High-sensitivity method for the determination of LSD and 2-oxo-3-hydroxy-LSD in oral fluid by liquid chromatography‒tandem mass spectrometry.

IF 2.8 4区医学 Q2 TOXICOLOGY

Forensic Toxicology Pub Date : 2022-07-01 DOI:10.1007/s11419-022-00622-0

Kelly Francisco da Cunha, Julia Martinelli Magalhães Kahl, Taís Regina Fiorentin, Karina Diniz Oliveira, Jose Luiz Costa

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引用次数: 0

Abstract

Purpose: We have developed and validated a high-sensitivity method to quantify lysergic acid diethylamide (LSD) and 2-oxo-3-hydroxy-LSD (OH-LSD) in oral fluid samples using liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC‒MS/MS). The method was applied to the quantification of both substances in 42 authentic oral fluid samples.

Methods: A liquid-liquid extraction was performed using 500 µL each of samples (oral fluid samples collected using Quantisal™ device) and dichloromethane/isopropanol mixture (1:1, v/v). Enzymatic hydrolysis was evaluated to cleave glucuronide metabolites.

Results: The limit of quantification was 0.01 ng/mL for both LSD and OH-LSD. The linearity was assessed between 0.01 and 5 ng/mL. Imprecision and bias were not higher than 10.2% for both analytes. Extraction recovery was higher than 69%. The analytes were stable in the autosampler at 10 °C for 24 h, and up to 30 days at 4 and -20 °C. The method was applied to the analysis of 42 oral fluid samples. LSD was detected in all samples (concentrations between 0.02 and 175 ng/mL), and OH-LSD was detected in 20 samples (concentrations between 0.01 and 1.53 ng/mL).

Conclusions: A high-sensitive method was fully validated and applied to authentic samples. To our knowledge, this is the first work to report concentrations of LSD and OH-LSD in authentic oral fluid samples.

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液相色谱-串联质谱法测定口服液中LSD和2-氧-3-羟基LSD的高灵敏度。

目的:建立并验证了液-液萃取-液相色谱-串联质谱(LC-MS /MS)定量口服液样品中麦角酸二乙胺(LSD)和2-氧-3-羟基LSD (OH-LSD)的高灵敏度方法。将该方法应用于42份正宗口服液样品中这两种物质的定量分析。方法:各样品(口服液样品采用Quantisal™装置采集)500µL，二氯甲烷/异丙醇混合物(1:1,v/v)进行液-液萃取。评价酶解对葡萄糖醛酸代谢产物的裂解作用。结果:LSD和OH-LSD的定量限均为0.01 ng/mL。在0.01 ~ 5 ng/mL之间进行线性评价。两种分析物的不精密度和偏差均不高于10.2%。提取回收率大于69%。分析物在10°C自动进样器中稳定24小时，在4°C和-20°C下可达30天。将该方法应用于42份口腔液体样本的分析。所有样品中均检测到LSD(浓度在0.02 ~ 175 ng/mL之间)，20个样品中检测到OH-LSD(浓度在0.01 ~ 1.53 ng/mL之间)。结论:该方法灵敏度高，可用于真实样品。据我们所知，这是第一次报道在真实口服液样本中LSD和OH-LSD浓度的工作。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Forensic Toxicology TOXICOLOGY-

CiteScore

5.80

自引率

9.10%

发文量

审稿时长

3 months

期刊介绍： The journal Forensic Toxicology provides an international forum for publication of studies on toxic substances, drugs of abuse, doping agents, chemical warfare agents, and their metabolisms and analyses, which are related to laws and ethics. It includes original articles, reviews, mini-reviews, short communications, and case reports. Although a major focus of the journal is on the development or improvement of analytical methods for the above-mentioned chemicals in human matrices, appropriate studies with animal experiments are also published. Forensic Toxicology is the official publication of the Japanese Association of Forensic Toxicology (JAFT) and is the continuation of the Japanese Journal of Forensic Toxicology (ISSN 0915-9606).