阿那曲唑阴道环中有关物质检测的方法学研究

The methodology study of related substances detection in compound anastrozole intravaginal ring

目的:建立阿那曲唑阴道环中有关物质的高效液相色谱(HPLC)检测方法并进行方法学研究。方法:在强酸、强碱、高温、氧化剂、强光照等条件下,对注塑成型法制备的阿那曲唑阴道环进行破坏试验。利用HPLC法考察阴道环的稳定性、精密度、检测限等。HPLC检测条件为色谱柱Diamonsil C18(2)(250 mm×4.6 mm,5μm);流动相乙腈-水(42:58,v/v);检测波长210nm;流速1.0ml/min;进样量20μl;柱温35℃。结果:阿那曲唑阴道环主成分与相关杂质及降解产物均分离良好,空白辅料对测定无干扰;检测限为3ng/ml;重复性相对标准偏差(RSD)1.6%,溶液稳定性RSD为1.8%。结论:本文所建立的阿那曲唑阴道环中有关物质的测定方法操作简单、专属性强、重复性好,可以为阿那曲唑阴道环质量控制提供依据。

Objective：To establish High Performance Liquid Chromatography（HPLC）method for detecting related substances in compound anastrozole vaginal ring,and to study on methodology of the HPLC method.Methods：The compound anastrozole vaginal ring was synthesized by the way of injection molding,and the breaking test was conducted under strong acid,strong alkaline,high temperature,oxidant or strong illumination.The repeatability,stability,accuracy,and the limit of detection（LOD）of the ring were also detected by HPLC method with a column of Diamonsil C18（2）（250 mm × 4.6 mm,5μm）and UV detection at 210 nm.The mobile phase consisted of acetonitrile water（42：58,v/v）at a flow rate of 1.0 ml/min.The sample size was 20μl and column temperature was 35 ℃.Results：The result of specificity test showed that the main drug and the related impurities,degradation products were well separated.Blank excipient had no interference for determination.Anastrozole detection limit was 3 ng/ml.The RSD of the reproducibility was 1.6 % and the RSD of the stability was 1.8 %.Conclusion：The established method for detecting related substances in compound anastrozole vaginal ring has the characteristics of operative simplicity,strong specificity and good repeatability.