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采用带氮磷检测的毛细管气液色谱法同时测定全血中氟西汀、阿米替林、去甲替林、曲米帕明、马普替林、氯米帕明和曲唑酮的比较性固相萃取研究。

A comparative solid-phase extraction study for the simultaneous determination of fluoxetine, amitriptyline, nortriptyline, trimipramine, maprotiline, clomipramine, and trazodone in whole blood by capillary gas-liquid chromatography with nitrogen-phosphorus detection.

作者信息

Martínez M A, Sánchez de la Torre C, Almarza E

机构信息

Department of Chemistry, National Institute of Toxicology, Ministry of Justice, C/ Luis Cabrera 9, 28002 Madrid, Spain.

出版信息

J Anal Toxicol. 2003 Sep;27(6):353-8. doi: 10.1093/jat/27.6.353.

Abstract

This paper reports the simultaneous detection of the seven antidepressants fluoxetine, amitriptyline, nortriptyline, trimipramine, maprotiline, clomipramine, and trazodone in whole blood at concentration levels of 100-2000 ng/mL by gas chromatography with a nitrogen-phosphorus detector (GC-NPD). A comparative and validation study using two solid-phase extraction (SPE) columns, Chem Elut and Bond Elut Certify, were developed regarding their recovery, precision, sensitivity, and matrix purification efficiency. The Chem Elut columns, a diatomaceous earth, are closely related to conventional liquid-liquid extraction. The Bond Elut Certify columns, more recently developed in the market, are a mixed SPE: reversed-phase and cation exchange sorbent. Recoveries of the compounds using Chem Elut columns at 500 ng/mL were in the range 30-50%, with intra- and interassay precisions of less than 9% and 17%, respectively. Limits of detection (LODs) and quantitation (LOQs) ranged from 13 to 146 ng/mL and from 44 to 485 ng/mL, respectively. Recoveries of the compounds using Bond Elut Certify columns at 500 ng/mL were in the range 59-84% with intra- and interassay precisions of less than 8% and 11%, respectively. LODs and LOQs ranged from 8 to 67 ng/mL and from 25 to 223 ng/mL, respectively. An excellent linearity was observed with both extraction procedures from the LOQs up to 2000 ng/mL. Higher recoveries, cleaner extracts, better sensitivity, better precision, and less solvent consumption and disposal were achieved for the screening of these antidepressants with the use of the mixed SPE Bond Elut Certify compared with Chem Elut columns.

摘要

本文报道了采用带氮磷检测器(GC-NPD)的气相色谱法,同时检测全血中浓度为100 - 2000 ng/mL的七种抗抑郁药,即氟西汀、阿米替林、去甲替林、曲米帕明、马普替林、氯米帕明和曲唑酮。开展了一项对比和验证研究,使用两种固相萃取(SPE)柱,即Chem Elut柱和Bond Elut Certify柱,考察它们在回收率、精密度、灵敏度和基质净化效率方面的表现。Chem Elut柱是一种硅藻土柱,与传统液液萃取密切相关。Bond Elut Certify柱是市场上较新开发的产品,是一种混合SPE柱:反相和阳离子交换吸附剂。使用Chem Elut柱在500 ng/mL时,化合物的回收率在30% - 50%之间,批内和批间精密度分别小于9%和17%。检测限(LOD)和定量限(LOQ)分别为13至146 ng/mL和44至485 ng/mL。使用Bond Elut Certify柱在500 ng/mL时,化合物的回收率在59% - 84%之间,批内和批间精密度分别小于8%和11%。LOD和LOQ分别为8至67 ng/mL和25至223 ng/mL。两种萃取方法从LOQ到2000 ng/mL均观察到良好的线性。与Chem Elut柱相比,使用混合SPE Bond Elut Certify柱筛选这些抗抑郁药时,回收率更高、提取物更纯净、灵敏度更高、精密度更好,且溶剂消耗和处理更少。

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