Journal
ANALYTICA CHIMICA ACTA
Volume 770, Issue -, Pages 75-84Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2013.02.001
Keywords
Illicit drugs; Amphetamines; Ecstasy; 3,4-Methylenedioxymethamphetamine; Derivatization; Solid-phase microextraction
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Funding
- Spanish Ministry of Economy and Competitiveness (Ministerio de Economia y Competitividad)
- FEDER [CTQ2009-08377, CTQ2010-18927]
- Ramon y Cajal research program
- FPI grant
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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 CLODS) 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 100 mL of sample containing 2 g of dipotassium monohydrogen phosphate trihydrate and 100 mu l of iBCF (1:1 in acetonitrile), for 40 min at 60 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 mu g L-1. (C) 2013 Elsevier B.V. All rights reserved.
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