title: Determination of amphetamine-type stimulants, cocaine and ketamine in human hair by liquid chromatography/linear ion trap-Orbitrap hybrid mass spectrometry.
abstract: An LTQ Orbitrap XL hybrid mass spectrometry method was developed for the determination of illicit drugs and their metabolites, including amphetamine (AP), methamphetamine (MA), dimethylamphetamine (DMA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), ketamine (KET), norketamine (NK), cocaine (COC) and benzoylecgonine (BE), in hair. Micropulverized extraction was employed for sample preparation using a small hair sample (2 cm piece or 0.2 mg). Recoveries of the analytes during sample preparation were estimated using fortified hair samples and ranged from 35.5% for COC to 71.7% for AP. High resolution full-scan mass spectra and unit resolution product-ion spectra were obtained with the Orbitrap analyzer and the linear ion-trap analyzer, respectively. High-resolution extracted ion chromatograms at a tolerance of 3 ppm were utilized for quantification. The analytes were identified using the product-ion spectra in combination with the accurate masses of the corresponding protonated molecules observed in the high-resolution mass spectra. Lower limits of quantification obtained from a 0.2 mg hair sample were 0.050 ng mg(-1) (MDMA, KET and BE), 0.10 ng mg(-1) (AP, MA, DMA, NK and COC) and 0.50 ng mg(-1) (MDA). Two reference materials were analyzed for verification, and segmental analysis of single strands of hair specimens from actual cases was performed.
authors.affiliation: National Research Institute of Police Science, 6-3-1 Kashiwanoha, Kashiwa, Chiba 277-0882, Japan. miyaguchi@nrips.go.jp
authors.forename: Hajime
authors.initials: H
authors.lastname: Miyaguchi
authors.forename: Hiroyuki
authors.initials: H
authors.lastname: Inoue
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000032:analysis; D000662:Amphetamines / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods; D003042:Cocaine / Q000031:analogs & derivatives / Q000032:analysis*; D006197:Hair / Q000737:chemistry*; D006801:Humans; D013287:Illicit Drugs / Q000032:analysis*; D007649:Ketamine / Q000031:analogs & derivatives / Q000032:analysis*; D057230:Limit of Detection; D008694:Methamphetamine / Q000031:analogs & derivatives / Q000032:analysis; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000032:analysis; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D000662:Amphetamines; D013287:Illicit Drugs; D008694:Methamphetamine; D015104:3,4-Methylenedioxyamphetamine; C005618:benzoylecgonine; D007649:Ketamine; D003042:Cocaine; C003714:dimethylamphetamine; D018817:N-Methyl-3,4-methylenedioxyamphetamine; C033419:norketamine