PMID- 10080646
OWN - NLM
STAT- MEDLINE
DCOM- 19990503
LR  - 20190831
IS  - 1387-2273 (Print)
IS  - 1387-2273 (Linking)
VI  - 723
IP  - 1-2
DP  - 1999 Feb 19
TI  - High sensitivity simultaneous determination in hair of the major constituents of 
      ecstasy (3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine and 
      3,4-methylene-dioxyethylamphetamine) by high-performance liquid chromatography 
      with direct fluorescence detection.
PG  - 195-202
AB  - A simple, but sensitive and specific high-performance liquid chromatographic 
      assay for the simultaneous determination of the major constituents of "ecstasy" 
      [i.e. 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine 
      (MDA), 3,4-methylenedioxyethylamphetamine (MDE)] with direct fluorimetric 
      detection, particularly intended for the routine analysis of hair, is described. 
      Hair samples (100 mg) were overnight incubated in 1 ml of 0.25 M HCl at 45 
      degrees C and extracted with a commercial liquid-liquid method. The dried residue 
      reconstituted with 500 microl of 0.05 M NaH2PO4 pH 5.2 was injected. Isocratic 
      reversed-phase liquid chromatography was carried out on a column (250x4.6 mm 
      I.D.) packed with spherical 5-microm poly(styrene-divinylbenzene) particles; the 
      mobile phase was composed of 0.1 M potassium phosphate (pH 3)-acetonitrile 
      (82:18). The excitation and the emission wavelengths were set to 285 and 320 nm, 
      respectively. Under the described conditions, MDA, MDMA and MDE eluted in 
      symmetric peaks with an analysis time of 30 min. The limit of detection was lower 
      than 1 ng/ml, with a signal-to-noise ratio of 5, for each compound in solution, 
      allowing a cut-off of 0.1 ng/mg in the hair matrix to be established. The 
      intra-day precision (n = 6) of the assay was characterised by RSDs between 1.0 
      and 3.0% and between 0.52 and 0.88% for concentrations of 10 and 100 ng/ml, 
      respectively; in day-to-day precision tests (n = 6), RSDs ranged between 5.12 and 
      11.12%, respectively, for the same concentrations. Interferences from as many as 
      92 therapeutic and/or abused drugs currently in use in the population were 
      excluded, including N-methyl-1-(3,4-methylenedioxyphenyl)-2 butanamine (MBDB).
FAU - Tagliaro, F
AU  - Tagliaro F
AD  - Institute of Forensic Medicine, Catholic University of the Sacred Heart, Rome, 
      Italy. ftmedl@borgoroma.univr.it
FAU - De Battisti, Z
AU  - De Battisti Z
FAU - Groppi, A
AU  - Groppi A
FAU - Nakahara, Y
AU  - Nakahara Y
FAU - Scarcella, D
AU  - Scarcella D
FAU - Valentini, R
AU  - Valentini R
FAU - Marigo, M
AU  - Marigo M
LA  - eng
PT  - Journal Article
PL  - Netherlands
TA  - J Chromatogr B Biomed Sci Appl
JT  - Journal of chromatography. B, Biomedical sciences and applications
JID - 9714109
RN  - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine)
SB  - IM
MH  - Chromatography, High Pressure Liquid/*methods
MH  - Hair/*chemistry
MH  - Humans
MH  - N-Methyl-3,4-methylenedioxyamphetamine/analogs & derivatives/*analysis
MH  - Reproducibility of Results
MH  - Sensitivity and Specificity
MH  - Spectrometry, Fluorescence
EDAT- 1999/03/18 00:00
MHDA- 1999/03/18 00:01
CRDT- 1999/03/18 00:00
PHST- 1999/03/18 00:00 [pubmed]
PHST- 1999/03/18 00:01 [medline]
PHST- 1999/03/18 00:00 [entrez]
AID - 10.1016/s0378-4347(98)00508-8 [doi]
PST - ppublish
SO  - J Chromatogr B Biomed Sci Appl. 1999 Feb 19;723(1-2):195-202. doi: 
      10.1016/s0378-4347(98)00508-8.