Peng Jun, Xiao Deli, He Hua, Zhao Hongyan, Wang Cuixia, Shi Tian, Shi Kexin
Department of Analytical Chemistry, China Pharmaceutical University, Nanjing, China.
Key Laboratory of Drug Quality Control and Pharmacovigilance, Ministry of Education, China Pharmaceutical University, Nanjing, China.
J Sep Sci. 2016 Jan;39(2):383-90. doi: 10.1002/jssc.201500751.
In this study, molecularly imprinting technology and stir bar absorption technology were combined to develop a microextraction approach based on a molecularly imprinted polymeric stir bar. The molecularly imprinted polymer stir bar has a high performance, is specific, economical, and simple to prepare. The obtained naftopidil-imprinted polymer-coated bars could simultaneously agitate and adsorb naftopidil in the sample solution. The ratio of template/monomer/cross-linker and conditions of template removal were optimized to prepare a stir bar with highly efficient adsorption. Fourier transform infrared spectroscopy, scanning electron microscopy, selectivity, and extraction capacity experiments showed that the molecularly imprinted polymer stir bar was prepared successfully. To utilize the molecularly imprinted polymer stir bar for the determination of naftopidil in complex body fluid matrices, the extraction time, stirring speed, eluent, and elution time were optimized. The limits of detection of naftopidil in plasma and urine sample were 7.5 and 4.0 ng/mL, respectively, and the recoveries were in the range of 90-112%. The within-run precision and between-run precision were acceptable (relative standard deviation <7%). These data demonstrated that the molecularly imprinted polymeric stir bar based microextraction with high-performance liquid chromatography was a convenient, rapid, efficient, and specific method for the precise determination of trace naftopidil in clinical analysis.
在本研究中,将分子印迹技术与搅拌棒吸附技术相结合,开发了一种基于分子印迹聚合物搅拌棒的微萃取方法。分子印迹聚合物搅拌棒性能优异、具有特异性、经济且制备简单。所制备的萘哌地尔印迹聚合物涂层搅拌棒能够同时搅拌并吸附样品溶液中的萘哌地尔。对模板/单体/交联剂的比例及模板去除条件进行了优化,以制备具有高效吸附性能的搅拌棒。傅里叶变换红外光谱、扫描电子显微镜、选择性及萃取容量实验表明成功制备了分子印迹聚合物搅拌棒。为将分子印迹聚合物搅拌棒用于复杂体液基质中萘哌地尔的测定,对萃取时间、搅拌速度、洗脱剂及洗脱时间进行了优化。血浆和尿液样品中萘哌地尔的检测限分别为7.5和4.0 ng/mL,回收率在90% - 112%范围内。批内精密度和批间精密度均可接受(相对标准偏差<7%)。这些数据表明,基于分子印迹聚合物搅拌棒的微萃取结合高效液相色谱法是临床分析中精确测定痕量萘哌地尔的一种简便、快速、高效且特异的方法。