Zhou Xiaoqing, He Man, Chen Beibei, Hu Bin
Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
Analyst. 2015 Mar 7;140(5):1662-71. doi: 10.1039/c4an02209b. Epub 2015 Jan 26.
An effective dual preconcentration method involving off-line hollow fiber liquid-liquid-liquid microextraction (HF-LLLME) and on-line sweeping micellar electrokinetic chromatography (sweeping-MEKC) was proposed for the determination of five second-generation antidepressants, including fluoxetine, sertraline, paroxetine, fluvoxamine and citalopram. In HF-LLLME, the analytes were extracted from the sample solution into phenetole impregnated in the pores of the hollow fiber and then back-extracted into 10 μL 0.1 mol L(-1) HAc inside the hollow fiber. Then, the acceptor phase was spiked with 2.8 μL isopropanol (IPA) and introduced into CE for sweeping. In the sweeping-MEKC process, five target analytes were separated in less than 15 min with a background electrolyte consisting of 76% (v/v) 50 mmol L(-1) citric acid (pH 2.2) containing 100 mmol L(-1) sodium dodecyl sulfate (SDS) and 24% (v/v) IPA. The hydrodynamic injection was performed at 50 mbar for 140 s. Under optimized conditions, the limits of detection were in the range of 0.40-1.55 μg L(-1) with enrichment factors of 1897- to 5952-fold for target analytes, with a dynamic linear range of 0.6/5.0-200 μg L(-1). The developed method demonstrated excellent clean-up ability and high enrichment factors and was successfully applied to the analysis of target analytes in human urine and plasma samples.
提出了一种有效的双重预富集方法,该方法包括离线中空纤维液-液-液微萃取(HF-LLLME)和在线吹扫胶束电动色谱法(吹扫-MEKC),用于测定5种第二代抗抑郁药,包括氟西汀、舍曲林、帕罗西汀、氟伏沙明和西酞普兰。在HF-LLLME中,分析物从样品溶液中萃取到浸渍在中空纤维孔中的苯乙醚中,然后反萃取到中空纤维内部10 μL 0.1 mol L(-1) HAc中。然后,在受体相中加入2.8 μL异丙醇(IPA),并引入毛细管电泳进行吹扫。在吹扫-MEKC过程中,5种目标分析物在不到15分钟内分离,背景电解质由76%(v/v)50 mmol L(-1)柠檬酸(pH 2.2)、100 mmol L(-1)十二烷基硫酸钠(SDS)和24%(v/v)IPA组成。在50 mbar下进行140 s的流体动力学进样。在优化条件下,检测限在0.40-1.55 μg L(-1)范围内,目标分析物的富集因子为1897-5952倍,动态线性范围为0.6/5.0-200 μg L(-1)。所建立的方法具有出色的净化能力和高富集因子,并成功应用于人体尿液和血浆样品中目标分析物的测定。