate and ephedrine hydrochloride in the prescription under a same system, which can not only ensure the efficacy of the products, but can also enable the quality of the products to be stable.
Description
Technical field
The invention belongs to the field of quality control of Chinese medicine preparation, particularly the method for quality control of xiaochuan pian.
Background technology
Xiaochuan pian is made up of Pericarpium Papaveris, Radix Platycodonis, Herba Ephedrae, Radix Glycyrrhizae four Chinese medicine thing, has the relieving cough and relieving asthma effect, is used for cough, asthma.Pericarpium Papaveris and Herba Ephedrae are principal agents in the prescription, are mainly used in treatment cough, asthma.And morphine is one of effective ingredient in the prescription in the Pericarpium Papaveris, but also has stronger addiction simultaneously, ephedrine hydrochloride also effective ingredient in the side of belonging to simultaneously in codeine phosphate and the Herba Ephedrae in the Pericarpium Papaveris, the curative effect that how much directly has influence on product of the content of these three indexs.As the Radix Platycodonis and the Radix Glycyrrhizae two flavor medicines of raw material, it is not differentiated the quality that then influences product.And the original standard of xiaochuan pian only provides the qualitative identification method of Pericarpium Papaveris and Herba Ephedrae, does not have the identification beacon of any assay and Radix Platycodonis and Radix Glycyrrhizae, and quality control index is too simple, can not carry out effective quality control to product.
Summary of the invention
A kind of drug effect that had both guaranteed product that the objective of the invention is to overcome above-mentioned shortcoming and provide, make constant product quality again, guaranteed that product is criticized and batch between repeatability, produce thereby better instruct, make technology controlling and process rationally strict more, can control the method for quality control of the xiaochuan pian of product quality effectively.
The method of quality control of a kind of xiaochuan pian of the present invention is included in the same system morphine, codeine phosphate, ephedrine hydrochloride is carried out assay simultaneously; Radix Platycodonis and Radix Glycyrrhizae in the prescription are carried out thin layer differentiate that step is as follows:
(1) chromatographic condition and system suitability experiment: with octadecylsilane chemically bonded silica is filler; With acetonitrile: 0.01mol/1 potassium dihydrogen phosphate: triethylamine: phosphoric acid=5: 95: 0.4: 0.2 is mobile phase; The detection wavelength is 220nm.Theoretical cam curve is calculated by the ephedrine hydrochloride peak should be not less than 10000;
(2) preparation of reference substance solution: it is an amount of that precision takes by weighing morphine, codeine phosphate, ephedrine hydrochloride reference substance, adds 0.1% hydrochloric acid solution and make the solution that every 1ml contains morphine 0.05mg, codeine phosphate 0.01mg, ephedrine hydrochloride 0.2mg, promptly;
(3) need testing solution preparation: get this product, remove coating, porphyrize, get about 1g, the accurate title, decide, and puts in the 50ml volumetric flask, accurate ammonia solution 1ml and the chloroform 25ml of adding claims to decide weight, supersound process (power 260w, frequency 40KHz) 30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with chloroform, shake up, filter, the accurate subsequent filtrate 5ml that draws adds 2% hydrochloric acid ethanol solution 2ml, shake up, water bath method, residue add that 0.1% hydrochloric acid solution 10ml is ultrasonic to make dissolving fully, filter, get subsequent filtrate, promptly;
(4) accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Every of this product contains Pericarpium Papaveris with morphine (C
17H
19O
3N) meter should be 0.16mg～1.06mg; Every of this product contains Pericarpium Papaveris with codeine phosphate (C
18H
21NO
3H
3PO
411/2H
2O) must not count and be less than 37 μ g; Every of this product contains Herba Ephedrae with ephedrine hydrochloride (C
10H
15NOHCl) must not count and be less than 2.38mg.
