Quantitative measurement of delta 9-tetrahydrocannabinol and two major metabolites in physiological specimens using capillary column gas chromatography negative ion chemical ionization mass spectrometry.
Quantitative measurement of delta 9-tetrahydrocannabinol and two major metabolites in physiological specimens using capillary column gas chromatography negative ion chemical ionization mass spectrometry.
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使用毛细管柱气相色谱负离子化学电离质谱法定量测量生理标本中的 δ9-四氢大麻酚和两种主要代谢物。
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发表时间：
1983
期刊：
影响因子：
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通讯作者：
D. Chinn
中科院分区：
文献类型：
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作者：
R. Foltz;K. McGinnis;D. Chinn
delta 9-四氢大麻酚及其两种代谢物，11-羟基-delta 9-四氢大麻酚和11-对-9-羧基-delta 9-四氢大麻酚，可以通过一种新的检测方法在单个1毫升的血液、血浆或尿液样本中进行测量，该检测方法结合了毛细管柱气相色谱法和负离子化学电离质谱法的相对快速提取程序。每种大麻素的氘标记类似物被添加到生理标本中作为内标。从每个样品中获得两种提取物：含有δ 9-四氢大麻酚和11-羟基δ 9-四氢大麻酚的中性馏分和含有11-对-9-羧基δ 9-四氢大麻酚的酸性馏分。中性馏分经三氟乙酸酐处理衍生化；酸性部分先用bf3 -甲醇处理，然后与三氟乙酸酐反应。在电子俘获的化学电离条件下，衍生化的δ 9-四氢大麻酚和11-对-9-羧基δ 9-四氢大麻酚提供了丰富的分子阴离子，非常适合于选定的离子监测。ho - thc -三氟乙酸酯的负离子化学电离谱显示无分子阴离子。因此，羟基代谢物的定量是通过监测CF3CO2分子阴离子损失形成的片段离子来实现的。判定可靠测量限为：11-正9-羧基- δ 9-四氢大麻酚0.1 ng ml-1， δ 9-四氢大麻酚0.2 ng ml-1, 11-羟基- δ 9-四氢大麻酚0.5 ng ml-1。本文给出了四个应用该方法分析具有医学法律意义的标本的例子。
delta 9-Tetrahydrocannabinol and two of its metabolites, 11-hydroxy-delta 9-tetrahydrocannabinol and 11-nor-9-carboxy-delta 9-tetrahydrocannabinol, can be measured in a single 1-ml sample of blood, plasma, or urine by a new assay which combines a relatively rapid extraction procedure with capillary column gas chromatography and negative ion chemical ionization mass spectrometry. Deuterium-labeled analogs of each cannabinoid are added to the physiological specimen as internal standards. Two extracts are obtained from each sample: a neutral fraction containing delta 9-tetrahydrocannabinol and 11-hydroxy-delta 9-tetrahydrocannabinol, and an acid fraction containing 11-nor-9-carboxy-delta 9-tetrahydrocannabinol. The neutral fraction is derivatized by treatment with trifluoroacetic anhydride; the acid fraction is first treated with BF3-methanol followed by reaction with trifluoroacetic anhydride. Under electron-capture chemical ionization conditions the derivatized delta 9-tetrahydrocannabinol and 11-nor-9-carboxy-delta 9-tetrahydrocannabinol give abundant molecular anions ideally suited for selected ion monitoring. The negative ion chemical ionization spectrum of the HO-THC-trifluoroacetate shows no molecular anion. Consequently, quantitation of the hydroxy metabolite is achieved by monitoring a fragment ion formed by loss of CF3CO2 from its molecular anion. The limits of reliable measurement are judged to be 0.1 ng ml-1 for 11-nor-9-carboxy-delta 9-tetrahydrocannabinol, 0.2 ng ml-1 for delta 9-tetrahydrocannabinol and 0.5 ng ml-1 for 11-hydroxy-delta 9-tetrahydrocannabinol. Four examples are given of the application of the assay to the analysis of specimens of medico-legal importance.