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目的:建立米非司酮胶囊有关物质测定的HPLC法,对其主要有关物质进行研究,制定有关物质合理限度,有效控制产品质量。方法:采用RP-HPLC法,色谱柱为C18柱,流动相:乙腈-10 mmol·L-1磷酸二氢钾溶液(用磷酸调节pH至2.5)(35∶65),流速1.0 mL·min-1,检测波长304 nm,柱温35℃。结果:米非司酮胶囊中的主要杂质为N-单去甲基米非司酮,既是副产物也是降解产物。A企业3批样品中该杂质含量均为0.5%,B企业3批样品中该杂质含量均为0.2%。A企业3批样品杂质总量为0.6%~0.7%,B企业3批样品杂质总量为0.2%~0.3%。结论:本方法可快速有效分离米非司酮胶囊中各有关物质。对已知、未知有关物质分别设定不同限度,可有效控制该药品质量。
OBJECTIVE: To establish a HPLC method for the determination of related substances in mifepristone capsules, to study the main related substances, to establish the reasonable limit of relevant substances and to effectively control the product quality. Methods: The column was C18 column with RP-HPLC method. The mobile phase consisted of acetonitrile-10 mmol·L-1 potassium dihydrogen phosphate (pH = 2.5 with phosphoric acid) (35:65), the flow rate was 1.0 mL · min- 1, detection wavelength 304 nm, column temperature 35 ℃. Results: The main impurity in mifepristone capsules was N-monodemethyl-mifepristone, which was both a by-product and a degradation product. In the three batches of samples of A enterprise, the impurity content is 0.5%, and the impurities in three batches of B enterprise are both 0.2%. The total amount of impurity samples from 3 batches of A enterprises was 0.6% ~ 0.7%, while that of B batches was 0.2% ~ 0.3%. Conclusion: This method can quickly and effectively separate all relevant substances in mifepristone capsules. The known and unknown substances were set different limits, which can effectively control the quality of the drug.