A highly efficient liquid chromatography–tandem mass spectrometry (LC–MS/MS) assay for etomidate and etomidate acid in urine, liver and kidney

IF 1.3 4区 医学 Q4 PHARMACOLOGY & PHARMACY Journal of pharmacological and toxicological methods Pub Date : 2023-12-21 DOI:10.1016/j.vascn.2023.107490
Tian-Fu He , Huan-hui Zhu , Xian-wen Lin , Yuan-yuan Tian , Li-min Sun , Xu Guan , Hai-Yan Zhang , Li Tan , Song-cai Wang
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Abstract

Etomidate (ETO) is a highly-efficient drug that can induce anesthesia with increasing doses, thus subject to strict regulation. However, an accurate and efficient method for ETO intake detection is currently lacking. Therefore, this study developed a straightforward sample preparation method using LC-MS/MS to analyze ETO and its primary metabolite, etomidate acid (ETA), in urine, liver, and kidney samples. Snap frozen pig liver and kidney samples were ground into a fine powder. Then, all the biological samples, including human urine, pig liver and kidney tissues, were deproteinized using acetonitrile and filtered for analysis. The separation was achieved in 9.01 min with gradient elution. The calibration curves ranged from 0.5 to 50 ng/mL for ETO in urine and 0.5 to 50 ng/g in liver and kidney, while the curves ranged from 1 to 100 ng/mL for ETA in urine and 1 to 100 ng/g in liver and kidney. The correlation coefficients (R2) were greater than 0.9957. The Limit of detection (LOD) and limit of quantitation (LOQ) for ETO were 0.2 and 0.5 ng/mL in urine samples and 0.2 and 0.5 ng/g in liver and kidney samples, respectively. For ETA, the LOD and LOQ were 0.5 and 1 ng/mL in urine samples and 0.5 and 1 ng/g in liver and kidney samples. This method was assessed by validation parameters, including selectivity, intra- and inter-day precision and accuracy, recovery, matrix effect, dilution integrity and stability. It was successfully applied to a practical case, revealing ETO and ETA concentrations in urine of 1.01 and 5.58 μg/mL, in liver samples of 12.30 and 1.13 μg/g, and in kidney samples of 6.95 and 4.23 μg/g. This suggests that the method is suitable for routine forensic detection of illicit ETO abuse.

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尿液、肝脏和肾脏中依托咪酯和依托咪酯酸的高效液相色谱-串联质谱(LC-MS/MS)测定法。
依托咪酯(ETO)是一种高效药物,可通过增加剂量诱导麻醉,因此受到严格管制。然而,目前还缺乏一种准确、高效的方法来检测 ETO 的摄入量。因此,本研究开发了一种简单的样品制备方法,利用 LC-MS/MS 分析尿液、肝脏和肾脏样品中的 ETO 及其主要代谢物依托咪酯酸 (ETA)。将快速冷冻的猪肝和猪肾样品研磨成细粉。然后,用乙腈对所有生物样本(包括人尿、猪肝和猪肾组织)进行脱蛋白处理,过滤后进行分析。采用梯度洗脱,分离时间为 9.01 分钟。尿液中 ETO 的定标曲线范围为 0.5 至 50 ng/mL,肝脏和肾脏的定标曲线范围为 0.5 至 50 ng/g;尿液中 ETA 的定标曲线范围为 1 至 100 ng/mL,肝脏和肾脏的定标曲线范围为 1 至 100 ng/g。相关系数(R2)大于 0.9957。尿液样本中 ETO 的检出限(LOD)和定量限(LOQ)分别为 0.2 和 0.5 纳克/毫升,肝脏和肾脏样本中分别为 0.2 和 0.5 纳克/克。尿样中 ETA 的最低检出限和最低定量限分别为 0.5 和 1 纳克/毫升,肝脏和肾脏样品中的最低检出限和最低定量限分别为 0.5 和 1 纳克/克。该方法的验证参数包括选择性、日内和日间精密度和准确度、回收率、基质效应、稀释完整性和稳定性。结果表明,尿液中的ETO和ETA浓度分别为1.01和5.58 μg/mL,肝脏样品中的ETO和ETA浓度分别为12.30和1.13 μg/g,肾脏样品中的ETO和ETA浓度分别为6.95和4.23 μg/g。这表明该方法适用于非法 ETO 滥用的常规法医检测。
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来源期刊
Journal of pharmacological and toxicological methods
Journal of pharmacological and toxicological methods PHARMACOLOGY & PHARMACY-TOXICOLOGY
CiteScore
3.60
自引率
10.50%
发文量
56
审稿时长
26 days
期刊介绍: Journal of Pharmacological and Toxicological Methods publishes original articles on current methods of investigation used in pharmacology and toxicology. Pharmacology and toxicology are defined in the broadest sense, referring to actions of drugs and chemicals on all living systems. With its international editorial board and noted contributors, Journal of Pharmacological and Toxicological Methods is the leading journal devoted exclusively to experimental procedures used by pharmacologists and toxicologists.
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