The method of quality control of above-mentioned xiaochuan pian also comprises the discriminating of Radix Platycodonis: take by weighing this product fine powder 0.5g, put in the tool plug test tube, add 10% hydrochloric acid solution 2ml, water-bath 1h takes out the centrifugal 10min of 3500r/min, incline and supernatant, transfer pH9～10 with ammonia, add chloroform 1ml, shake well, the centrifugal 10min of 3000r/min gets chloroform layer as need testing solution; Other gets Radix Platycodonis control medicinal material 0.2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: butanone: formic acid: water=10: 0.5: 0.5: 0.5 is developing solvent, launch, take out, dry, under ultra-violet lamp (365nm), inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle.
The method of quality control of above-mentioned xiaochuan pian comprises that also the thin layer of Radix Glycyrrhizae is differentiated: takes by weighing this product fine powder 0.5g, puts in the tool plug test tube, add methanol 2ml, and ultrasonic 30 minutes, take out, stir evenly, leave standstill clarification, supernatant is as need testing solution.Extracting liquorice control medicinal material 0.1g shines medical material solution in pairs with legal system in addition; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 2.5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-formic acid-glacial acetic acid-water (15: 1: 1: 2) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to colour developing in 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle.
The present invention compared with prior art by above technical scheme as can be known, comprises morphine, codeine phosphate, Determination of Ephedrine Hydrochloride assay method, the thin layer discrimination method of Radix Platycodonis and Radix Glycyrrhizae.Adopt high performance liquid chromatography under same system, simultaneously morphine, codeine phosphate, ephedrine hydrochloride in the prescription to be carried out assay, again medicine such as Radix Platycodonis and Radix Glycyrrhizae in the product is effectively differentiated simultaneously.Both guaranteed the drug effect of product, made constant product quality again, guaranteed that product is criticized and batch between repeatability, produce thereby better instruct, make technology controlling and process rationally strict more, can control product quality effectively.
Description of drawings
Fig. 1: morphine, codeine phosphate, ephedrine hydrochloride mixing reference substance;
Fig. 2: xiaochuan pian test sample;
Fig. 3: Herba Ephedrae negative sample;
Fig. 4: Pericarpium Papaveris negative sample;
Fig. 5: morphine standard curve;
Fig. 6: codeine phosphate standard curve;
Fig. 7: ephedrine hydrochloride standard curve.
The specific embodiment
The below routine by experiment beneficial effect that further specifies the inventive method.
Experimental example: morphine, codeine phosphate, Determination of Ephedrine Hydrochloride are measured
(1) selection of mobile phase:
Mobile phase 1:0.05mol/1 potassium dihydrogen phosphate-methanol-acetonitrile-triethylamine (80: 10: 10: 0.3);
Mobile phase 2:0.05mol/1 potassium dihydrogen phosphate-methanol-acetonitrile-triethylamine (75: 7: 18: 0.4);
Mobile phase 3:0.05mol/1 potassium dihydrogen phosphate-methanol-acetonitrile-triethylamine (78: 7: 15: 0.2);
Mobile phase 4: water-acetonitrile-phosphoric acid (90: 10: 0.1);
Mobile phase 5:0.01mol/1 potassium dihydrogen phosphate-acetonitrile-phosphoric acid (90: 10: 0.1);
Mobile phase 6:0.01mol/1 potassium dihydrogen phosphate-acetonitrile-phosphoric acid-triethylamine (90: 5: 0.2: 0.2);
Mobile phase 7:0.01mol/1 potassium dihydrogen phosphate-acetonitrile-triethylamine-phosphoric acid (95: 5: 0.4: 0.2)
By the analysis of above comparative test result, characteristics such as it is suitable that mobile phase 7 has retention time, and sample separation is effective, feminine gender is noiseless.Analyze according to follow-up test simultaneously and sum up, when the ephedrine hydrochloride theoretical cam curve reaches 10000, separate all greater than 1.5, so should be not less than 10000 in ephedrine hydrochloride peak theoretical cam curve.
