National Institute of Scientific Investigation, 331-1 Shinwol 7-Dong, Yang-Chun Gu, Seoul, South Korea.
J Pharm Biomed Anal. 2011 Jul 15;55(5):1096-103. doi: 10.1016/j.jpba.2011.03.020. Epub 2011 Mar 21.
The present study describes a gas chromatography/tandem mass spectrometry-negative ion chemical ionization assay (GC/MS/MS-NCI) for simultaneous analysis of Δ(9)-tetrahydrocannabinol (THC) and 11-nor-9-carboxy-tetrahydrocannabinol (THCCOOH) in hair. Each hair sample, of approximately 20mg, was weighed and the sample was dissolved in 1ml of 1M sodium hydroxide (30min at 85°C) in the presence of THC-d(3) and THCCOOH-d(3). For the analysis of THC, hair samples were extracted with n-hexane:ethyl acetate (9:1) two times; acetic acid and sodium acetate buffer were added for the analysis of THCCOOH, and hair samples were re-extracted with n-hexane:ethyl acetate (9:1) two times. The extracts were then derivatized with pentafluoropropionic anhydride (PFPA) and pentafluoropropanol (PFPOH). This method allowed the analysis of THC and THCCOOH using the GC/MS/MS-NCI assay. This method was also fully validated and applied to hair specimens (n=54) collected from known cannabis users whose urine test results were positive. The concentrations of THC and THCCOOH in hair ranged from 7.52 to 60.41ng/mg and from 0.10 to 11.68pg/mg, respectively. In this paper, we simultaneously measured THC and THCCOOH in human hair using GC/MS/MS-NCI without requiring different sample preparation and derivatization procedures. The analytical sensitivity for THCCOOH in hair was good, while that for THC in hair needs to be improved in further study.
本研究描述了一种气相色谱/串联质谱-负化学电离(GC/MS/MS-NCI)法,用于同时分析头发中的 Δ(9)-四氢大麻酚(THC)和 11-去甲-9-羧基-四氢大麻酚(THCCOOH)。每个约 20mg 的头发样本称重后,在 30min 内于 85°C 下加入 THC-d(3) 和 THCCOOH-d(3),溶解于 1ml 1M 氢氧化钠中。对于 THC 的分析,头发样品用正己烷:乙酸乙酯(9:1)提取两次;对于 THCCOOH 的分析,加入乙酸和乙酸钠缓冲液,然后用正己烷:乙酸乙酯(9:1)再提取两次。然后用五氟丙酰基酐(PFPA)和五氟丙醇(PFPOH)对提取物进行衍生化。该方法允许使用 GC/MS/MS-NCI 测定法分析 THC 和 THCCOOH。该方法也经过全面验证,并应用于从尿液检测结果为阳性的已知大麻使用者采集的头发样本(n=54)。头发中 THC 和 THCCOOH 的浓度范围分别为 7.52-60.41ng/mg 和 0.10-11.68pg/mg。本文使用 GC/MS/MS-NCI 同时测量了人发中的 THC 和 THCCOOH,无需不同的样品制备和衍生化程序。头发中 THCCOOH 的分析灵敏度良好,而头发中 THC 的分析灵敏度需要在进一步研究中提高。