Tu Yi-Yi, Hsieh Ming-Mu, Chang Sarah Y
Department of Chemistry, National Kaohsiung Normal University, Taiwan.
Electrophoresis. 2015 Nov;36(21-22):2828-2836. doi: 10.1002/elps.201500260. Epub 2015 Oct 13.
A rapid, simple and sensitive method for the detection of piperazinyl phenothiazine drugs using dispersive liquid-liquid microextraction (DLLME) combined with field-amplified sample stacking (FASS) in CE was developed. Sensitivity parameters that affect the extraction and FASS efficiency, such as the type and volume of disperser solvent, extraction time, addition of salt, and efficiency of FASS, were investigated and optimized. Note that the conductivity ratio between BGE and sample zone was measured to be 2300. Under optimal extraction and stacking conditions, the calibration curve, which ranged from 0.3 to 160 ng/mL, demonstrated good linearity with a correlation coefficient r≧ 0.9900. The LODs of prochlorperazine (Pcp), trifluoperazine (Tfp), perphenazine (Ppa), and fluphenazine (Fpa) at an S/N of 3 were 0.1, 0.1, 0.07, and 0.08 ng/mL, respectively. An approximately 1000-fold to 2500-fold improvement in sensitivity was achieved for the four tested analytes compared to conventional CZE without DLLME. The recoveries of all phenothiazines in urine and plasma ranged from 85.7 to 107.6% and 95.6 to 105.4%, respectively. The proposed method was demonstrated to be a rapid and convenient method for the determination of four piperazinyl phenothiazine drugs in human urine and plasma.
开发了一种快速、简单且灵敏的方法，用于在毛细管电泳（CE）中使用分散液液微萃取（DLLME）结合场放大进样（FASS）检测哌嗪基吩噻嗪类药物。研究并优化了影响萃取和FASS效率的灵敏度参数，如分散剂溶剂的类型和体积、萃取时间、盐的添加以及FASS效率。注意，测量得到背景电解质（BGE）与样品区之间的电导率比为2300。在最佳萃取和富集条件下，校准曲线范围为0.3至160 ng/mL，具有良好的线性，相关系数r≧0.9900。在信噪比为3时，奋乃静（Pcp）、三氟拉嗪（Tfp）、奋乃静（Ppa）和氟奋乃静（Fpa）的检测限分别为0.1、0.1、0.07和0.08 ng/mL。与不使用DLLME的传统毛细管区带电泳（CZE）相比，四种被测分析物的灵敏度提高了约1000倍至2500倍。尿液和血浆中所有吩噻嗪类药物的回收率分别为85.7%至107.6%和95.6%至105.4%。所提出的方法被证明是一种快速便捷的方法，用于测定人尿液和血浆中的四种哌嗪基吩噻嗪类药物。
