title: Detection of methamphetamine, methylenedioxymethamphetamine, and 3,4-methylenedioxy-N-ethylamphetamine in spiked plasma by HPLC and TLC.
abstract: HPLC and TLC methods were developed for separation and detection of some amphetamine analogs: methamphetamine (MA); 3,4-methylenedioxymethamphetamine (MDMA, "ecstasy"); and 3,4-methylenedioxy-N-ethylamphetamine (MDEA) in spiked plasma samples. The methods are based on purple chromogens formed by displacement reaction of these secondary aliphatic amine-bearing drugs with 7,7,8,8-tetracyanoquinodimethane at 80 degrees C for 25 min. For HPLC, both normal phase (silica gel) and RP (C18) columns were used. With the former, good detection limits in plasma were obtained with a 6 min run: 70, 100, and 500 ng/mL for MDMA, MA, and MDEA, respectively. For TLC, hexane-chloroform (1 + 9) and benzene-diethyl ether-petroleum ether (40-60 degrees)-acetonitrile-ethyl methyl ketone (2 + 3.5 + 3.5 + 0.5 + 0.5) were used as mobile phases for silica gel 60 TLC and cyano-bonded silica gel HPTLC plates, respectively. The former offered more sensitive results than the latter. Influence of evaporation steps on recovery and interferences for the HPLC and TLC methods were investigated. The developed methods are selective, simple, and easily applicable.
authors.affiliation: Istanbul University, Faculty of Pharmacy, Department of Analytical Chemistry, Istanbul, Turkey. aoztunc@istanbul.edu.tr
authors.forename: Aysel
authors.initials: A
authors.lastname: Oztunç
authors.forename: Armağan
authors.initials: A
authors.lastname: Onal
authors.forename: Sidika Ertürk
authors.initials: SE
authors.lastname: Toker
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000031:analogs & derivatives* / Q000032:analysis; D000097:Acetonitriles / Q000737:chemistry; D000473:Alkanes / Q000737:chemistry; D001554:Benzene / Q000737:chemistry; D002021:Buffers; D002074:Butanones / Q000737:chemistry; D002623:Chemistry Techniques, Analytical; D002725:Chloroform / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D002855:Chromatography, Thin Layer / Q000379:methods*; D004986:Ether / Q000737:chemistry; D006586:Hexanes / Q000737:chemistry; D008694:Methamphetamine / Q000032:analysis*; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000032:analysis*; D015203:Reproducibility of Results; D013696:Temperature
chemical_list: D000097:Acetonitriles; D000473:Alkanes; D002021:Buffers; D002074:Butanones; D006586:Hexanes; D004986:Ether; D008694:Methamphetamine; D015104:3,4-Methylenedioxyamphetamine; C005222:methylethyl ketone; D002725:Chloroform; D001554:Benzene; D018817:N-Methyl-3,4-methylenedioxyamphetamine; C051800:3,4-methylenedioxyethamphetamine; C004544:naphtha; C032159:acetonitrile