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Solid-phase extraction with liquid chromatography and ultraviolet detection for the assay of antidepressant drugs in human plasma

化学 色谱法 固相萃取 马普替林 洗脱 多塞平 高效液相色谱法 吸附剂 萃取(化学) 乙酸钠 醋酸 地昔帕明 丙咪嗪 吸附 有机化学 医学 替代医学 病理 药理学 神经科学 生物 海马体 抗抑郁药
作者
A. Bakkali,E Corta,J I Ciria,Luis Á. Berrueta,Blanca Gallo,Francisca Vicente
出处
期刊:Talanta [Elsevier]
卷期号:49 (4): 773-783 被引量:42
标识
DOI:10.1016/s0039-9140(99)00087-9
摘要

A solid-phase extraction (SPE) method for sample clean-up followed by a reversed-phase high-performance liquid chromatography (HPLC) procedure for the assay of five antidepressant drugs (trazodone, doxepin, desipramine, maprotiline and imipramine) is reported. The drugs were recovered from plasma buffered at a suitable pH using C18 Bond-Elut cartridges and mixtures of methanol–aqueous buffer as washing and elution solvents. The recoveries of the drugs using other sorbent materials (C8, C2, cyclohexyl, cyanopropyl and phenyl Bond Elut and copolymer HLB waters cartridges) were also examined. The selectivity of SPE was examined by using spiked plasma samples and the CH cartridge gave rise to the cleanest extracts. Cyclohexyl cartridges were conditioned successively with 2 ml of methanol and 1 ml of acetic acid–sodium acetate buffer (0.1 M, pH 4.0). Plasma sample was buffered at pH 4.0 and then applied to the sorbent. The washing step was performed subsequently with 1.5 ml of acetate buffer (0.1 M, pH 4.0), 100 μl of acetonitrile and 1 ml of methanol–acetate buffer (30:70, v/v). Finally, the analytes were eluted with 0.5 ml of methanol–acetate buffer (70:30, v/v). The extract was evaporated to dryness, reconstituted in mobile phase, and chromatographed on a reversed-phase C18 column with ultraviolet detection at 215 nm. The recoveries of trazodone, doxepin, desipramine, maprotiline and imipramine from spiked plasma samples using the CH cartridge were 58 2, 84 3, 83 3, 83 3 and 82 2%, respectively. The within-day and between-day repeatabilities were lower than 6% and 9%, respectively. The linearity of calibrations for the five antidepressants was between 0.005 and 2 μg/ml. The limits of detection were 1 ng/ml for trazodone, doxepin and desipramine and 2 ng/ml for maprotiline and imipramine.
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