复方左炔诺孕酮阴道环中有关物质检测的方法学研究  

The methodology study on the detection of the related substance in compound levonorgestrel vaginal ring

作　　者：郑直[1,2] 张倩[1,2] 宁美英 

机构地区：[1]国家卫生计生委科学技术研究所药物和医用材料研究中心,北京100081 [2]北京协和医学院研究生院

出　　处：《中国计划生育学杂志》2017年第5期297-303,共7页Chinese Journal of Family Planning

基　　金："十三五"国家重点研发计划课题(2016YFC1000904)

摘　　要：目的:建立复方左炔诺孕酮(LNG)阴道环中有关物质的高效液相色谱(HPLC)检测方法,并对该方法进行方法学研究。方法:经紫外光谱法确定吸收波长,利用双波长法进行HPLC的检测。在强酸、强碱、高温、氧化剂、强光照等条件下,分别对注塑成型法制备的LNG和炔雌醇(EE)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。实验方法为色谱柱DiamonsilR C18(250mm×4.6mm,5μm);流动相乙腈-水体积比5248;LNG和EE的检测波长分别为240nm和205nm;柱温35℃;流速1.0ml/min。结果:专属性实验结果显示,复方LNG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。结论:所建立的复方LNG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。Objective：To construct High Performance Liquid Chromatography （HPLC） method for detecting the relative substance in compound Levonorgestrel vaginal ring,and then to study on methodology of this HPLC method.Methods：The absorbing wavelength was decided by the ultraviolet ultraviolet spectrometry method.Then the HPLC method was detected by the dual wavelength detection method.The compound LNG vaginal ring was synthesized by the way of injection molding,and then breaking test of the compound LNG vaginal ring conducted under the condition of strong acid,strong alkaline,high temperature,oxidizing agent and strong illumination.And the repeatability,stability,accuracy,and the limit of detection （LOD） of the ring were also detected by HPLC method.The chromatographic condition included that,chromatographic column was Diamonsil R C18 （250 mm ×4.6 mm,5 μm）,mobile phase was acetonitrile water 52：48,detection wavelength of LNG was 240 nm and detection wavelength of EE was 205nm,column temperature was 35 ℃ and flow rate was 1.0 ml/min.Results：The result of specificity test showed that,the main peak and the correlated peaks were well separated.Blank excipient couldn＇t affect the main peaks.Conclusion：The established method for testing compound LNG vaginal ring has the characteristics of operative simplicity,strong specificity and good repeatability.

关 键 词：左炔诺孕酮 炔雌醇 阴道环 方法学验证 高效液相色谱 

分 类 号：R927.1[医药卫生—药学]