Laboratory of Forensic Toxicology, Department of Biomedical, Surgical and Dental Science, via Luigi Mangiagalli 37, 20133 Milan, Italy.
J Pharm Biomed Anal. 2018 Jun 5;155:1-6. doi: 10.1016/j.jpba.2018.03.031. Epub 2018 Mar 16.
THC, CBD, CBN, THC-COOH and 11-OH-THC are the most popular markers of cannabis consumption and abuse. The use of this drug is a serious social problem worldwide. In this study, a method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) operated in electron ionization (EI) with simple and rapid liquid-liquid extraction (LLE) and derivatization was developed and validated for the simultaneous determination of THC, CBD, CBN and 11-OH-THC in hair samples. The detection of all compounds was based on multiple reaction monitoring (MRM) transitions. The most important advantage of this method is the single-step, quick, easy and effective sample extraction procedure for THC, CBD, CBN and 11-OH-THC. The method showed a good linearity with a correlation coefficient (r) between 0.997 and 0.999 for all substances. The variation coefficient (%CV) was <5% for THC, 11-OH-THC and CBD and <13% for CBN. The limit of detection (LOD) was 0.03 pg/mg for 11-OH-THC and it ranged from 0.3 to 1.4 pg/mg for THC, CBD and CBN. The limit of quantification was 0.1 pg/mg for 11-OH-THC and it ranged from 0.9 to 4.7 pg/mg for THC, CBD and CBN. Analytical recovery was higher than 88% for 11-OH-THC and it ranged between 68 and 97% for THC, CBD and CBN. Intra- and inter-assay precision and accuracy were always lower than 9-14% and 5-9%, respectively. In parallel, we have quantified the THC-COOH level, following the methods previously set-up by us. The whole procedure was successfully applied to more than 200 different hair samples from cannabis consumers, disclosing the presence of 11-OH-THC in a range between 0.2 pg/mg and 27 pg/mg, and the presence of THC-COOH in a range between 0.05 pg/mg and 42.05 pg/mg. These data provided a good start towards the use of 11-THC-OH as alternative hair biomarker of cannabis consumption.
大麻素(THC)、大麻二酚(CBD)、大麻环萜酚(CBN)、四氢大麻酸(THC-COOH)和 11-羟基-四氢大麻酚(11-OH-THC)是最常用于检测大麻使用和滥用的标志物。该药物的使用是全球范围内一个严重的社会问题。在这项研究中,开发并验证了一种基于气相色谱-串联质谱(GC-MS/MS)的方法,该方法在电子电离(EI)模式下操作,采用简单快速的液-液萃取(LLE)和衍生化方法,用于同时检测头发样本中的 THC、CBD、CBN 和 11-OH-THC。所有化合物的检测均基于多重反应监测(MRM)转换。该方法的一个重要优势是 THC、CBD、CBN 和 11-OH-THC 的单步、快速、简单、有效的样品提取程序。该方法对所有物质均表现出良好的线性,相关系数(r)在 0.997 到 0.999 之间。THC、11-OH-THC 和 CBD 的变异系数(%CV)均<5%,CBN 的变异系数(%CV)均<13%。11-OH-THC 的检测限(LOD)为 0.03pg/mg,THC、CBD 和 CBN 的检测限(LOD)范围为 0.3 到 1.4pg/mg。11-OH-THC 的定量限(LOQ)为 0.1pg/mg,THC、CBD 和 CBN 的定量限(LOQ)范围为 0.9 到 4.7pg/mg。11-OH-THC 的分析回收率高于 88%,THC、CBD 和 CBN 的分析回收率范围在 68%到 97%之间。内标和日间精密度和准确度始终低于 9-14%和 5-9%。同时,我们根据我们之前建立的方法对 THC-COOH 水平进行了定量。整个过程成功应用于 200 多个来自大麻使用者的不同头发样本,结果显示 11-OH-THC 的浓度范围在 0.2pg/mg 到 27pg/mg 之间,THC-COOH 的浓度范围在 0.05pg/mg 到 42.05pg/mg 之间。这些数据为将 11-THC-OH 作为大麻使用的替代毛发生物标志物的使用提供了良好的开端。