固相萃取法从人尿中分离五种常见抗抑郁药，用于 HPLC-DAD 分析。
Fabric phase sorptive extraction for the isolation of five common antidepressants from human urine prior to HPLC-DAD analysis.
机构信息
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, GR-54124 Thessaloniki, Greece.
International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL, USA.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Jun 15;1118-1119:171-179. doi: 10.1016/j.jchromb.2019.04.045. Epub 2019 Apr 25.
An innovative fabric phase sorptive extraction-high performance liquid chromatography-diode array detection (FPSE-HPLC-DAD) method is developed and validated herein for the simultaneous extraction and analysis of five common antidepressants (venlafaxine, paroxetine, fluoxetine, amitriptyline, clomipramine) in human urine samples. Separation was obtained using a reverse phase column LiChroCART-LiChrospher®100 RP-8e (5 μm, 250 × 4 mm) with diode array detection monitoring at 235 nm. Gradient elution was applied at a flow rate of 1.2 mL/min with a mobile phase that consisted of acetonitrile and ammonium acetate (0.05 M). Fabric Phase Sorptive Extraction was evaluated for the first time with regards to the extraction of the examined antidepressants from human urine and proved to be a rapid, simple, environmentally friendly, efficient, and selective sample preparation approach. Sol-gel graphene sorbent, coated on cellulose FPSE media, were the most efficient among other with different polarities. The absolute recovery values were 25.5% for venlafaxine, 33.9% for paroxetine, 67.0% for fluoxetine, 43.0% for amitriptyline and 29.0% for clomipramine, while relative recoveries were higher than 90%. The developed method provides satisfactory limit of detection 0.15 ng/μL.
本文建立并验证了一种新颖的纤维增强相固相萃取-高效液相色谱-二极管阵列检测（FPSE-HPLC-DAD）方法，用于同时提取和分析人尿样中的五种常见抗抑郁药（文拉法辛、帕罗西汀、氟西汀、阿米替林、氯米帕明）。采用反相柱 LiChroCART-LiChrospher®100 RP-8e（5μm，250×4mm），以二极管阵列检测在 235nm 处监测，实现了分离。以乙腈和乙酸铵（0.05M）为流动相，在 1.2mL/min 的流速下进行梯度洗脱。首次评估了纤维增强相固相萃取法从人尿中提取所考察的抗抑郁药的情况，结果表明该方法是一种快速、简单、环保、高效、选择性的样品前处理方法。涂覆在纤维素 FPSE 介质上的溶胶-凝胶石墨烯吸附剂在不同极性的吸附剂中表现出最高的效率。文拉法辛的绝对回收率为 25.5%，帕罗西汀为 33.9%，氟西汀为 67.0%，阿米替林为 43.0%，氯米帕明为 29.0%，而相对回收率均高于 90%。所建立的方法提供了令人满意的检测限 0.15ng/μL。
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