UHPLC测定盐酸氟西汀原料药中甲醛及其测量不确定度评定  

Determination and uncertainty evaluation of formaldehyde in fluoxetine hydrochloride raw material by UHPLC

作　　者：李永利[1] 陈鹰[1] 李杰[1] LI Yongli;CHEN Ying;LI Jie(Shanghai Key Laboratoiy of Online Testing and Control Technology,Shanghai Institute of Measurement and Testing Technology,Shanghai 201203)

机构地区：[1]上海市计量测试技术研究院在线检测与控制技术重点实验室,上海201203

出　　处：《分析试验室》2021年第10期1206-1211,共6页Chinese Journal of Analysis Laboratory

基　　金：上海市科学技术委员会科研计划项目(17142203200);上海市计量测试技术研究院项目(I00RY1911)资助。

摘　　要：采用超快速液相色谱(UHPLC)建立了快速测定盐酸氟西汀原料药中甲醛残留的方法。样品经50%乙腈-水溶液提取,酸性条件下与2,4-二硝基苯肼发生衍生化反应,采用超快速液相色谱仪外标法测定盐酸氟西汀原料药中甲醛的含量,添加量为5~20μg/g时,平均回收率为96.8%~99.0%。评估了测量方法的不确定度。盐酸氟西汀原料药中甲醛含量的测量结果表示为(7.40±0.46)μg/g,k=2。方法适用于盐酸氟西汀中甲醛的快速检测。A method was developed for the determination of formaldehyde in fluoxetine hydrochloride raw material by ultra-high performance liquid chromatography( UHPLC). The analytes in fluoxetine hydrochloride raw material were extracted with 50% aqueous acetonitrile,and derivatized with 2,4-dinitrophenylhydrazine to form 2,4-dinitrophenylhydrazone. The recoveries were 96. 8% to 99. 0% when the spiked amount of formaldehyde in the raw material was in the range 5-20 μg/g,and the uncertainty of the measurement results was evaluated on the base of analysis of relevant factors. The determination result was( 7. 40 ± 0. 46) μg/g,k= 2. The method is suitable for the determination of formaldehyde in fluoxetine hydrochloride raw material,providing reference for the control measurement and uncertainty evaluation of formaldehyde in fluoxetine hydrochloride.

关 键 词：甲醛 液相色谱 盐酸氟西汀 衍生化 不确定度 

分 类 号：O657.7[理学—分析化学]