(2) need testing solution preparation method screening
According to alkaloidal physicochemical property, we adopt different extracting method respectively, as index, the results are shown in following table with morphine, codeine phosphate, Determination of Ephedrine Hydrochloride.
| Method | Content results mg/g | ||
| Morphine | Codeine phosphate | Ephedrine hydrochloride | |
| 1 | 2.3437 | 0.5306 | 6.2187 |
| 2 | 0.7579 | 0.2027 | 3.2336 |
| 3 | 0.3697 | 0.2068 | 1.6308 |
| 4 | 2.6004 | 0.6202 | 7.1746 |
| 5 | 2.3266 | 0.6542 | 7.3392 |
Result of the test shows, with the extracting method of method 5 as sample.
(3) extraction time is selected
Adopt different extraction times to investigate, as index, select the optimum extraction time, the results are shown in following table with morphine, codeine phosphate, Determination of Ephedrine Hydrochloride.
| Extraction time (minute) | Content results mg/g | ||
| Morphine | Codeine | Ephedrine hydrochloride | |
| 10 | 1.7438 | 0.4885 | 5.5347 |
| 20 | 2.2571 | 0.6452 | 7.0338 |
| 30 | 2.4092 | 0.6836 | 7.4892 |
| 40 | 2.4051 | 0.6892 | 7.4781 |
| 50 | 2.3793 | 0.6789 | 7.4310 |
| 60 | 1.7438 | 0.4885 | 5.5347 |
Result of the test shows that uniform content after ultrasonic 30 minutes was advisable so ultrasonic time is selected for use in 30 minutes.
(4) mensuration of negative control experiment and solvent peak
Get the negative preparation of negative preparation of scarce Pericarpium Papaveris and scarce Herba Ephedrae,, make scarce Pericarpium Papaveris negative control product solution and scarce Herba Ephedrae negative control product solution with method according to need testing solution.Get scarce Pericarpium Papaveris negative control product respectively, lack each 10 μ l of Herba Ephedrae negative control product, test sample and reference substance solution, inject chromatograph of liquid, test, the results are shown in Figure 1,2,3,4 by above-mentioned chromatographic condition.
Above result of the test shows: negative control solution with reference substance, the corresponding position of test sample chromatographic peak on noiseless, method is feasible.
(5) linear relationship is investigated
Morphine, codeine phosphate, ephedrine hydrochloride mixing contrast solution 10 μ l that precision is measured variable concentrations inject chromatograph of liquid, carry out morphine, codeine phosphate, ephedrine hydrochloride mensuration, with morphine, codeine phosphate, ephedrine hydrochloride peak area A
Morphine, A
Codeine phosphate, A
Ephedrine hydrochloride is to morphine, codeine phosphate, ephedrine hydrochloride concentration C
Morphine, C
Codeine phosphate, C
Ephedrine hydrochlorideCarry out linear regression, equation of linear regression: A
Morphine=38062 C
Morphine-3828, A
Codeine phosphate=29191C
Codeine phosphate+ 758, A
Ephedrine hydrochloride=3940C
Ephedrine hydrochloride+ 886, the morphine range of linearity: 0.1253～2.0040 μ g, the codeine phosphate range of linearity: 0.0250～0.4000 μ g, the ephedrine hydrochloride range of linearity: 0.4983～7.9720 μ g, morphine correlation coefficient r=0.9999, codeine phosphate correlation coefficient r=0.9999, ephedrine hydrochloride correlation coefficient r=0.9998, former point equation A is crossed in match
Morphine=38034 C
Morphine, A
Codeine phosphate=29218 C
Codeine phosphate, A
Ephedrine hydrochloride=3942 C
Ephedrine hydrochlorideAdvance full scale equation with minimum point peak area generation respectively and former point equation is crossed in match, the morphine relative deviation is 0.37%, the codeine phosphate relative deviation is 0.48%, the ephedrine hydrochloride relative deviation is 0.20%, relative standard deviation is all less than 1%, and therefore visual full scale equation intercept levels off to zero, all can calculate content with one point external standard method.According to experimental result, morphine is in 0.1253～2.0040 μ g scope, and codeine phosphate is in 0.0250～0.4000 μ g scope, and ephedrine hydrochloride concentration is in 0.4983～7.9720 μ g scope, and peak area and sample size are good linear relationship.The results are shown in following table and Fig. 5,6,7.
