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基于乙酸盐的多分析物加合物形成在液相色谱-串联质谱法法医毒理学信号分离定量中的应用——以水杨酸作为模型药物的讨论

Application of combined acetate salt based multiple analyte adduct formation in signal separated quantification performed for the purposes of forensic toxicology with liquid chromatography-tandem mass spectrometry - Discussion on the basis of salicylic acid applied as a model drug.

作者信息

Dziadosz Marek

机构信息

Institute of Legal Medicine, Hannover Medical School (MHH), Carl-Neuberg-Str. 1, D-30625 Hannover, Germany.

出版信息

Forensic Sci Int. 2019 Apr;297:249-253. doi: 10.1016/j.forsciint.2019.02.025. Epub 2019 Feb 22.

DOI:10.1016/j.forsciint.2019.02.025
PMID:30849692
Abstract

In this work the examination of analyte adduct formation by the application of both sodium acetate and lithium acetate was performed with salicylic acid used as a model drug. Additionally, on the basis of combined acetate salt based multiple analyte adduct ions it was aimed to investigate the generation of different analyte precursor ions and their application in signal separated quantification with liquid chromatography-tandem mass spectrometry. Adduct identification experiments were performed by infusion experiments and resulted in an optimised detection of analyte adduct ions with lithium acetate, sodium acetate and combined lithium acetate/sodium acetate. Sample preparation based on a fast protein precipitation with a methanol solution containing lithium acetate and sodium acetate. A Luna 5 μm C18 (2) 100 A, 150 mm × 2 mm analytical column and a mobile phase composed of an HO/methanol = 3%/97% (v/v) solution with 10 mmol l ammonium acetate and 0.1% acetic acid were used for chromatographic purposes. The linearity was investigated in the range of 5-500 μg/ml. The limit of detection (LOD of 1.2 μg/ml) and quantification (LOQ 4.0 μg/ml) together with other results of validation experiments revealed that this strategy can be applied for salicylic acid quantification.

摘要

在这项工作中,以水杨酸作为模型药物,通过应用醋酸钠和醋酸锂来检测分析物加合物的形成。此外,基于基于醋酸盐的多种分析物加合物离子,旨在研究不同分析物前体离子的产生及其在液相色谱 - 串联质谱信号分离定量中的应用。通过输注实验进行加合物鉴定实验,结果实现了对醋酸锂、醋酸钠以及醋酸锂/醋酸钠组合的分析物加合物离子的优化检测。基于用含有醋酸锂和醋酸钠的甲醇溶液进行快速蛋白质沉淀的样品制备方法。使用Luna 5μm C18(2) 100Å、150mm×2mm分析柱以及由HO/甲醇 = 3%/97% (v/v) 溶液与10mmol l醋酸铵和0.1%醋酸组成的流动相进行色谱分析。在5 - 500μg/ml范围内研究线性。检测限(LOD为1.2μg/ml)和定量限(LOQ为4.0μg/ml)以及其他验证实验结果表明,该策略可用于水杨酸的定量分析。

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