PMID- 16099938
OWN - NLM
STAT- MEDLINE
DCOM- 20060111
LR  - 20191210
IS  - 0009-9147 (Print)
IS  - 0009-9147 (Linking)
VI  - 51
IP  - 10
DP  - 2005 Oct
TI  - Drug testing in blood: validated negative-ion chemical ionization gas 
      chromatographic-mass spectrometric assay for enantioselective measurement of the 
      designer drugs MDEA, MDMA, and MDA and its application to samples from a 
      controlled study with MDMA.
PG  - 1811-22
AB  - BACKGROUND: The enantiomers of the designer drugs 3,4-methylenedioxyamphetamine 
      (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and 
      3,4-methylenedioxyethylamphetamine (MDEA) differ in their pharmacologic and 
      toxicologic potency. The aim of this study was to develop an assay for measuring 
      these enantiomers in small plasma volumes and to analyze samples from a 
      controlled study with MDMA. METHODS: The analytes were extracted from < or = 0.2 
      mL of plasma by mixed-mode solid-phase extraction. After derivatization with 
      S-(-)-heptafluorobutyrylprolyl chloride, the resulting diastereomers were 
      separated by gas chromatography (HP-5MS) within 17 min and detected by mass 
      spectrometry in the negative-ion chemical ionization mode. The method was fully 
      validated and applied to samples from a controlled study in which a single dose 
      of racemic MDMA (75 mg) was administered. RESULTS: The derivatized enantiomers 
      were well separated and detected with good sensitivity. The assay was linear (per 
      enantiomer) at 1-50 microg/L for MDA and 5-250 microg/L for MDMA and MDEA. 
      Analytical recovery, accuracy, repeatability, and intermediate precision data 
      were within required limits. Extraction yields were 82.1%-95.3%. In the study 
      samples, concentrations of R-(-)-MDMA significantly exceeded those of S-(+)-MDMA. 
      Their ratios (R vs S) were always >1.0 and increased over time. Concentrations of 
      S-(+)-MDA exceeded those of R-(-)-MDA, their ratios (R vs S) also increasing over 
      time but remaining <1.0. CONCLUSIONS: This assay enables sensitive, reliable, and 
      fast enantioselective measurement of MDA, MDMA, and MDEA in small volumes of 
      plasma. The controlled study data confirm previous findings of MDMA and MDA 
      enantiomer ratios (R vs S) increasing over time after ingestion of racemic MDMA.
FAU - Peters, Frank T
AU  - Peters FT
AD  - Department of Experimental and Clinical Toxicology, Institute of Experimental and 
      Clinical Pharmacology and Toxicology, University of Saarland, Homburg, Germany.
FAU - Samyn, Nele
AU  - Samyn N
FAU - Lamers, Caroline T J
AU  - Lamers CT
FAU - Riedel, Wim J
AU  - Riedel WJ
FAU - Kraemer, Thomas
AU  - Kraemer T
FAU - de Boeck, Gert
AU  - de Boeck G
FAU - Maurer, Hans H
AU  - Maurer HH
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
PT  - Validation Study
DEP - 20050811
PL  - England
TA  - Clin Chem
JT  - Clinical chemistry
JID - 9421549
RN  - 4764-17-4 (3,4-Methylenedioxyamphetamine)
RN  - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine)
RN  - ML1I4KK67B (3,4-methylenedioxyethamphetamine)
SB  - IM
MH  - 3,4-Methylenedioxyamphetamine/*analogs & derivatives/*blood
MH  - Dose-Response Relationship, Drug
MH  - Gas Chromatography-Mass Spectrometry/*methods
MH  - Humans
MH  - N-Methyl-3,4-methylenedioxyamphetamine/*blood
MH  - Sensitivity and Specificity
MH  - Stereoisomerism
MH  - Substance Abuse Detection/methods
MH  - Time Factors
EDAT- 2005/08/16 09:00
MHDA- 2006/01/13 09:00
CRDT- 2005/08/16 09:00
PHST- 2005/08/16 09:00 [pubmed]
PHST- 2006/01/13 09:00 [medline]
PHST- 2005/08/16 09:00 [entrez]
AID - clinchem.2005.052746 [pii]
AID - 10.1373/clinchem.2005.052746 [doi]
PST - ppublish
SO  - Clin Chem. 2005 Oct;51(10):1811-22. doi: 10.1373/clinchem.2005.052746. Epub 2005 
      Aug 11.