HPLC法测定不同来源米非司酮胶囊的有关物质  

HPLC determination of related substances in mifepristone capsules from different soures

作　　者：施捷[1] 车宝泉[1] 郑焱 尹光[1] 周立春[1] 

机构地区：[1]北京市药品检验所,北京100035 [2]华润紫竹药业有限公司,北京100024

出　　处：《药物分析杂志》2014年第3期480-484,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：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-10mmol·L^-1磷酸二氢钾溶液（用磷酸调节pH至2．5）（35：65），流速1．0mL·min^-1。，检测波长304nm，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 an HPLC method for the determination of related substances in mifepristone cap- sules, and to study its principal related substances and set reasonable limits for related substances to improve the quality control for mifepristone capsules. Methods： Related substances were analyzed by the RP - HPLC method. The Crscolumn was used and a mixture of acetonitrile and phosphate BS（ 10 mmol·L^-1 potassium dihydrogen phos- phate,adjusted to pH 2. 5 with phosphoric acid）（35： 65） was used as the mobile phase. The flow rate was 1.0 mL ·min^-1, and the detection wavelength was 304 nm, and the column temperature was 35 ℃. Results： The main impu- rity was N - mono - demethylated mifepristone, which was both a by - product and a degradation product. The con- tent of this impurity in 3 batches of manufacturer A was 0.5%, and that in 3 batches of manufacturer B was 0. 2%. The total content of impurities in 3 batches of manufacturer A was 0. 6% -0.7%, and in 3 batches of manufacturer B was 0.2% -0. 3%. Conclusion： Mifepristone and its related substances were obviously separated under the chromatographic system described above. The limit for N - mono - demethylated mifepristone was 1.0% and the limit for other individual impurities was 0. 2% and the limit for total impurities was 1.5%. This method can control the quality of mifepristone capsules effectively.

关 键 词：米非司酮 N-单去甲基米非司酮 N N-双去甲基米非司酮 杂质限度 高效液相色谱法 胶囊质量控制 

分 类 号：R917[医药卫生—药物分析学]