Quantitative determination of phenothiazine derivatives in human plasma using monolithic silica solid-phase extraction tips and gas chromatography-mass spectrometry
Quantitative determination of phenothiazine derivatives in human plasma using monolithic silica solid-phase extraction tips and gas chromatography-mass spectrometry
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DOI：
10.1016/j.chroma.2011.02.070
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发表时间：
2011-05-06
影响因子：
4.1
通讯作者：
Sato, Keizo
中科院分区：
文献类型：
--
作者：
Kumazawa, Takeshi;Hasegawa, Chika;Sato, Keizo
使用微量移液器吸头进行固相萃取 (SPE) 是在质谱分析之前制备样品的有用技术。然而，大多数商用 SPE 吸头的负载能力不足以进行定量测定。在本文中，我们描述了一种快速定量微量分析五种吩噻嗪衍生物（氯丙嗪、左美丙嗪、丙嗪、异丙嗪和曲美嗪）的方法，使用最近推出的 C-18 整体式硅胶 SPE 针头 MonoTip C-18 从人血浆中提取。可以在 5 分钟内从 0.1 mL 血浆样品中提取药物，用甲醇洗脱，然后将洗脱液直接注射到气相色谱仪中，然后进行质谱分析。萃取过程的每个步骤仅需要 0.7 mL 溶剂。添加到血浆中的五种吩噻嗪的回收率为 91-95%，每种药物的定量限在 0.25 至 2.0 ng/0.1 mL 之间。日内和日间变异系数最大为 11%。经过验证的方法已成功用于定量人类受试者口服药物后左美丙嗪的血浆浓度。这种新方法有望作为快速、定量测定血浆样品中药物浓度的预处理具有广泛的应用。 (C) 2011 Elsevier B.V. 保留所有权利。
Solid-phase extraction (SPE) using micropipette tips is a useful technique to prepare samples prior to mass spectrometry. However, most commercial SPE tips have loading capacities that are insufficient for quantitative determination. In this paper, we describe a rapid method for quantitative microanalysis of five phenothiazine derivatives, chlorpromazine, levomepromazine, promazine, promethazine and trimeprazine, using a recently introduced C-18 monolithic silica SPE tip, the MonoTip C-18, for extraction from human plasma. The drugs could be extracted within 5 min from 0.1-mL plasma samples, eluted with methanol, and the eluate injected directly into a gas chromatograph prior to mass spectrometry analysis. Only 0.7 mL of solvent was required for each step of the extraction process. The recoveries of the five phenothiazines spiked into plasma were 91-95% and the limits of quantification for each drug were between 0.25 and 2.0 ng/0.1 mL. The maximum intra- and inter-day coefficient of variation was 11%. The validated method was successfully used to quantify the plasma concentration of levemepromazine in a human subject after oral administration of the drug. This new method is expected to have wide applications as a pretreatment for the rapid, quantitative determination of drug concentrations in plasma samples. (C) 2011 Elsevier B.V. All rights reserved.