title: Improved gas chromatography-negative ion chemical ionization tandem mass spectrometric method for determination of 11-nor-Δ9-tetrahydrocannabinol-9-carboxylic acid in hair using mechanical pulverization and bead-assisted liquid-liquid extraction.
abstract: A gas chromatography-negative ion chemical ionization tandem mass spectrometric (GC-NCI-MS/MS) method was developed and validated for the determination of 11-nor-Δ(9)-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in human hair. After decontamination, hair samples were weighed (25mg), mechanically pulverized with a bead mill, and incubated in 0.7 mL of 1.0M sodium hydroxide at 95 °C for 30 min. Bead-assisted liquid-liquid extraction was performed with n-hexane:ethyl acetate (9:1, v/v), a method developed in our laboratory. The extract was evaporated to dryness, derivatized with pentafluoropropanol and pentafluoropropionic anhydride, and analyzed by GC-MS/MS in the negative ion chemical ionization mode using methane as the reagent gas. The linear ranges were 0.05-10.0 pg/mg for THC-COOH with the coefficient of determination (r(2) = 0.9976). The intra-day and inter-day precisions were within 1.7 and 13.8%, respectively. The intra-day and inter-day accuracies were -4.8 to 10.0% and -3.9 to 3.8%, respectively. The limit of detection and quantification were 0.015 and 0.05 pg/mg, respectively. The recoveries were in the range of 79.4-87.1%. The results indicate that the proposed method is simple, rapid, accurate, and precise for determination of THC-COOH in hair. The method identified THC-COOH in hair specimens from suspected marijuana abusers.
authors.affiliation: Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office, 706 Banporo, Seocho-gu, Seoul 137-730, Republic of Korea.
authors.forename: Jin Young
authors.initials: JY
authors.lastname: Kim
authors.forename: Jae Chul
authors.initials: JC
authors.lastname: Cheong
authors.forename: Jae Il
authors.initials: JI
authors.lastname: Lee
authors.forename: Moon Kyo
authors.initials: MK
authors.lastname: In
mesh_terms: D002623:Chemistry Techniques, Analytical / Q000379:methods; D002849:Chromatography, Gas; D013759:Dronabinol / Q000031:analogs & derivatives* / Q000032:analysis; D053593:Forensic Toxicology; D006197:Hair / Q000737:chemistry*; D006801:Humans; D057230:Limit of Detection; D008297:Male; D011619:Psychotropic Drugs / Q000032:analysis*; D015813:Substance Abuse Detection / Q000379:methods; D053719:Tandem Mass Spectrometry
chemical_list: D011619:Psychotropic Drugs; C009411:delta(6)-tetrahydrocannabinol-7-oic acid; D013759:Dronabinol