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一种用于测定全血中氨磺必利的经过验证的气相色谱/质谱法。

A validated GC/MS method for the determination of amisulpride in whole blood.

作者信息

Papoutsis Ioannis, Rizopoulou Anna, Nikolaou Panagiota, Pistos Constantinos, Spiliopoulou Chara, Athanaselis Sotiris

机构信息

Department of Forensic Medicine and Toxicology, Faculty of Medicine, National and Kapodistrian University of Athens, 75 Mikras Asias, Athens 115 27, Greece.

Department of Forensic Medicine and Toxicology, Faculty of Medicine, National and Kapodistrian University of Athens, 75 Mikras Asias, Athens 115 27, Greece.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Feb 1;947-948:111-6. doi: 10.1016/j.jchromb.2013.12.024. Epub 2013 Dec 26.

DOI:10.1016/j.jchromb.2013.12.024
PMID:24412693
Abstract

A sensitive GC/MS method for the determination of amisulpride in whole blood was developed, optimized and validated. Sample preparation included solid-phase extraction using HF Bond Elut C18 cartridges and further derivatization with heptafluorobutyric anhydride (HFBA). The limits of detection and quantification were 3.00 and 10.0 μg/L, respectively. The calibration curves were linear up to 1000 μg/L (R(2)≥0.991). Absolute recovery ranged from 94.2 to 101%. Accuracy was found to be between -8.7 and 1.9% and imprecision was less than 10.0%. The developed method covers the generally accepted therapeutic range but it can also cover levels above them. This makes our method suitable for the determination of amisulpride not only for clinical purposes on psychiatric patients, but also during the investigation of forensic cases where amisulpride is involved.

摘要

建立、优化并验证了一种灵敏的气相色谱/质谱联用(GC/MS)法用于测定全血中的氨磺必利。样品制备包括使用HF Bond Elut C18柱进行固相萃取,并用七氟丁酸酐(HFBA)进一步衍生化。检测限和定量限分别为3.00和10.0 μg/L。校准曲线在高达1000 μg/L范围内呈线性(R(2)≥0.991)。绝对回收率在94.2%至101%之间。准确度在-8.7%至1.9%之间,精密度小于10.0%。所建立的方法涵盖了普遍接受的治疗范围,但也能涵盖高于该范围的水平。这使得我们的方法不仅适用于精神病患者临床目的的氨磺必利测定,也适用于涉及氨磺必利的法医案件调查。

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