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使用半自动样品制备和液相色谱-串联质谱检测法高灵敏度测定小鼠血浆中的丙戊酸。

High sensitivity determination of valproic acid in mouse plasma using semi-automated sample preparation and liquid chromatography with tandem mass spectrometric detection.

作者信息

Pucci Vincenzo, Monteagudo Edith, Bonelli Fabio

机构信息

Istituto di Ricerche di Biologia Molecolare P. Angeletti, Merck Sharp and Dohme Research Laboratories, Via Pontina km 30.600, 00040 Pomezia, Roma, Italy.

出版信息

Rapid Commun Mass Spectrom. 2005;19(24):3713-8. doi: 10.1002/rcm.2249.

DOI:10.1002/rcm.2249
PMID:16299698
Abstract

A high-throughput liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) assay using automated sample preparation has been developed for the determination of valproic acid (VPA) in mouse plasma. A liquid-handling system was programmed to prepare calibration standard solutions in plasma, as well as quality controls and clinical samples. Plasma protein precipitation was performed on a 96-well plate, and the collected supernatant was directly injected into a reversed-phase LC/ESI-MS/MS system in the negative ionization mode. The calibration curve for VPA was linear over a dynamic range of 0.15-100 microg/mL. The limit of detection was 75 ng/mL and the lower limit of quantitation was 150 ng/mL. Intra- and inter-day validation assays of the semi-automated plasma analysis showed satisfactory accuracy and precision.

摘要

已开发出一种使用自动样品制备的高通量液相色谱/电喷雾电离串联质谱(LC/ESI-MS/MS)分析法,用于测定小鼠血浆中的丙戊酸(VPA)。编写了一个液体处理系统程序,以制备血浆中的校准标准溶液以及质量控制样品和临床样品。在96孔板上进行血浆蛋白沉淀,收集的上清液直接注入反相LC/ESI-MS/MS系统的负离子模式下。VPA的校准曲线在0.15 - 100μg/mL的动态范围内呈线性。检测限为75 ng/mL,定量下限为150 ng/mL。半自动血浆分析的日内和日间验证分析显示出令人满意的准确度和精密度。

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