Automated determination of ethyl carbamate in stone-fruit spirits using headspace solid-phase microextraction and gas chromatography–tandem mass spectrometry

Lachenmeier, Dirk W.; Nerlich, Uta; Kuballa, Thomas

doi:10.1016/j.chroma.2005.12.086

Cited by 91 publications

(78 citation statements)

References 23 publications

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“…The LOD and LOQ values, obtained for sweet/medium sweet model wines, were similar to those obtained by other authors employing HS-SPME/GC-MS-SIM (3 and 10 g/L) [19] to determine EC in beers, red wines, white wines, grape brandies and Chinese rice wines. On the other hand, considerable higher LOD and LOQ values (30 and 110 g/L) were obtained by Lachenmeier et al [9] using HS-SPME/GC-MS-MS in stone-fruit spirits. These high values may be explained to the fact that stone-fruit spirits contain considerably higher levels of EC (in the mg/L range) and also contain much higher levels of alcohol, which interfere with SPME extraction, so that the samples have to be diluted.…”

Section: Quantification Approach For Assessment Of Ethyl Carbamatementioning

confidence: 99%

“…As previous tests indicated the potential of this methodology to detected EC, this methodology was adopted to EC determinations. According to Lachenmeier et al [9], CW/DVB fibre present high extraction efficiency for EC, as nowadays this fibre is not commercially available, a SPME fibre presenting a wide range of applications, including the EC, was selected. The SPME holder for manual sampling and fibre were purchased from Supelco (Aldrich, Bellefonte, PA, USA).…”

Section: Hs-spme Methodologymentioning

confidence: 99%

“…Apprehension related to EC occurrence in alcoholic beverages arose in 1985, when relatively high levels were detected by Canadian authorities in brandies and others liquors [9,10]. Consequently, maximum level of EC was firstly established by Canada authorities for alcoholic beverages, according to the consumption patterns and ADI (acceptable daily intake) value evaluation: 30 g/L for table wine, 100 g/L for fortified wines, 150 g/L for distilled spirits, and 400 g/L for fruit brandies and liquors [11,12].…”

Section: Introductionmentioning

confidence: 99%

“…EC has been determined in fortified Madeira wines by SPE followed by GC-MS [15,16], and by derivatization with 9-xanthydrol, followed by high performance liquid chromatography (HPLC) [17]. More recently, a solvent-free methodology was used: solid phase microextraction (SPME) [9,18,19]. This methodology presents several advantages when compared with conventional solvent extraction procedures.…”

Section: Introductionmentioning

confidence: 99%

“…The extraction step is followed mainly by GC-MS analysis [7,13,15,16]. To achieve the adequate sensitivity for EC detection, an injector equipped with a unit for large volume injection [7], or MS-SIM (selected ion monitoring) [13,19] or MS-MS acquisition modes (GC-MS-MS) [9,14,21] were used. Onedimensional chromatographic processes are widely applied in the analysis of food products.…”

Section: Introductionmentioning

confidence: 99%

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Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine

Perestrelo

Petronilho

Câmara

et al. 2010

Journal of Chromatography A

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a b s t r a c tAn analytical methodology based on headspace solid phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC × GC-ToFMS) was developed for the identification and quantification of the toxic contaminant ethyl carbamate (EC) directly in fortified wines. The method performance was assessed for dry/medium dry and sweet/medium sweet model wines, and for quantification purposes, calibration plots were performed for both matrices using the ion extraction chromatography (IEC) mode (m/z 62). Good linearity was obtained with a regression coefficient (r 2 ) higher than 0.981. A good precision was attained (R.S.D. <20%) and low detection limits (LOD) were achieved for dry (4.31 g/L) and sweet (2.75 g/L) model wines. The quantification limits (LOQ) and recovery for dry wines were 14.38 g/L and 88.6%, whereas for sweet wines were 9.16 g/L and 99.4%, respectively. The higher performance was attainted with sweet model wine, as increasing of glucose content improves the volatile compound in headspace, and a better linearity, recovery and precision were achieved. The analytical methodology was applied to analyse 20 fortified Madeira wines including different types of wine (dry, medium dry, sweet, and medium sweet) obtained from several harvests in Madeira Island (Portugal). The EC levels ranged from 54.1 g/L (medium dry) to 162.5 g/L (medium sweet).

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Section: Quantification Approach For Assessment Of Ethyl Carbamatementioning

confidence: 99%

Section: Hs-spme Methodologymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine

Perestrelo

Petronilho

Câmara

et al. 2010

Journal of Chromatography A

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Ethyl Carbamate (Urethane)

Hamlet

2008

Process‐Induced Food Toxicants

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High‐sensitive Electrochemical Determination of Ethyl Carbamate Using Urethanase and Glutamate Dehydrogenase Modified Electrode

Zhang

Tian

et al. 2016

Electroanalysis

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An amperometric biosensor for ethyl carbamate (EC) was developed for the first time through the cascade reactions of urethanase and glutamate dehydrogenase (GLDH). Urethanase decomposes ethyl carbamate to produce ammonia, which converts to L‐glutamate under the catalysis of GLDH in the presence of α‐ketoglutarate and NADH. Then the change of NADH can be detected chronoamperometrically. The two enzymes were entrapped into chitosan/gelatine/γ‐glycidoxy propyl trimethoxy silane sol‐gel and immobilized on the surface of pyrolytic graphite electrode (PGE). The modified electrode was characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Under the optimized conditions, the amperometric EC biosensor exhibits a linear detection range from 0.5 to 40 μM with a low detection limit of 5.30 nM. The biosensor was successfully used to detect EC in mimic Chinese rice wine samples, and satisfactory recovery and relative standard deviation were achieved.

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Automated determination of ethyl carbamate in stone-fruit spirits using headspace solid-phase microextraction and gas chromatography–tandem mass spectrometry

Cited by 91 publications

References 23 publications

Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine

Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine

Ethyl Carbamate (Urethane)

High‐sensitive Electrochemical Determination of Ethyl Carbamate Using Urethanase and Glutamate Dehydrogenase Modified Electrode

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