| Morphine concentration (μ g/ml) | 12.5250 | 25.0500 | 50.1000 | 100.2000 | 200.4000 |
| The morphine peak area | 475545 | 982073 | 1918595 | 3733990 | 7674467 |
| 473814 | 980721 | 1922188 | 3716095 | 7641111 | |
| The morphine average peak area | 474680 | 981397 | 1920392 | 3725043 | 7657789 |
| Codeine phosphate concentration (μ g/ml) | 2.5000 | 5.0000 | 10.0000 | 20.0000 | 40.0000 |
| The codeine phosphate peak area | 72580 | 150295 | 296872 | 574462 | 1169068 |
| 73270 | 149961 | 297963 | 571514 | 1176172 | |
| The codeine phosphate average peak area | 72925 | 150128 | 297418 | 572988 | 1172620 |
| Ephedrine hydrochloride concentration (μ g/ml) | 49.8250 | 99.6500 | 199.3000 | 398.6000 | 797.2000 |
| The ephedrine hydrochloride peak area | 196315 | 402013 | 801710 | 1534487 | 3159749 |
| 196486 | 402327 | 807128 | 1525900 | 3153767 | |
| The ephedrine hydrochloride average peak area | 196401 | 402170 | 804419 | 1530194 | 3156758 |
(6) precision test
Precision is measured morphine, codeine phosphate, ephedrine hydrochloride mixing reference substance solution (0.0501mg/ml, 0.01mg/ml, 0.1993mg/ml) 10 μ l injection chromatograph of liquid, repeat sample introduction 5 times, calculated by peak area with morphine, codeine phosphate, ephedrine hydrochloride, morphine RSD is 0.23%, codeine phosphate RSD is 0.22%, and ephedrine hydrochloride RSD is 0.12%.The results are shown in following table
| Measure number of times | 1 | 2 | 3 | 4 | 5 | On average | RSD％ |
| The morphine peak area | 1915523 | 1916831 | 1914266 | 1908913 | 1906815 | 1912470 | 0.23 |
| The codeine phosphate peak area | 292587 | 293303 | 293423 | 294070 | 292541 | 293185 | 0.22 |
| The ephedrine hydrochloride peak area | 803370 | 803949 | 804803 | 803408 | 802269 | 803560 | 0.12 |
(7) replica test
Get same lot number test sample, prepare 5 parts of need testing solutions according to [assay] method, with the calculated by peak area of morphine, codeine phosphate, ephedrine hydrochloride, morphine RSD=1.90%, codeine phosphate RSD=1.35%, ephedrine hydrochloride RSD=1.89%.The results are shown in following table.
| Sequence number | Response rate % | ||
| Morphine | Codeine phosphate | Ephedrine hydrochloride | |
| 1 | 2.1212 | 0.7651 | 7.8570 |
| 2 | 2.0516 | 0.7481 | 7.9596 |
| 3 | 2.1632 | 0.7507 | 7.9923 |
| 4 | 2.1077 | 0.7550 | 8.1928 |
| 5 | 2.1207 | 0.7372 | 7.8021 |
| 6 | 2.1212 | 0.7651 | 7.8570 |
| Average content mg/g | 2.1129 | 0.7512 | 7.9608 |
| RSD％ | 1.90 | 1.35 | 1.89 |
(8) stability test
Precision is measured same need testing solution, and time sample introduction is in accordance with regulations surveyed 6 times altogether, with morphine, codeine phosphate, ephedrine hydrochloride calculated by peak area, the result shows, test sample in 10h, no significant change before and after morphine, codeine phosphate, the ephedrine hydrochloride peak area integrated value.
