EMAIL THIS PAGE TO A FRIEND

Analytica chimica acta

In-sample derivatization-solid-phase microextraction of amphetamines and ecstasy related stimulants from water and urine.


PMID 23498689

Abstract

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 μL 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 μg L(-1).

Related Materials

Product #

Image

Description

Molecular Formula

Add to Cart

M6403
(±)-3,4-Methylenedioxymethamphetamine hydrochloride
C11H15NO2 · HCl
M5029
(±)-3,4-Methylenedioxymethamphetamine hydrochloride solution, analytical standard, for drug analysis, 1.0 mg/mL in methanol
C11H15NO2 · HCl
A-007
(±)-Amphetamine solution, 1.0 mg/mL in methanol, ampule of 1 mL, certified reference material
C9H13N
A-011
(±)-Amphetamine solution, 100 μg/mL in methanol, ampule of 1 mL, certified reference material
C9H13N
M-013
(±)-MDMA solution, 1.0 mg/mL in methanol, ampule of 1 mL, certified reference material
C11H15NO2
M139
S(+)-3,4-Methylenedioxymethamphetamine hydrochloride, solid
C11H15NO2 · HCl
57317 SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 60 μm (partially crosslinked phase), for use with autosampler/HPLC, needle size 24 ga, StableFlex fiber
57310-U SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (partially crosslinked phase), needle size 24 ga, for use with manual holder
57346-U SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (partially crosslinked phase), fused silica fiber, for use with manual holder, needle size 23 ga
57311 SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (partially crosslinked phase), needle size 24 ga, for use with autosampler
57345-U SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (partially crosslinked phase), for use with autosampler, needle size 23 ga
57326-U SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm, needle size 24 ga, StableFlex, for use with manual holder
57327-U SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm, needle size 24 ga, StableFlex, for use with autosampler
57293-U SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm, needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
57902-U SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (bonded phase), for use with autosampler, needle size 23 ga, metal alloy fiber
FFA57293-U SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm, needle size 23 ga, Stableflex, for use with multi fiber exchanger
FFA57327-U SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm, for use with multi fiber exchanger, needle size 24 ga, Stableflex
57359-U SPME Portable Field Sampler, coating Polydimethylsiloxane/Divinylbenzene (PDMS/DVB)