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Quantitative Determination of Methohexital in Human Whole Blood by Liquid Chromatography Tandem Mass Spectrometry
Journal of Chromatographic Science ( IF 1.3 ) Pub Date : 2021-03-27 , DOI: 10.1093/chromsci/bmab024
Yi Zhang, Yunfeng Zhang, Chunfeng Zhai

A rapid, simple and sensitive liquid chromatography tandem mass spectrometry method for the determination of methohexital in human whole blood was developed and validated. Ethyl acetate/n-hexane (9:1) was used as extraction solvent while aprobarbital was used as internal standard. Methohexital was recovered by liquid–liquid extraction from 100 μL of human whole blood. The mobile phase was water-acetonitrile, and an ACQUITY BEH C18 (2.1 × 100 mm, 1.7 μm) column was adopted. Negative electrospray ionization source and multiply reaction monitoring mode were applied. The transitions of m/z were 261.2/42.2 and 261.2/119.0 for methohexital. The limit of detection was 0.5 ng/mL, which was lower than the previous methods. Wide linear range (2–2,000 ng/mL) with a good correlation coefficient (r > 0.99) was also obtained. The intra- and inter- day precisions represented by relative standard deviation were <11.5%, and the recoveries were >79.67%. This analytical method involved small sample volume and had been proven to be rapid, easy, sensitive and specific. Therefore, it could be used for the clinical analysis of methohexital.

中文翻译:

液相色谱串联质谱法定量测定人全血中的甲己糖

建立并验证了一种快速、简便、灵敏的液相色谱串联质谱法测定人全血中甲己酮的方法。乙酸乙酯/正己烷 (9:1) 用作萃取溶剂,而阿普巴比妥用作内标。通过从 100 μL 人全血中的液-液萃取法回收美索西妥。流动相为水-乙腈,采用 ACQUITY BEH C18 (2.1 × 100 mm, 1.7 μm) 色谱柱。采用负电喷雾离子源和多反应监测模式。m/z 的离子对为 261.2/42.2 和 261.2/119.0,methohexital。检测限为 0.5 ng/mL,低于之前的方法。还获得了具有良好相关系数 (r > 0.99) 的宽线性范围 (2–2,000 ng/mL)。以相对标准偏差表示的日内和日间精密度<11.5%,回收率>79.67%。这种分析方法涉及的样品量很小,并且已被证明是快速、简单、灵敏和特异性的。因此,可用于美索妥的临床分析。
更新日期:2021-03-27
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