Park Meejung, Kim Jihyun, Park Yuran, In Sanghwan, Kim Eunmi, Park Yonghoon
Drug and Forensic Toxicology Division, National Forensic Service, 10 Ipchunro, Wonju, Kangwon-do 220-170, Republic of Korea.
Drug and Forensic Toxicology Division, National Forensic Service, 10 Ipchunro, Wonju, Kangwon-do 220-170, Republic of Korea.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Feb 1;947-948:179-85. doi: 10.1016/j.jchromb.2013.12.036. Epub 2014 Jan 2.
Hair analysis has been regarded as an alternative method to urine analysis in forensic and criminal cases. Cannabis (marijuana) is one of the most widely used drugs in the world and it has been controlled in South Korea since 1976. Identification of 11-nor-9-carboxy-tetrahydrocannabinol (THCCOOH) in hair can be an important proof of cannabis use because it can exclude the possibility of passive cannabis smoke exposure. In this study, we described a quantitative method of THCCOOH in hair using simple liquid-liquid extraction (LLE), selective column switching liquid chromatography with electrospray ionization (ESI)-MS(3). For the column switching system three columns (precolumn, trap column and analytical column) were used. Valve switch from the precolumn to the trap column was set from 3.0 to 4.0 min because THCCOOH appeared around 3.5 min with this precolumn. After 4.0 min the valve was switched to the original position and the analytes in the trap column were eluted onto the analytical column. Resolution occurred in this column and eluted into the ESI-MS(3) system. The internal standard was THCCOOH-d3. We used ESI-negative-MS(3) transition of ions at m/z 343 to 299 to 245 (343/299/245) and m/z 346 to 302 to 248 (346/302/248) for quantification of THCCOOH and THCCOOH-d3, respectively. The validation results of selectivity, matrix effect, recovery, linearity, precision and accuracy, and processed sample stability were satisfactory. The limit of detection (LOD) was 0.05 pg/mg and the limit of quantification (LOQ) was 0.10 pg/mg. The range of concentration of THCCOOH from 98 authentic human hair was 0.13-15.75 pg/mg. This method was successfully applied in the analysis of authentic human hair samples.
在法医和刑事案件中，毛发分析被视为尿液分析的一种替代方法。大麻是世界上使用最广泛的毒品之一，自1976年起在韩国受到管制。毛发中11-去甲-9-羧基-四氢大麻酚（THCCOOH）的鉴定可作为使用大麻的重要证据，因为它可以排除被动接触大麻烟雾的可能性。在本研究中，我们描述了一种使用简单液液萃取（LLE）、具有电喷雾电离（ESI）-MS(3)的选择性柱切换液相色谱法对毛发中THCCOOH进行定量的方法。对于柱切换系统，使用了三根柱子（预柱、捕集柱和分析柱）。预柱到捕集柱的阀切换设置为3.0至4.0分钟，因为在此预柱条件下THCCOOH在3.5分钟左右出现。4.0分钟后，阀切换回原始位置，捕集柱中的分析物被洗脱到分析柱上。在该柱上实现分离，然后洗脱进入ESI-MS(3)系统。内标为THCCOOH-d3。我们分别使用m/z 343至299至245（343/299/245）和m/z 346至302至248（346/302/248）的ESI负离子-MS(3)离子跃迁对THCCOOH和THCCOOH-d3进行定量。选择性、基质效应、回收率、线性、精密度和准确度以及处理后样品稳定性的验证结果均令人满意。检测限（LOD）为0.05 pg/mg，定量限（LOQ）为0.10 pg/mg。98份真实人发中THCCOOH的浓度范围为0.13 - 15.75 pg/mg。该方法成功应用于真实人发样品的分析。
