PMID- 17158009
OWN - NLM
STAT- MEDLINE
DCOM- 20071005
LR  - 20191210
IS  - 1872-6283 (Electronic)
IS  - 0379-0738 (Linking)
VI  - 171
IP  - 2-3
DP  - 2007 Sep 13
TI  - A validated SPME-GC-MS method for simultaneous quantification of club drugs in 
      human urine.
PG  - 142-50
AB  - A solid-phase microextraction-gas chromatographic-mass spectrometric (SPME-GC-MS) 
      method has been developed and validated for measuring four club drugs in human 
      urine. These drugs include gamma-hydroxybutyrate (GHB), ketamine (KET), 
      methamphetamine (MAMP), and methylenedioxymethamphetamine (MDMA). These drugs are 
      referred to as 'club drugs' because of their prevalence at parties and raves. 
      Deuterium labeled internal standards for each of the four drugs was included in 
      the assay to aid in quantitation. The drugs were spiked into human urine and 
      derivatized using pyridine and hexylchloroformate to make them suitable for GC-MS 
      analysis. The SPME conditions of extraction time/temperature and desorption 
      time/temperature were optimized to yield the highest peak area for each of the 
      four drugs. The final SPME parameters included a 90 degrees C extraction for 
      20min with a 1min desorption in the GC injector at 225 degrees C using a 
      splitless injection. All SPME work was done using a 100microm PDMS fiber by 
      Supelco. The ratio of pyridine to hexylchloroformate for derivatization was also 
      optimized. The GC separation was carried out on a VF-5ht column by Varian (30m, 
      0.25mm i.d., 0.10microm film thickness) using a temperature program of 150-270 
      degrees C at 10 degrees C/min. The instrument used was a ThermoFinnigan Trace 
      GC-Polaris Q interfaced with a LEAP CombiPal autosampler. The data was collected 
      by using extracted ion chromatograms of marker m/z values for each drug from the 
      total ion chromatograms (TIC) (full scan mode). Calibration curves with R(2)>0.99 
      were generated each day using the peak area ratios (peak area drug/peak area 
      internal standard) versus concentration. The validated method resulted in 
      intra-day and inter-day precision (% R.S.D.) of less than 15% and a % error of 
      less than 15% for four concentrations in the range of 0.05-20microg/mL (MAMP) and 
      0.10-20microg/mL (GHB, KET, and MDMA). This method has the advantage of an easy 
      sample preparation with acceptable accuracy and precision for the simultaneous 
      quantification of these four drugs of abuse and shows no interference from the 
      urine matrix.
FAU - Brown, Stacy D
AU  - Brown SD
AD  - The Citadel, Chemistry Department, 171 Moultrie Street, Charleston, SC 
      29409-6220, United States. stacy.brown@citadel.edu
FAU - Rhodes, Daniel J
AU  - Rhodes DJ
FAU - Pritchard, Boyd J
AU  - Pritchard BJ
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
PT  - Validation Study
DEP - 20061208
PL  - Ireland
TA  - Forensic Sci Int
JT  - Forensic science international
JID - 7902034
RN  - 0 (Central Nervous System Agents)
RN  - 0 (Formates)
RN  - 0 (Illicit Drugs)
RN  - 0 (Indicators and Reagents)
RN  - 0 (Pyridines)
RN  - 0 (hexylchloroformate)
RN  - 44RAL3456C (Methamphetamine)
RN  - 690G0D6V8H (Ketamine)
RN  - 7G33012534 (Sodium Oxybate)
RN  - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine)
RN  - NH9L3PP67S (pyridine)
SB  - IM
MH  - Central Nervous System Agents/chemistry/urine
MH  - *Forensic Toxicology
MH  - Formates/chemistry/urine
MH  - *Gas Chromatography-Mass Spectrometry
MH  - Humans
MH  - Illicit Drugs/*urine
MH  - Indicators and Reagents
MH  - Ketamine/chemistry/urine
MH  - Methamphetamine/chemistry/urine
MH  - Molecular Structure
MH  - N-Methyl-3,4-methylenedioxyamphetamine/chemistry/urine
MH  - Pyridines
MH  - Sodium Oxybate/chemistry/urine
MH  - *Solid Phase Microextraction
MH  - Substance Abuse Detection/*methods
EDAT- 2006/12/13 09:00
MHDA- 2007/10/06 09:00
CRDT- 2006/12/13 09:00
PHST- 2006/06/29 00:00 [received]
PHST- 2006/10/20 00:00 [revised]
PHST- 2006/10/27 00:00 [accepted]
PHST- 2006/12/13 09:00 [pubmed]
PHST- 2007/10/06 09:00 [medline]
PHST- 2006/12/13 09:00 [entrez]
AID - S0379-0738(06)00669-4 [pii]
AID - 10.1016/j.forsciint.2006.10.015 [doi]
PST - ppublish
SO  - Forensic Sci Int. 2007 Sep 13;171(2-3):142-50. doi: 
      10.1016/j.forsciint.2006.10.015. Epub 2006 Dec 8.