Johansson E, Norén K, Sjövall J, Halldin M M
Department of Pharmacognosy, Uppsala University, Sweden.
Biomed Chromatogr. 1989 Jan;3(1):35-8. doi: 10.1002/bmc.1130030109.
A gas chromatographic-mass spectrometric (GC/MS) method for analysis of delta 1-tetrahydrocannabinol (delta 1-THC) in human fat samples is described. The fat sample, obtained from heavy marihuana users 1 week before and 4 weeks after smoking, is homogenized in hexane + 2-propanol, centrifuged, and the supernatant mixed with Lipidex 5000. The solvent is evaporated and the dried gel is packed in a glass column. delta 1-THC is eluted from the column with methanol + water + acetic acid, diluted with water and the eluent is passed through a bed of Octadecylsilane-bonded silica. After washing and drying, the retained delta 1-THC is eluted with hexane, derivatized with N-methyl-N-(t-butyl-dimethysilyl)trifluoroacetamide (MTBSTFA) and finally purified by HPLC on an Octadecyl Sl 100 column in methanol. The amount of delta 1-THC is determined by GC/MS, using selected ion monitoring, and a deuterated internal standard. The recovery of delta 1-THC is about 80%, and the concentration of delta 1-THC in the fat samples analysed ranged between 0.4 and 193 ng/g wet tissue.
描述了一种用于分析人体脂肪样品中δ1-四氢大麻酚（δ1-THC）的气相色谱-质谱（GC/MS）方法。从重度大麻使用者吸烟前1周和吸烟后4周获取的脂肪样品，在己烷 + 2-丙醇中匀浆，离心，上清液与Lipidex 5000混合。蒸发溶剂，将干燥的凝胶装入玻璃柱。用甲醇 + 水 + 乙酸从柱中洗脱δ1-THC，用水稀释，洗脱液通过十八烷基硅烷键合硅胶柱床。洗涤并干燥后，用己烷洗脱保留的δ1-THC，用N-甲基-N-（叔丁基-二甲基硅烷基）三氟乙酰胺（MTBSTFA）衍生化，最后在甲醇中的十八烷基Sil 100柱上通过HPLC纯化。使用选择离子监测和氘代内标通过GC/MS测定δ1-THC的含量。δ1-THC的回收率约为80%，所分析的脂肪样品中δ1-THC的浓度范围为0.4至193 ng/g湿组织。
