title: Rapid and simple determination of psychotropic phenylalkylamine derivatives in human hair by gas chromatography-mass spectrometry using micro-pulverized extraction.
abstract: A gas chromatography-mass spectrometric (GC-MS) method was developed and validated for the determination of five psychotropic phenylalkylamine derivatives (amphetamine, AP; methamphetamine, MA; 3,4-methylenedioxyamphetamine, MDA; 3,4-methylenedioxymethamphetamine, MDMA; norketamine, NKT) in human hair. Hair samples (10mg) were washed with distilled water and acetone, mechanically pulverized for 1.5 min with a bead mill, and then incubated in 1 mL of methanol under ultrasonication at 50 degrees C for 1h. The resulting solutions were evaporated to dryness, derivatized using heptafluorobutyric anhydride (HFBA) at 50 degrees C for 30 min, and analyzed by GC-MS. The linear ranges were 0.1-20.0 ng/mg for AP and MA and 0.05-20.0 ng/mg for MDA, MDMA, and NKT, with the coefficients of determination (r(2)>0.9982). The intra-day and inter-day precisions were within 11.5% and 12.8%, respectively. The intra-day and inter-day accuracies were -4.1% to 5.8% and -6.6% to 4.2%, respectively. The limits of detections (LODs) for each compound were lower than 0.028 ng/mg. The recoveries were in the range of 78.9-101.2%. Based on these results, the method proved to be effective for the rapid and simple determination of phenylalkylamine derivatives in hair specimens.
authors.affiliation: Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office, Seoul, Republic of Korea. paxus@spo.go.kr
authors.forename: Jin Young
authors.initials: JY
authors.lastname: Kim
authors.forename: Soon Ho
authors.initials: SH
authors.lastname: Shin
authors.forename: Jae Il
authors.initials: JI
authors.lastname: Lee
authors.forename: Moon Kyo
authors.initials: MK
authors.lastname: In
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000032:analysis; D000661:Amphetamine / Q000032:analysis; D053593:Forensic Toxicology; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006197:Hair / Q000737:chemistry*; D006213:Hallucinogens / Q000032:analysis*; D006801:Humans; D007649:Ketamine / Q000031:analogs & derivatives / Q000032:analysis; D057230:Limit of Detection; D008694:Methamphetamine / Q000032:analysis; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000032:analysis; D015813:Substance Abuse Detection / Q000379:methods*
chemical_list: D006213:Hallucinogens; D008694:Methamphetamine; D015104:3,4-Methylenedioxyamphetamine; D007649:Ketamine; D000661:Amphetamine; D018817:N-Methyl-3,4-methylenedioxyamphetamine; C033419:norketamine