| Time (hour) | Peak area | ||
| Morphine | Codeine phosphate | Ephedrine |
|
| 0 | 1921317 | 472061 | 742402 |
| 2 | 1916356 | 471056 | 741764 |
| 4 | 1921800 | 470776 | 742901 |
| 6 | 1928790 | 468770 | 745880 |
| 8 | 1928874 | 462201 | 749547 |
| 10 | 1929939 | 466324 | 747888 |
| RSD％ | 0.29 | 0.79 | 0.43 |
(9) average recovery test
Get this product 0.5g, 6 parts, the accurate title, decide, in the 50ml volumetric flask, accurate morphine, codeine phosphate, ephedrine hydrochloride mixing reference substance solution (1.5180mg/ml, 0.3024mg/ml, the 4.0150mg/ml) 1ml of adding, according to test sample processing method and [assay] method, carry out morphine, codeine phosphate, ephedrine hydrochloride assay, the results are shown in following table.
| Sequence number | Response rate % | ||
| Morphine | Codeine phosphate | Ephedrine hydrochloride | |
| 1 | 94.17 | 95.66 | 98.34 |
| 2 | 93.70 | 96.70 | 97.98 |
| 3 | 93.36 | 94.89 | 97.19 |
| 4 | 93.86 | 95.03 | 98.57 |
| 5 | 94.24 | 95.31 | 98.65 |
| 6 | 94.20 | 95.92 | 98.36 |
| Average recovery rate % | 93.92 | 95.58 | 98.18 |
| RSD％ | 0.38 | 0.70 | 0.55 |
Result of the test shows that morphine application of sample average recovery rate is 93.92%, and RSD is 0.38%; Codeine phosphate application of sample average recovery rate is 95.58%, and RSD is 0.70%; Ephedrine hydrochloride application of sample average recovery rate is 98.18%, and RSD is 0.55%; Reach standard-required, method is feasible.
(10) ten batch sample assays
Press the assay operation, measure morphine, codeine phosphate, the ephedrine hydrochloride content of 10 lot number preparations, the results are shown in following table.
| Lot number | Content mg/g | ||
| Morphine | Codeine phosphate | Ephedrine hydrochloride | |
| 20050401 | 2.0356 | 0.6387 | 8.6221 |
| 20050402 | 2.0103 | 0.6558 | 7.6767 |
| 20050403 | 2.1396 | 0.6485 | 9.0026 |
| 20050404 | 2.1378 | 0.6446 | 8.155 |
| 20050405 | 2.2887 | 0.6283 | 8.4871 |
| 20050406 | 2.369 | 0.6473 | 8.7372 |
| 20050407 | 2.173 | 0.6446 | 8.3786 |
| 20050408 | 2.2038 | 0.6455 | 8.0608 |
| 20050409 | 2.2605 | 0.6503 | 8.2921 |
| 20050410 | 2.127 | 0.6482 | 7.5968 |
Morphine content scope * average yield (%) ÷ output (g)=44 3g in morphine content limit (mg/g) in the xiaochuan pian=Pericarpium Papaveris inventory (g) * Pericarpium Papaveris medical material * (0.6～4mg/g) * 59.73% ÷, 35 0g=0.45mg/g～3.02mg/g, i.e. 0.16mg/ sheet～1.06mg/ sheet;
Codeine phosphate content limit * average yield (%) ÷ output (g)=443g * 0.12mg/g in codeine phosphate content limit (mg/g) in the xiaochuan pian=Pericarpium Papaveris inventory (g) * Pericarpium Papaveris medical material * 70.38% ÷ 350g=0.11mg/g, i.e. 37 μ g/ sheets;
Ephedrine hydrochloride limit * average yield (%) ÷ output (g)=443g * 10mg/g in ephedrine hydrochloride content limit (mg/g) in the xiaochuan pian=Herba Ephedrae inventory (g) * Herba Ephedrae medical material * 53.76% ÷ 350g=6.80mg/g, i.e. 2.38mg/ sheet.
