Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1108, Issue 1, Pages 116-120Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2005.12.086
Keywords
solid-phase microextraction (SPME); gas chromatography (GC); tandem mass spectrometry (MS/MS); ethyl carbamate (urethane); stone-fruit spirits
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A fully automated procedure using headspace solid-phase microextraction (HS-SPME) followed by gas chromatographic/tandem mass spectrometric (GC/MS/MS) detection was developed for the determination of the toxic contaminant ethyl carbamate (C) in stone-fruit spirits. After addition of deuterated internal standard, the optimised HS-SPME extraction with carbowax/divinylbenzene fibres (30 min at 70 degrees C) was done applying salting out with sodium chloride in the presence of pH 7 buffer solution. For quantitative analysis the characteristic fragmentations of m/z 74 > 44 and m/z 62 > 44 for ethyl carbamate as well as m/z 64 > 44 for ethyl carbamate-d(5) were monitored in the multiple reaction monitoring (MRM) mode using a triple quadrupole instrument. In the validation studies, ethyl carbamate exhibited good linearity with a regression coefficient of 0.998. The limits of detection and quantitation were 0.03 and 0.11 mg/l. The precision never exceeded 4.3% (intraday) and 8.2% (interday) at any of the concentrations examined. A good agreement of analysis results in comparison to conventional sample clean-up over diatomaceous earth columns was found (R = 0.956, Bias 0.08 mg/l). The new HS-SPME/GC/MS/MS procedure is suitable for the fast. reliable and inexpensive determination of ethyl carbamate in alcoholic beverages in an automated, and therefore, convenient procedure. (c) 2006 Elsevier B.V. All rights reserved.
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