Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, P R China.
Electrophoresis. 2010 Jan;31(4):714-23. doi: 10.1002/elps.200900425.
A method based on poly (methacrylic acid-co-ethylene glycol dimethacrylate) monolith microextraction and octadecylphosphonic acid-modified zirconia-coated CEC followed by field-enhanced sample injection preconcentration technique was proposed for sensitive CE-UV analysis of six antidepressants (doxepin, clozapine, imipramine, paroxetine, fluoxetine and chlorimipramine) in human plasma and urine. A poly(methacrylic acid-co-ethylene glycol dimethacrylate) monolithic capillary column was introduced for the extraction of antidepressants from urine and plasma samples. The hydrophobic main chains and acidic pendant groups of the monolithic column make it a superior material for extraction of basic analytes from aqueous matrix. After extraction, the desorption solvent, which normally provided an excellent medium to ensure direct compatibility for field-enhanced sample injection in CE, was analyzed by CE directly. By the use of alkylphosphonate-modified zirconia-coated CEC for separation of the basic compounds of antidepressants, high separation efficiency and resolution were achieved because that both hydrophobic interaction between analytes and alkylphosphonate-modified zirconia coat and electrophoretic effect work on the separation of antidepressants. The best separation was achieved using a buffer composed of 0.3 M ammonium acetate (adjusted to pH 4.5 with 1 M acetic acid) and 35% ACN v/v, with a temperature and voltage of 20 degrees C and 20 kV, respectively. By applying both preconcentration procedures, LODs of 11.4-51.5 and 3.7-17.0 microg/L were achieved for the six antidepressants in human plasma and urine, respectively. Excellent method of reproducibility was found over a linear range of 50-5000 microg/L in plasma and urine sample.
一种基于聚（甲基丙烯酸-co-乙二醇二甲基丙烯酸酯）整体微萃取和十八烷基膦酸修饰的氧化锆涂层 CEC 后场增强样品注入预浓缩技术的方法被提出，用于灵敏的 CE-UV 分析人血浆和尿液中的六种抗抑郁药（多虑平、氯氮平、丙咪嗪、帕罗西汀、氟西汀和氯米帕明）。 一种聚（甲基丙烯酸-co-乙二醇二甲基丙烯酸酯）整体毛细管柱被引入用于从尿液和血浆样品中提取抗抑郁药。整体柱的疏水性主链和酸性侧基使其成为从水性基质中提取碱性分析物的优异材料。 萃取后，通常提供出色介质以确保在 CE 中直接兼容场增强样品注入的洗脱溶剂直接通过 CE 进行分析。通过使用烷基膦酸修饰的氧化锆涂层 CEC 分离抗抑郁药的碱性化合物，实现了高分离效率和分辨率，因为分析物与烷基膦酸修饰的氧化锆涂层之间的疏水相互作用和电泳效应都对抗抑郁药的分离起作用。使用由 0.3 M 乙酸铵（用 1 M 乙酸调至 pH 4.5）和 35% ACN v/v 组成的缓冲液，在 20°C 和 20 kV 的温度和电压下，实现了最佳分离。通过应用两种浓缩程序，在人血浆和尿液中，六种抗抑郁药的 LODs 分别达到了 11.4-51.5 和 3.7-17.0 μg/L。在血浆和尿液样品中，在 50-5000 μg/L 的线性范围内，发现了出色的重现性方法。
