PMID- 23498689
OWN - NLM
STAT- MEDLINE
DCOM- 20130917
LR  - 20131121
IS  - 1873-4324 (Electronic)
IS  - 0003-2670 (Linking)
VI  - 770
DP  - 2013 Apr 3
TI  - In-sample derivatization-solid-phase microextraction of amphetamines and ecstasy 
      related stimulants from water and urine.
PG  - 75-84
LID - S0003-2670(13)00207-9 [pii]
LID - 10.1016/j.aca.2013.02.001 [doi]
AB  - A solid-phase microextraction (SPME) method for the determination of five 
      amphetamine type stimulants (ATSs) in water and urine samples is presented. 
      Analytes were simultaneously derivatized with iso-butyl chloroformate (iBCF) in 
      the aqueous sample while being extracted, improving in this way the 
      extractability of ATSs and permitting their determination by gas 
      chromatography-mass spectrometry (GC-MS). The SPME procedure was carefully 
      optimized in order to achieve adequate limits of detection (LODs) for 
      environmental concentrations. Hence, different operational parameters were 
      considered: type of SPME coating, ionic strength, basic catalyzer and 
      derivatizing agent amount, extraction time and temperature. The final SPME 
      procedure consists into the extraction of 100mL of sample containing 2 g of 
      dipotassium monohydrogen phosphate trihydrate and 100 muL of iBCF (1:1 in 
      acetonitrile), for 40 min at 60 degrees C with a polydimethylsiloxane-divinylbenzene 
      (PDMS-DVB) fiber. Under these conditions, LODs in wastewater ranged from 0.4 to 2 
      ng L(-1), relative recoveries in the 84-114% range and relative standard 
      deviations (RSD) lower than 15% were obtained. The application of the method to 
      wastewater and river water samples showed the ecstasy ATS, 
      3,4-methylenedioxymethamphetamine (MDMA), as the most frequently detected, 
      followed by methamphetamine, in concentrations around 20 ng L(-1). Finally, the 
      method was downscaled and also validated with urine samples, proving its good 
      performance with this matrix too: RSD<11%, recoveries in the 98-110% range and 
      LODs lower than 0.1 mug L(-1).
CI  - Copyright (c) 2013 Elsevier B.V. All rights reserved.
FAU - Racamonde, Ines
AU  - Racamonde I
AD  - Department of Analytical Chemistry, Nutrition and Food Sciences, IIAA-Institute 
      for Food Analysis and Research, University of Santiago de Compostela, Santiago de 
      Compostela, Spain.
FAU - Rodil, Rosario
AU  - Rodil R
FAU - Quintana, Jose Benito
AU  - Quintana JB
FAU - Cela, Rafael
AU  - Cela R
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20130212
PL  - Netherlands
TA  - Anal Chim Acta
JT  - Analytica chimica acta
JID - 0370534
RN  - 0 (Water Pollutants, Chemical)
RN  - CK833KGX7E (Amphetamine)
RN  - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine)
SB  - IM
MH  - Amphetamine/*analysis/*urine
MH  - Gas Chromatography-Mass Spectrometry
MH  - Humans
MH  - Limit of Detection
MH  - Molecular Structure
MH  - N-Methyl-3,4-methylenedioxyamphetamine/*analysis/*urine
MH  - Reference Standards
MH  - Rivers/*chemistry
MH  - *Solid Phase Microextraction
MH  - Water Pollutants, Chemical
EDAT- 2013/03/19 06:00
MHDA- 2013/09/18 06:00
CRDT- 2013/03/19 06:00
PHST- 2012/10/18 00:00 [received]
PHST- 2012/12/14 00:00 [revised]
PHST- 2013/02/01 00:00 [accepted]
PHST- 2013/03/19 06:00 [entrez]
PHST- 2013/03/19 06:00 [pubmed]
PHST- 2013/09/18 06:00 [medline]
AID - S0003-2670(13)00207-9 [pii]
AID - 10.1016/j.aca.2013.02.001 [doi]
PST - ppublish
SO  - Anal Chim Acta. 2013 Apr 3;770:75-84. doi: 10.1016/j.aca.2013.02.001. Epub 2013 
      Feb 12.