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一种通过液相色谱-串联质谱法测定全血中大麻素的高效、稳健方法。

An Efficient, Robust Method for the Determination of Cannabinoids in Whole Blood by LC-MS-MS.

作者信息

Tiscione Nicholas B, Miller Russell, Shan Xiaoqin, Sprague Jessica, Yeatman Dustin Tate

机构信息

Palm Beach County Sheriff's Office, 3228 Gun Club Road, West Palm Beach, FL 33406, USA

Palm Beach County Sheriff's Office, 3228 Gun Club Road, West Palm Beach, FL 33406, USA.

出版信息

J Anal Toxicol. 2016 Oct;40(8):639-648. doi: 10.1093/jat/bkw063. Epub 2016 Jul 29.

DOI:10.1093/jat/bkw063
PMID:27474359
Abstract

Due to the high prevalence of cannabinoids in forensic toxicology casework, it is desirable to have an efficient method that uses a small volume of blood and requires a minimal sample preparation. Although many methods have been reported, they are often labor intensive, require special sample preparation materials, use 1 mL or more of specimen or are difficult to replicate. The liquid chromatography with tandem mass spectrometry (LC-MS-MS) method presented herein employs a rapid and simple liquid-liquid extraction, has been successfully applied in two different laboratories, uses 0.5 mL of specimen and was extensively validated. The validated limit of detection and limit of quantitation were 1 ng/mL for delta-9-tetrahydrocannabinol (THC) and 11-hydroxy-delta-9-tetrahydrocannabinol (OH-THC) and 5 ng/mL for 11-nor-9-carboxy-delta-9-tetrahydrocannabinol (THCA). Each analyte demonstrated a zero-order linear range (r > 0.990) with 1/x weighting of 1-40 ng/mL for THC and OH-THC and 5-200 ng/mL for THCA. The coefficient of variation of replicate analyses was within 14%. Bias was within ±13% of the prepared concentration. The validated method provides a sensitive, efficient and robust procedure for the quantitation of cannabinoids in blood using LC-MS-MS and a sample volume of 0.5 mL.

摘要

由于大麻素在法医毒理学案件检测中普遍存在,因此需要一种高效的方法,该方法使用少量血液且样品制备要求最低。尽管已经报道了许多方法,但它们通常劳动强度大,需要特殊的样品制备材料,使用1 mL或更多的样本,或者难以重复。本文介绍的液相色谱-串联质谱(LC-MS-MS)方法采用快速简单的液-液萃取,已在两个不同实验室成功应用,使用0.5 mL样本,并经过广泛验证。δ-9-四氢大麻酚(THC)和11-羟基-δ-9-四氢大麻酚(OH-THC)的验证检测限和定量限均为1 ng/mL,11-去甲-9-羧基-δ-9-四氢大麻酚(THCA)的验证检测限和定量限均为5 ng/mL。每种分析物在1-40 ng/mL(THC和OH-THC)和5-200 ng/mL(THCA)的1/x加权下均呈现零级线性范围(r > 0.990)。重复分析的变异系数在14%以内。偏差在制备浓度的±13%以内。该验证方法为使用LC-MS-MS和0.5 mL样本体积定量血液中的大麻素提供了一种灵敏、高效且稳健的程序。

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