title: Target screening and confirmation of 35 licit and illicit drugs and metabolites in hair by LC-MSMS.
abstract: A liquid chromatography-tandem mass spectrometry (LC-MSMS) target screening in 50mg hair was developed and fully validated for 35 analytes (Δ9-tetrahidrocannabinol (THC), morphine, 6-acetylmorphine, codeine, methadone, fentanyl, amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, benzoylecgonine, cocaine, lysergic acid diethylamide, ketamine, scopolamine, alprazolam, bromazepam, clonazepam, diazepam, flunitrazepam, 7-aminoflunitrazepam, lorazepam, lormetazepam, nordiazepam, oxazepam, tetrazepam, triazolam, zolpidem, zopiclone, amitriptyline, citalopram, clomipramine, fluoxetine, paroxetine and venlafaxine). Hair decontamination was performed with dichloromethane, and incubation in 2 mL of acetonitrile at 50°C overnight. Extraction procedure was performed in 2 steps, first liquid-liquid extraction, hexane:ethyl acetate (55:45, v:v) at pH 9, followed by solid-phase extraction (Strata-X cartridges). Chromatographic separation was performed in AtlantisT3 (2.1 mm × 100 mm, 3 μm) column, acetonitrile and ammonium formate pH 3 as mobile phase, and 32 min total run time. One transition per analyte was monitored in MRM mode. To confirm a positive result, a second injection monitoring 2 transitions was performed. The method was specific (no endogenous interferences, n=9); LOD was 0.2-50 pg/mg and LOQ 0.5-100 pg/mg; linearity ranged from 0.5-100 to 2000-20,000 pg/mg; imprecision <15%; analytical recovery 85-115%; extraction efficiency 4.1-85.6%; and process efficiency 2.5-207.7%; 27 analytes showed ion suppression (up to -86.2%), 4 ion enhancement (up to 647.1%), and 4 no matrix effect; compounds showed good stability 24-48 h in autosampler. The method was applied to 17 forensic cases. In conclusion, a sensitive and specific target screening of 35 analytes in 50mg hair, including drugs of abuse (THC, cocaine, opiates, amphetamines) and medicines (benzodiazepines, antidepressants) was developed and validated, achieving lower cut-offs than Society of Hair Testing recommendations.
authors: Servicio de Toxicología Forense, Instituto de Ciencias Forenses, Universidad de Santiago de Compostela, Spain.
authors: Elena
authors: E
authors: Lendoiro
authors: Oscar
authors: O
authors: Quintela
authors: Ana
authors: A
authors: de Castro
authors: Angelines
authors: A
authors: Cruz
authors: Manuel
authors: M
authors: López-Rivadulla
authors: Marta
authors: M
authors: Concheiro
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods; D053593:Forensic Toxicology; D006197:Hair / Q000737:chemistry*; D006801:Humans; D013287:Illicit Drugs / Q000032:analysis*; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods; D009294:Narcotics / Q000032:analysis*; D004364:Pharmaceutical Preparations / Q000032:analysis*; D015813:Substance Abuse Detection; D019966:Substance-Related Disorders / Q000175:diagnosis
chemical_list: D013287:Illicit Drugs; D009294:Narcotics; D004364:Pharmaceutical Preparations