Determination of the amount of acetylspiramycin tablets. The microbial method is usually used, and its operation is cumbersome and time-consuming, and it is difficult to meet the needs of production. According to the literature, spiramycin has a large absorption of ultraviolet zui at a length of 232 nm. Therefore, the content of acetylspiramycin was determined by ultraviolet spectrophotometry. The measurement conditions were examined. In comparison with the biological method, the results were satisfactory. The method is simple and rapid, and can be used as a reference for the pharmaceutical manufacturer to control the spiramycin tablets and their intermediate quality.
1 instruments, drugs and reagents UV spectrophotometer; Japan Shimadzu UV-2l0l acetylspiramycin reference substance; Hunan Yueyang City Drug Testing Institute acetylspiramycin tablets and intermediates Harbin Chinese Medicine Third Plant methanol for analytical analysis
7.8 Phosphate buffer: embedded in the Chinese Pharmacopoeia appendix.
2 Determination of the conditions of the choice of acetylspiramycin ultraviolet absorption spectrum: weigh the appropriate amount of acetylspiramycin, dissolved in methanol, and made a solution of 10μg / ml with distilled water, with distilled water as a blank, in μV-2lO1 UV spectrophotometry The automatic scanning (wavelength of 200 to 300 nm) has a large absorption of zui at a wavelength of 232 nm.
The relationship between concentration and absorbance: accurately weigh the appropriate amount of acetylspiramycin standard, dissolve it with methanol, and make the concentration of 5, 7, 10, 13, 15, 18, 20 μg/ml with distilled water, and measure the absorbance at 232 nm. It was found to be linear with absorbance in the range of 5 - l8 μg / ml. The linear equation was: A = 0.001323 + 0.0305 × C, and the correlation coefficient was R = 0.9993.
The relationship between blank storage and absorbance: Precision aliquots of acetylspiramycin standard three aliquots, dissolved in methanol, respectively, distilled water, 7.8 phosphate buffer, methanol made l0μg / ml dissolution, determination of absorbance. It can be seen that the blank liquid has little effect on the warmth. In this experiment, distilled water was used as the dilution blank.
3 Determination of the content of acetylspiramycin tablets Take 10 pieces of this product for precise weighing. After grinding, accurately weigh the appropriate amount (about equivalent to 0.1g of spiramycin) and dissolve it in 20ml methanol to the lOOml volumetric flask. Dilute the distilled water to the mark. The absorbance was measured at 232 nm with distilled water as a blank, and the content was calculated from the standard curve.
4 The recovery experiment accurately weighed three parts of acetylspiramycin, and added dextrin, magnesium stearate and other auxiliary materials according to the prescription, and mixed evenly. The average recovery rate was 98.98% and the coefficient of variation was 0.27%.
5 UV spectrophotometry and bioassay comparison Take the same batch of spiramycin tablets, measured by two methods.
discuss;
1. The results of this experiment indicate that hexyl cyanomycin is in various concentrations. The large absorption of zui is about 232 nm, and the absorbance is linear with the concentration in the range of 5-18 μg/ml.
2. Due to the difference between the reference substance and its potency, the curves obtained by different reference materials are slightly different, so the standard curve should be used for each batch of production.
3. This method can be used in pharmaceutical factories after several times of comparison, and the intermediate content is controlled during the production of the spiral mold.
4. After the sample is dissolved in methanol, which dilution is used, the author measured the results with 7.8 phosphate buffer after several experiments, and the results were close with methanol or distilled water. From the economic and other aspects, the experiment chose distilled water. .
1 instruments, drugs and reagents UV spectrophotometer; Japan Shimadzu UV-2l0l acetylspiramycin reference substance; Hunan Yueyang City Drug Testing Institute acetylspiramycin tablets and intermediates Harbin Chinese Medicine Third Plant methanol for analytical analysis
7.8 Phosphate buffer: embedded in the Chinese Pharmacopoeia appendix.
2 Determination of the conditions of the choice of acetylspiramycin ultraviolet absorption spectrum: weigh the appropriate amount of acetylspiramycin, dissolved in methanol, and made a solution of 10μg / ml with distilled water, with distilled water as a blank, in μV-2lO1 UV spectrophotometry The automatic scanning (wavelength of 200 to 300 nm) has a large absorption of zui at a wavelength of 232 nm.
The relationship between concentration and absorbance: accurately weigh the appropriate amount of acetylspiramycin standard, dissolve it with methanol, and make the concentration of 5, 7, 10, 13, 15, 18, 20 μg/ml with distilled water, and measure the absorbance at 232 nm. It was found to be linear with absorbance in the range of 5 - l8 μg / ml. The linear equation was: A = 0.001323 + 0.0305 × C, and the correlation coefficient was R = 0.9993.
The relationship between blank storage and absorbance: Precision aliquots of acetylspiramycin standard three aliquots, dissolved in methanol, respectively, distilled water, 7.8 phosphate buffer, methanol made l0μg / ml dissolution, determination of absorbance. It can be seen that the blank liquid has little effect on the warmth. In this experiment, distilled water was used as the dilution blank.
3 Determination of the content of acetylspiramycin tablets Take 10 pieces of this product for precise weighing. After grinding, accurately weigh the appropriate amount (about equivalent to 0.1g of spiramycin) and dissolve it in 20ml methanol to the lOOml volumetric flask. Dilute the distilled water to the mark. The absorbance was measured at 232 nm with distilled water as a blank, and the content was calculated from the standard curve.
4 The recovery experiment accurately weighed three parts of acetylspiramycin, and added dextrin, magnesium stearate and other auxiliary materials according to the prescription, and mixed evenly. The average recovery rate was 98.98% and the coefficient of variation was 0.27%.
5 UV spectrophotometry and bioassay comparison Take the same batch of spiramycin tablets, measured by two methods.
discuss;
1. The results of this experiment indicate that hexyl cyanomycin is in various concentrations. The large absorption of zui is about 232 nm, and the absorbance is linear with the concentration in the range of 5-18 μg/ml.
2. Due to the difference between the reference substance and its potency, the curves obtained by different reference materials are slightly different, so the standard curve should be used for each batch of production.
3. This method can be used in pharmaceutical factories after several times of comparison, and the intermediate content is controlled during the production of the spiral mold.
4. After the sample is dissolved in methanol, which dilution is used, the author measured the results with 7.8 phosphate buffer after several experiments, and the results were close with methanol or distilled water. From the economic and other aspects, the experiment chose distilled water. .
Chongqing "Terson" Coptis", Department of Chongqing Shizhu Tujia Autonomous County specialty, China National Geographic Indications (native geographical products). Produced in Shizhu County Huangshui National Forest Park, also known as "Coptis". Ranunculaceae Coptis Coptis chinensis Franch dry rhizomes, medicinal products "taste even", Department of commonly used precious Chinese medicine, Shizhu County is the original production of Coptis, Coptis town, the production of Because of good quality, was identified as "Sinopharm" "Authentic Coptis".
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