title: A sensitive semi-micro column HPLC method with peroxyoxalate chemiluminescence detection and column switching for determination of MDMA-related compounds in hair.
abstract: A sensitive semi-micro column HPLC method with peroxyoxalate chemiluminescence (POCL) detection and column switching has been developed for simultaneous determination of 3,4-methylenedioxymethamphetamine (MDMA) and related compounds, for example 3,4-methylenedioxyamphetamine, methamphetamine, and amphetamine, in hair. After digestion of the hair with 1 mol L-1 sodium hydroxide the compounds were extracted with n-heptane and derivatized with 4-(N,N-dimethylaminosulfonyl)-7-fluoro-2,1,3-benzoxadiazole. A mixture of hydrogen peroxide and bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate in acetonitrile was used as post-column CL reagent. Calibration plots showed linearity was good (r=0.999); detection limits were 0.02-0.16 ng mg-1 hair at a signal-to-noise ratio of 3. The precision of the method, as RSD (n=5), in intra-day and inter-day assays was better than 5.0 and 6.9%, respectively. The proposed method was sufficiently sensitive to detect low ng mg-1 levels of MDMA and related compounds in hair, and could be used for quantification of the compounds in hair samples from patients treated in a chemical dependency unit.
authors.affiliation: Department of Clinical Pharmacy, Graduate School of Biomedical Sciences, Nagasaki University, 1-14 Bunkyo-machi, Nagasaki, 852-8521, Japan, and Mississippi State Hospital, Whitfield 39193, USA.
authors.forename: Shinichi
authors.initials: S
authors.lastname: Nakamura
authors.forename: Mitsuhiro
authors.initials: M
authors.lastname: Wada
authors.forename: Brian L
authors.initials: BL
authors.lastname: Crabtree
authors.forename: Patricia M
authors.initials: PM
authors.lastname: Reeves
authors.forename: John H
authors.initials: JH
authors.lastname: Montgomery
authors.forename: H Joseph
authors.initials: HJ
authors.lastname: Byrd
authors.forename: Shiro
authors.initials: S
authors.lastname: Harada
authors.forename: Naotaka
authors.initials: N
authors.lastname: Kuroda
authors.forename: Kenichiro
authors.initials: K
authors.lastname: Nakashima
mesh_terms: D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation* / Q000379:methods*; D006197:Hair / Q000737:chemistry; D006801:Humans; D008163:Luminescent Measurements / Q000295:instrumentation* / Q000379:methods*; D015394:Molecular Structure; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000032:analysis* / Q000737:chemistry; D010070:Oxalates / Q000032:analysis* / Q000737:chemistry; D012680:Sensitivity and Specificity
chemical_list: D010070:Oxalates; C044622:peroxyoxalate; D018817:N-Methyl-3,4-methylenedioxyamphetamine