On-line SPE LC-MS/MS for the quantification of Δ9-tetrahydrocannabinol (THC) and its two major metabolites in human peripheral blood by liquid chromatography tandem mass spectrometry
On-line SPE LC-MS/MS for the quantification of Δ9-tetrahydrocannabinol (THC) and its two major metabolites in human peripheral blood by liquid chromatography tandem mass spectrometry
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DOI：
10.1007/s00216-011-4708-x
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发表时间：
2011-04-01
影响因子：
4.3
通讯作者：
Weinmann, Wolfgang
中科院分区：
文献类型：
--
作者：
Koenig, Stefan;Aebi, Beat;Weinmann, Wolfgang
开发了一种用于测定人全血中Delta 9-四氢大麻酚（THC）及其两种代谢产物Delta 9-（11-OH）-四氢大麻酚（11-OH-THC）和11-去甲-Delta 9-羧基-四氢大麻酚（THC-COOH）的通用和稳健的分析方法，并验证了该方法可用于法医毒理学。将蛋白质沉淀、集成固相萃取和在线富集、高效液相色谱分离和三重四极杆质谱仪检测相结合。用于三种大麻素的线性范围对于THC和11-OH-THC为0.5至20 ng/mL，对于THC-COOH为2.5至100 ng/mL，因此涵盖法医用途的要求。所有三种分析物的相关系数均达到0.9980或更好。与我们之前的GC-MS方法相反，该方法未观察到THC-COOH葡萄糖醛酸苷的相关水解，这显然导致THC-COOH浓度的人为增加，因为在相转移催化甲基化步骤期间，葡萄糖醛酸苷-结合物在高pH值下发生水解。
A universal and robust analytical method for the determination of Delta 9-tetrahydrocannabinol (THC) and two of its metabolites Delta 9-(11-OH)-tetrahydrocannabinol (11-OH-THC) and 11-nor-Delta 9-carboxy-tetrahydrocannabinol (THC-COOH) in human whole blood was developed and validated for use in forensic toxicology. Protein precipitation, integrated solid phase extraction and on-line enrichment followed by high-performance liquid chromatography separation and detection with a triple quadrupole mass spectrometer were combined. The linear ranges used for the three cannabinoids were from 0.5 to 20 ng/mL for THC and 11-OH-THC and from 2.5 to 100 ng/mL for THC-COOH, therefore covering the requirements for forensic use. Correlation coefficients of 0.9980 or better were achieved for all three analytes. No relevant hydrolysis was observed for THC-COOH glucuronide with this procedure - in contrast to our previous GC-MS procedure, which obviously lead to an artificial increase of the THC-COOH concentration due to the hydrolysis of the glucuronide-conjugate occurring at high pH during the phase-transfer catalyzed methylation step.