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UHPLC-QqQ-MS/MS 法在人死后标本中β-肾上腺素阻断剂(β-阻滞剂)定量分析中的应用。

Application of UHPLC-QqQ-MS/MS Method for Quantification of Beta-Adrenergic Blocking Agents (β-Blockers) in Human Postmortem Specimens.

机构信息

Department of Forensic Medicine, Wroclaw Medical University, 4 J. Mikulicza-Radeckiego Street, 50345 Wroclaw, Poland.

Institute of Toxicology Research, 45 Kasztanowa Street, 55093 Borowa, Poland.

出版信息

Molecules. 2024 Sep 27;29(19):4585. doi: 10.3390/molecules29194585.

Abstract

Betablockers are one of the most frequently used medications in cardiology. They can lead to fatal drops in blood pressure and heart rhythm disturbances. Death is functional, and poisoning with this group of drugs can be difficult to detect. The liquid-liquid extraction (LLE) method developed using ethyl acetate at pH 9 successfully identified 18 β-blockers in human blood. The method's limit of quantification (LOQ) was in the range of 0.1 to 0.5 ng/mL. No carryover of substances between samples was detected, and no interfering ion current signals were observed in the biological samples at the retention times of the compounds or internal standards. All compounds had a coefficient of determination (R) above 0.995. Intraday and interday precision (RSD%) and accuracy (RE%) for low and high QC levels were within 1.7-12.3% and -14.4 to 14.1%, respectively. Very good recovery (80.0-119.6%) and matrix effect (±20.0%) values were achieved for all compounds. In addition, fragmentation spectra were collected for all the examined substances, and high-resolution spectra were presented for landiolol and metipranolol, because they are not available in commercial HRMS spectra databases. The developed method was applied in authentic postmortem samples.

摘要

β受体阻滞剂是心脏病学中最常用的药物之一。它们可能导致致命的血压下降和心律紊乱。死亡是功能性的,并且这种药物组的中毒很难被检测到。使用乙酸乙酯在 pH 9 下开发的液-液萃取(LLE)方法成功地在人血中鉴定出 18 种β受体阻滞剂。该方法的定量下限(LOQ)在 0.1 至 0.5ng/mL 范围内。在样品之间未检测到物质的夹带,并且在化合物或内标物的保留时间处未观察到生物样品中的干扰离子电流信号。所有化合物的决定系数(R)均大于 0.995。低和高 QC 水平的日内和日间精密度(RSD%)和准确度(RE%)分别在 1.7-12.3%和-14.4 至 14.1%之间。所有化合物均获得了非常好的回收率(80.0-119.6%)和基质效应(±20.0%)。此外,为所有检查的物质收集了碎片图谱,并为拉地洛尔和美替洛尔呈现了高分辨率图谱,因为它们在商业 HRMS 图谱数据库中不可用。所开发的方法已应用于真实的死后样本。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/25e8/11477679/61aad030570c/molecules-29-04585-g001a.jpg

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