According to calculating, every of this product contains Pericarpium Papaveris with morphine (C
17H
19O
3N) meter should be 0.16mg～1.06mg; Every of this product is with codeine phosphate (C
18H
21NO
3H
3PO
411/2H
2O) must not count and be less than 37 μ g; Every of this product contains Herba Ephedrae with ephedrine hydrochloride (C
10H
15NOHCl) must not count and be less than 2.38mg;
Embodiment:
The method of quality control of xiaochuan pian comprises:
1, the discriminating of Radix Platycodonis:
Take by weighing this product fine powder 0.5g, put in the tool plug test tube, add 10% hydrochloric acid solution 2ml, water-bath 1h, take out, the centrifugal 10min of 3500r/min, inclining supernatant, transfers pH9～10 with ammonia, add chloroform 1ml, shake well, the centrifugal 10min of 3000r/min gets chloroform layer as need testing solution; Other gets Radix Platycodonis control medicinal material 0.2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: butanone: formic acid: water=10: 0.5: 0.5: 0.5 is developing solvent, launch, take out, dry, under ultra-violet lamp (365nm), inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle.
2, the discriminating of Radix Glycyrrhizae:
Take by weighing this product fine powder 0.5g, put in the tool plug test tube, add methanol 2ml, ultrasonic 30 minutes, take out, stir evenly, leave standstill clarification, supernatant is as need testing solution.Extracting liquorice control medicinal material 0.1g shines medical material solution in pairs with legal system in addition; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 2.5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-formic acid-glacial acetic acid-water (15: 1: 1:2) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to colour developing in 105 ℃.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle.
3, morphine, codeine phosphate, Determination of Ephedrine Hydrochloride are measured
(1) chromatographic condition and system suitability experiment: with octadecylsilane chemically bonded silica is filler; With acetonitrile: 0.01mol/1 potassium dihydrogen phosphate: triethylamine: phosphoric acid=5: 95: 0.4: 0.2 is mobile phase; The detection wavelength is 220nm.Theoretical cam curve is calculated by the ephedrine hydrochloride peak should be not less than 10000;
(2) preparation of reference substance solution: it is an amount of that precision takes by weighing morphine, codeine phosphate, ephedrine hydrochloride reference substance, adds 0.1% hydrochloric acid solution and make the solution that every 1ml contains morphine 0.05mg, codeine phosphate 0.01mg, ephedrine hydrochloride 0.2mg, promptly;
(3) need testing solution preparation: get this product, remove coating, porphyrize, get about 1g, the accurate title, decide, and puts in the 50ml volumetric flask, accurate ammonia solution 1ml and the chloroform 25ml of adding claims to decide weight, supersound process (power 260w, frequency 40KHz) 30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with chloroform, shake up, filter, the accurate subsequent filtrate 5ml that draws adds 2% hydrochloric acid ethanol solution 2ml, shake up, water bath method, residue add that 0.1% hydrochloric acid solution 10ml is ultrasonic to make dissolving fully, filter, get subsequent filtrate, promptly;
(4) accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Every of this product contains Pericarpium Papaveris with morphine (C
17H
19O
3N) meter should be 0.16mg～1.06mg; Every of this product contains Pericarpium Papaveris with codeine phosphate (C
18H
21NO
3H
3PO
411/2H
2O) must not count and be less than 37 μ g; Every of this product contains Herba Ephedrae with ephedrine hydrochloride (C
10H
15NOHCl) must not count and be less than 2.38mg.
