分散液-液微萃取结合HPLC测定富马酸替诺福韦酯中9-丙烯基腺嘌呤  

Dispersive liquid-liquid microextraction combined HPLC to determine contents of 9-propenyladenine in tenofovir disoproxil fumarate

作　　者：闫鹏飞 崔毅轩 刘迪[1] 马晴 冯鹏磊 葛瑶 蒋晔[1] YAN Peng-fei;CUI Yi-xuan;LIU Di;MA Qing;FENG Peng-lei;GE Yao;JIANG Ye(Pharmacy College,Hebei Medical University,Shijiazhuang 050017)

机构地区：[1]河北医科大学药学院

出　　处：《分析试验室》2019年第12期1432-1435,共4页Chinese Journal of Analysis Laboratory

基　　金：国家级大学生创新性实验计划项目(USIP2018016)资助

摘　　要：将分散液-液微萃取与HPLC结合,建立了测定富马酸替诺福韦酯中的基因毒性杂质9-丙烯基腺嘌呤的分析方法。同时对影响萃取效率的各项参数如萃取剂的种类及用量、分散剂的种类及用量、溶液体系pH、离子强度及萃取时间等进行了优化。将样品用水溶解,调节溶液至pH 9.0,NaCl浓度为3 g/L,以300μL正庚醇为萃取剂,萃取时间为3 min,3000 r/min离心3 min,取上层进行液相分析。结果表明,9-丙烯基腺嘌呤在1.22~366 ng/mL范围内线性关系良好,检测限为0.41 ng/mL,平均回收率为96.2%~97.8%,RSD<1.0%。方法满足富马酸替诺福韦酯中基因毒性杂质9-丙烯基腺嘌呤的测定要求。A method for the rapid determination of the genotoxic impurity 9-propenyladenine in tenofovir disoproxil fumarate was established by combining dispersive liquid-liquid microextraction with HPLC.The parameters affecting the extraction efficiency,such as the type and amount of the extractant,the type and amount of the dispersant,the pH of the solution system,the ionic strength and the extraction time were optimized simultaneously.The sample was dissolved in water,then the pH of the solution was adjusted to 9.0 and the concentration of NaCl was 3 g/L.300μL of n-heptanol was used as the extractant and the extraction time was 3 min.After centrifuged at 3000 r/min for 3 min,the upper layer was taken for the HPLC analysis.The results showed that 9-propenyladenine has a good linearity in the range of 1.22-366 ng/mL,and the limit of detection was 0.41 ng/mL.The average recoveries were 96.2%-97.8%,with RSDs no more than 1.0%.This method can fulfil requirements for determination of the genotoxic impurity 9-propenyladenine in tenofovir disoproxil fumarate.

关 键 词：分散液-液微萃取 基因毒性杂质 9-丙烯基腺嘌呤 含量测定 富马酸替诺福韦酯 

分 类 号：O657.31[理学—分析化学] X832[理学—化学]