液相色谱-串联质谱法测定口腔液中麦角酸二乙酰胺（LSD）和2-氧代-3-羟基-LSD的高灵敏度方法

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

作者信息

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

机构信息

Campinas Poison Control Center, University of Campinas, Campinas, São Paulo, 13083‑859, Brazil.

Faculty of Medical Sciences, University of Campinas, Campinas, São Paulo, 13083‑859, Brazil.

出版信息

Forensic Toxicol. 2022 Jul;40(2):322-331. doi: 10.1007/s11419-022-00622-0. Epub 2022 Apr 12.

DOI:10.1007/s11419-022-00622-0

PMID:36454414

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.

摘要

目的

我们开发并验证了一种高灵敏度方法，用于使用液液萃取和液相色谱 - 串联质谱法（LC - MS/MS）对口腔液样本中的麦角酸二乙酰胺（LSD）和2-氧代-3-羟基-LSD（OH-LSD）进行定量。该方法应用于42份真实口腔液样本中这两种物质的定量分析。

方法

使用500μL每份样本（使用Quantisal™装置采集的口腔液样本）和二氯甲烷/异丙醇混合物（1:1，v/v）进行液液萃取。评估了酶促水解以裂解葡萄糖醛酸代谢物。

结果

LSD和OH-LSD的定量限均为0.01 ng/mL。在0.01至5 ng/mL之间评估了线性。两种分析物的不精密度和偏差均不高于10.2%。萃取回收率高于69%。分析物在自动进样器中于10°C下稳定24小时，在4°C和-20°C下稳定长达30天。该方法应用于42份口腔液样本的分析。所有样本中均检测到LSD（浓度在0.02至175 ng/mL之间），20份样本中检测到OH-LSD（浓度在0.01至1.53 ng/mL之间）。