Claims (4)
1. the method for quality control of an xiaochuan pian comprises the steps:
(1) chromatographic condition and system suitability experiment: with octadecylsilane chemically bonded silica is filler; With acetonitrile: 0.01mol/l potassium dihydrogen phosphate: triethylamine: phosphoric acid=5: 95: 0.4: 0.2 is mobile phase; The detection wavelength is 220nm, and theoretical cam curve is calculated by the ephedrine hydrochloride peak should be not less than 10000;
(2) preparation of reference substance solution: it is an amount of that precision takes by weighing morphine, codeine phosphate, ephedrine hydrochloride reference substance, adds 0.1% hydrochloric acid solution and make the solution that every 1ml contains morphine 0.05mg, codeine phosphate 0.01mg, ephedrine hydrochloride 0.2mg, promptly;
(3) need testing solution preparation: get this product, remove coating, porphyrize, get about 1g, the accurate title, decide, and puts in the 50ml volumetric flask, accurate ammonia solution 1ml and the chloroform 25ml of adding claims to decide weight, ultrasonic (power 260w, frequency 40KHz) handled 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with chloroform, shake up, filter, the accurate subsequent filtrate 5ml that draws adds 2% hydrochloric acid ethanol solution 2ml, shake up, water bath method, residue add that 0.1% hydrochloric acid solution 10ml is ultrasonic to make dissolving fully, filter, get subsequent filtrate, promptly;
(4) accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
2. the method for quality control of xiaochuan pian as claimed in claim 1, wherein the discrimination method of Radix Platycodonis is: take by weighing this product fine powder 0.5g, put in the tool plug test tube, add 10% hydrochloric acid solution 2ml, water-bath 1h takes out the centrifugal 10min of 3500r/min, incline and supernatant, transfer pH9～10 with ammonia, add chloroform 1ml, shake well, the centrifugal 10min of 3000r/min gets chloroform layer as need testing solution; Other gets Radix Platycodonis control medicinal material 0.2g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate: butanone: formic acid: water=10: 0.5: 0.5: 0.5 is developing solvent, launches, take out, dry, under the 365nm ultra-violet lamp, inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle.
3. the method for quality control of xiaochuan pian as claimed in claim 1 or 2, wherein the thin layer discrimination method of Radix Glycyrrhizae is: take by weighing this product fine powder 0.5g, put in the tool plug test tube, add methanol 2ml, ultrasonic 30 minutes, take out, stir evenly, leave standstill clarification, supernatant is as need testing solution; Extracting liquorice control medicinal material 0.1g shines medical material solution in pairs with legal system in addition; Test according to thin layer chromatography, draw each 2.5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-formic acid-glacial acetic acid-water=15: 1: 1: 2 was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, in 105 ℃ be heated to the colour developing clear, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the same color speckle.
4. the method for quality control of xiaochuan pian as claimed in claim 3, wherein every of this product contains Pericarpium Papaveris and should be 0.16mg～1.06mg in morphine; Every of this product contains Pericarpium Papaveris must not be less than 37 μ g in codeine phosphate; Every of this product contains Herba Ephedrae must not be less than 2.38mg in ephedrine hydrochloride.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100778766A CN101112424B (en) | 2007-08-07 | 2007-08-07 | Quality control method of asthma tablets |
Applications Claiming Priority (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507821A (en) * | 2011-10-26 | 2012-06-20 | 陕西方舟制药有限公司 | Method for detecting effective components in dyspnea-cough relieving capsules |
| CN103063792A (en) * | 2012-12-25 | 2013-04-24 | 贵州省科晖制药厂 | Quality test method of phlegm eliminating and cough stopping granules for children |
| CN113189225A (en) * | 2021-04-24 | 2021-07-30 | 无锡济煜山禾药业股份有限公司 | Method for simultaneously determining content of 3 alkaloids in strong loquat syrup |
-
2007
- 2007-08-07 CN CN2007100778766A patent/CN101112424B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507821A (en) * | 2011-10-26 | 2012-06-20 | 陕西方舟制药有限公司 | Method for detecting effective components in dyspnea-cough relieving capsules |
| CN103063792A (en) * | 2012-12-25 | 2013-04-24 | 贵州省科晖制药厂 | Quality test method of phlegm eliminating and cough stopping granules for children |
| CN113189225A (en) * | 2021-04-24 | 2021-07-30 | 无锡济煜山禾药业股份有限公司 | Method for simultaneously determining content of 3 alkaloids in strong loquat syrup |
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| CN101112424B (en) | 2010-06-09 |
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