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气相色谱-串联质谱法检测和定量人血和尿中新出现的药物依他喹酮

Analytical method for detection and quantification of new emerging drug etaqualone in human blood and urine by gas chromatography tandem mass spectrometry.

机构信息

Department of Forensic Analytical Toxicology, West China School of Basic Science and Forensic Medicine, Sichuan University, Chengdu, China.

Department of Legal Medicine, College of Basic Medical Sciences, Inner Mongolia Medical University, Hohhot, China.

出版信息

Leg Med (Tokyo). 2022 Nov;59:102125. doi: 10.1016/j.legalmed.2022.102125. Epub 2022 Jul 19.

DOI:10.1016/j.legalmed.2022.102125
PMID:35932525
Abstract

Analytical procedure for detection and quantification of etaqualone in human blood and urine using GC-MS/MS was established and applied to authentic human samples obtained from volunteers. A liquid-liquid extraction method was employed. Each 1.0 mL of blood or urine was alkalized and extracted with diethyl ether. The solvent layer was evaporated to dryness and reconstituted with methanol then analyzed by GC-MS/MS. linear relationships within the concentration range of 1-100 ng/mL were obtained in calibrators for both blood and urine, demonstrating correlation coefficients values being>0.999. For blood and urine samples, the intra-day assay precision and accuracy values are each less than 3.65%, 7.13%, and 6.02%, 9.12%; those values of the inter-day assay are each less than 1.82%, 6.74%, and 3.99%, 7.41%. The extraction recovery rates for etaqualone ranged from 98.7% to 106%. The lower limit of quantifications was 1.0 ng/mL in both blood and urine. Stabilities of etaqualone in blood and urine were satisfactory under various temperatures within 15 days. 8.51 and 2.06 ng/mL of etaqualone in blood and urine were detected at 4 h later oral ingestion; 6.91 and 3.94 ng/mL of etaqualone were also detected 30 min and 2 h later smoking from blood and urine.

摘要

建立了一种使用 GC-MS/MS 检测和定量人血和尿中依他喹酮的分析方法,并将其应用于从志愿者获得的真实人体样本。采用液液萃取法。将 1.0mL 的血液或尿液碱化,用二乙醚提取。将溶剂层蒸发至干燥,用甲醇重新溶解,然后用 GC-MS/MS 分析。在血液和尿液校准器中,浓度范围为 1-100ng/mL 内均获得线性关系,相关系数值均>0.999。对于血液和尿液样本,日内测定精密度和准确度值均小于 3.65%、7.13%和 6.02%、9.12%;日间测定值均小于 1.82%、6.74%和 3.99%、7.41%。依他喹酮的提取回收率范围为 98.7%-106%。血液和尿液中的定量下限均为 1.0ng/mL。依他喹酮在血液和尿液中的稳定性在 15 天内各种温度下均令人满意。口服 4 小时后,血液和尿液中分别检测到 8.51 和 2.06ng/mL 的依他喹酮;从血液和尿液中也检测到 30 分钟和 2 小时后吸烟的 6.91 和 3.94ng/mL 的依他喹酮。

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