Simultaneous quantification of major cannabinoids and metabolites in human urine and plasma by HPLC-MS/MS and enzyme-alkaline hydrolysis

被引:53
作者
Aizpurua-Olaizola, Oier [1 ]
Zarandona, Iratxe [1 ]
Ortiz, Laura [1 ]
Navarro, Patricia [1 ]
Etxebarria, Nestor [1 ]
Usobiaga, Aresatz [1 ]
机构
[1] Univ Basque Country UPV EHU, Analyt Chem Dept, Barrio Sarriena S-N, Leioa 48940, Basque Country, Spain
关键词
cannabinoids and metabolites; plasma and urine analysis; enzymatic-alkaline glucuronide hydrolysis; high performance liquid chromatography-mass spectrometry; solid-phase extraction; CHROMATOGRAPHY-MASS SPECTROMETRY; SOLID-PHASE EXTRACTION; LIQUID-CHROMATOGRAPHY; DELTA(9)-TETRAHYDROCANNABINOL; CANNABIDIOL; EXPOSURE; PLANTS; BLOOD; THC; MS;
D O I
10.1002/dta.1998
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) method for simultaneous quantification of 9-tetrahydrocannabinol (THC), its two metabolites 11-hydroxy-9-tetrahydrocannabinol (11-OH-THC) and 11-nor-9-carboxy-9-tetrahydrocannabinol (THC-COOH), and four additional cannabinoids (cannabidiol (CBD), cannabigerol (CBG), tetrahydrocannabivarin (THCV), and cannabinol (CBN)) in 1mL of human urine and plasma was developed and validated. The hydrolysis process was studied to ensure complete hydrolysis of glucuronide conjugates and the extraction of a total amount of analytes. Initially, urine and plasma blank samples were spiked with THC-COOH-glucuronide and THC-glucuronide, and four different pretreatment methods were compared: hydrolysis-free method, enzymatic hydrolysis with Escherichia Coli -glucuronidase, alkaline hydrolysis with 10M NaOH, and enzyme-alkaline tandem hydrolysis. The last approach assured the maximum efficiencies (close to 100%) for both urine and plasma matrices. Regarding the figures of merit, the limits of detection were below 1ng/mL for all analytes, the accuracy ranged from 84% to 115%, and both within-day and between-day precision were lower than 12%. Finally, the method was successfully applied to real urine and plasma samples from cannabis users. Copyright (c) 2016 John Wiley & Sons, Ltd.
引用
收藏
页码:626 / 633
页数:8
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