Automated determination of ethyl carbamate in stone-fruit spirits using headspace solid-phase microextraction and gas chromatography–tandem mass spectrometry
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CONTRIBUTORS:
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JOURNAL:
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Journal of Chromatography A,
1108(1),
116 -
120.
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YEAR:
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2006
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PUB TYPE:
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Journal Article
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SUBJECT(S):
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Solid-phase microextraction (SPME); Gas chromatography (GC); Tandem mass spectrometry (MS/MS); Ethyl carbamate (urethane); Stone-fruit spirits
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DISCIPLINE:
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Chemistry
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HTTP:
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http://dx.doi.org/10.1016/j.chroma.2005.12.086
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LANGUAGE:
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English
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PUB ID:
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103-424-186
(Last edited on
2006/02/13 00:41:35 US/Mountain)
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SPONSOR(S):
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ABSTRACT:
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 (EC) in stone-fruit spirits. After addition of deuterated internal standard, the optimised HS-SPME extraction with carbowax/divinylbenzene fibres (30 min at 70 °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-d5 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.
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