PMID- 10654563
OWN - NLM
STAT- MEDLINE
DCOM- 20000309
LR  - 20190513
IS  - 0146-4760 (Print)
IS  - 0146-4760 (Linking)
VI  - 24
IP  - 1
DP  - 2000 Jan-Feb
TI  - Rapid analysis of amphetamine, methamphetamine, MDA, and MDMA in urine using 
      solid-phase microextraction, direct on-fiber derivatization, and analysis by 
      GC-MS.
PG  - 11-6
AB  - A rapid, sensitive, and solvent-free procedure for the simultaneous determination 
      of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine (MDA), and 
      3,4-methylenedioxymethamphetamine (MDMA) in urine was developed using solid-phase 
      microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) in the 
      selected ion monitoring mode. A headspace vial containing the urine sample, NaOH, 
      NaCl, and amphetamine-d3 as the internal standard was heated at 100 degrees C for 
      20 min. A polydimethylsiloxane fiber was maintained in the vial headspace for 10 
      min in order to adsorb the amphetaminic compounds, which were subsequently 
      derivatized by exposing the fiber to trifluoroacetic anhydride for 20 min in the 
      headspace of another vial maintained at 60 degrees C for 20 min. The 
      trifluoroacetyl derivatives were desorbed in the GC injection port for 5 min. 
      Several parameters were considered during the method optimization process. These 
      included a comparison of SPME with or without headspace, the required 
      derivatization procedure, and the influence of temperature on the headspace 
      extraction and derivatization methods. The optimized method was validated for the 
      four compounds tested. Calibration curves showed linearity in the range 50-1000 
      ng/mL (r = 0.9946-0.9999). Recovery data were 71.89-103.24%. The quantitation 
      limits were 10 ng/mL for amphetamine and methamphetamine and 20 ng/mL for MDA and 
      MDMA. All of these data recommend the applicability of the method for use in the 
      analytical routine of a forensic laboratory.
FAU - Jurado, C
AU  - Jurado C
AD  - Instituto Nacional de Toxicologia, Sevilla, Spain. quim@sev.inaltox.es
FAU - Gimenez, M P
AU  - Gimenez MP
FAU - Soriano, T
AU  - Soriano T
FAU - Menendez, M
AU  - Menendez M
FAU - Repetto, M
AU  - Repetto M
LA  - eng
PT  - Comparative Study
PT  - Journal Article
PL  - England
TA  - J Anal Toxicol
JT  - Journal of analytical toxicology
JID - 7705085
RN  - 0 (Dimethylpolysiloxanes)
RN  - 0 (Sympathomimetics)
RN  - 44RAL3456C (Methamphetamine)
RN  - 4764-17-4 (3,4-Methylenedioxyamphetamine)
RN  - CK833KGX7E (Amphetamine)
RN  - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine)
SB  - IM
MH  - 3,4-Methylenedioxyamphetamine/*urine
MH  - Amphetamine/*urine
MH  - Dimethylpolysiloxanes/*chemistry
MH  - Gas Chromatography-Mass Spectrometry
MH  - Humans
MH  - Methamphetamine/*urine
MH  - Microchemistry
MH  - N-Methyl-3,4-methylenedioxyamphetamine/*urine
MH  - Reproducibility of Results
MH  - Sensitivity and Specificity
MH  - Substance Abuse Detection/*methods
MH  - Sympathomimetics/*urine
MH  - Temperature
MH  - Time Factors
EDAT- 2000/02/02 09:00
MHDA- 2000/03/11 09:00
CRDT- 2000/02/02 09:00
PHST- 2000/02/02 09:00 [pubmed]
PHST- 2000/03/11 09:00 [medline]
PHST- 2000/02/02 09:00 [entrez]
AID - 10.1093/jat/24.1.11 [doi]
PST - ppublish
SO  - J Anal Toxicol. 2000 Jan-Feb;24(1):11-6. doi: 10.1093/jat/24.1.11.