Malfará Wilson Roberto, Bertucci Carlo, Costa Queiroz Maria Eugênia, Dreossi Carvalho Sonia Ap, Pires Bianchi Maria de Lourdes, Cesarino Evandro José, Crippa José Alexandre, Costa Queiroz Regina Helena
Department of Psychiatry and Psychology, Faculty of Medicine of Ribeirão Preto, University of São Paulo, Avenida do Café s/n, Monte Alegre, CEP 14040-903 Ribeirão Preto, SP, Brazil.
J Pharm Biomed Anal. 2007 Aug 15;44(4):955-62. doi: 10.1016/j.jpba.2007.04.005. Epub 2007 Apr 8.
A new high-performance liquid chromatography method is presented for the determination of 10 frequently prescribed tricyclic and nontricyclic antidepressants: imipramine, amitriptyline, clomipramine, fluoxetine, sertraline, paroxetine, citalopram, mirtazapine, moclobemide and duloxetine. The simple and accurate sample preparation step, consisted of liquid:liquid extraction with recoveries ranging between 72% and 86%, except for moclobemide (59%). Separation was obtained using a reverse phase Select B column under isocratic conditions with UV detection (230 nm). The mobile phase consisted of 35% of a mixture of acetonitrile/methanol (92:8, v/v) and 65% of 0.25 mol L(-1) sodium acetate buffer, pH 4.5. The standard curves were linear over a working range of 2.5-1000 ng mL(-1) for moclobemide, 5-2000 ng mL(-1) for citalopram, duloxetine, fluoxetine, 10-2000 ng mL(-1) for sertraline, imipramine, paroxetine, mirtazapine and clomipramine. The intra-assay and inter-assay precision and accuracy were studied at three concentrations (50, 200, and 500 ng mL(-1)). The intra-assay coefficients of variation (CVs) for all compounds were less than 8.8%, and all inter-CVs were less than 10%. Limits of quantification were 2.5 ng mL(-1) for moclobemide, 5 ng mL(-1) for citalopram, duloxetine and amitriptyline, and 10 ng mL(-1) for mirtazapine, paroxetine, imipramine, fluoxetine, sertraline, and clomipramine. No interference of the drugs normally associated with antidepressants was observed. The method has been successfully applied to the analysis of real samples, for the drug monitoring of ten frequently prescribed tricyclic and non-tricyclic antidepressant drugs.
本文介绍了一种新型高效液相色谱法，用于测定10种常用的三环和非三环抗抑郁药：丙咪嗪、阿米替林、氯米帕明、氟西汀、舍曲林、帕罗西汀、西酞普兰、米氮平、吗氯贝胺和度洛西汀。简单准确的样品制备步骤包括液 - 液萃取，回收率在72%至86%之间，但吗氯贝胺除外（59%）。在等度条件下使用反相Select B柱进行分离，并采用紫外检测（230 nm）。流动相由35%的乙腈/甲醇混合物（92:8，v/v）和65%的0.25 mol L(-1)醋酸钠缓冲液（pH 4.5）组成。吗氯贝胺的标准曲线在2.5 - 1000 ng mL(-1)的工作范围内呈线性，西酞普兰、度洛西汀、氟西汀在5 - 2000 ng mL(-1)呈线性，舍曲林、丙咪嗪、帕罗西汀、米氮平和氯米帕明在10 - 2000 ng mL(-1)呈线性。在三个浓度（50、200和500 ng mL(-1)）下研究了批内和批间精密度与准确度。所有化合物的批内变异系数（CVs）均小于8.8%，所有批间CVs均小于10%。吗氯贝胺的定量限为2.5 ng mL(-1)，西酞普兰、度洛西汀和阿米替林为5 ng mL(-1)，米氮平、帕罗西汀、丙咪嗪、氟西汀、舍曲林和氯米帕明为10 ng mL(-1)。未观察到通常与抗抑郁药相关的药物干扰。该方法已成功应用于实际样品分析，用于监测10种常用三环和非三环抗抑郁药的药物情况。
