Determination of Ethyl Carbamate in Sake Using Headspace Solid Phase Microextraction

Horii, Sachie; Goto, Kuniyasu

doi:10.1002/j.2050-0416.2010.tb00415.x

Cited by 18 publications

(17 citation statements)

References 17 publications

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“…That is, the concentration of ethanol had minimal effect on the analysis of EC. This is in agreement with the results for the PA fibre used in sake and the CW‐DVB fibre .…”

Section: Resultssupporting

confidence: 92%

“…The limit of quantitation (LOQ, signal‐to‐noise ratio 10) of EC was 3.96 µg L −1 , and the limit of detection (LOD, signal‐to‐noise ratio = 3) was 1.19 µg L −1 . The LOD corresponded very well to the limit obtained with the DVB/CAR/PDMS fibre (1.21 µg L −1 ) , and was lower than that obtained in sake also with the PA fibre (6.7 µg L −1 ) , which was related to the longer extraction time and good separation.…”

Section: Resultssupporting

confidence: 77%

“…Thus an extraction time of 45 min was selected to save time. Although the extraction time was longer than the 15 min used in sake , the 30 min used in wine or stone‐fruit spirits , a total analysis time of 57 min per sample was enough in continuous determination, which was substantially faster than the >2 h time period of the widely used SPE‐GC‐MS method. Sample throughput was twice as fast.…”

Section: Resultsmentioning

confidence: 99%

“…The divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fibre was once judged to be better for EC extraction in Chinese rice wine . In addition, recent research shows that the polyacrylate (PA) fibre gives good results with sake , a similar alcoholic beverage to Chinese rice wine. As a result, the DVB/CAR/PDMS or PA fibre could be the most suitable for EC extraction in Chinese rice wine.…”

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Rapid determination of ethyl carbamate in Chinese rice wine using headspace solid-phase microextraction and gas chromatography-mass spectrometry

Liu

Zhao

2012

J. Inst. Brew.

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Ethyl carbamate (EC) is a naturally occurring toxic contaminant that may imply a risk to human health and is usually found in alcoholic beverages such as Chinese rice wine. An automated procedure for the rapid determination of EC in Chinese rice wine was developed by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Using propyl carbamate as internal standard, the optimized HS-SPME sampling with a polyacrylic fibre was 45 min at 70 C after applying 38.8% NaCl to saturate the sample. This method showed good linearity over a range of 25-600 mg L À1(R 2 = 0.997). The recovery, relative standard deviation and limit of detection were 90.21-97.35%, lower than 2.89% and 1.19 mg L À1, respectively. Additionally, the ethanol concentration had no effect on the analysis of EC. The total analysis time of 57 min per sample in continuous determination was twice as fast as the widely used solid-phase extraction-GC-MS method. This solventfree HS-SPME-GC-MS procedure is suitable for the rapid, automated, and therefore convenient, determination of EC in Chinese rice wine.

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“…That is, the concentration of ethanol had minimal effect on the analysis of EC. This is in agreement with the results for the PA fibre used in sake and the CW‐DVB fibre .…”

Section: Resultssupporting

confidence: 92%

Section: Resultssupporting

confidence: 77%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Rapid determination of ethyl carbamate in Chinese rice wine using headspace solid-phase microextraction and gas chromatography-mass spectrometry

Liu

Zhao

2012

J. Inst. Brew.

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“…Approaches for sample preparation included Extrelut extraction [10,14,18], headspace solid-phase microextraction (HS-SPME) [6,19,20], and solid-phase extraction (SPE) [12,17]. An alternative way to decrease matrix effects is the use of derivatization of EC with xanthydrol for HPLC/MS analysis [21].…”

Section: Introductionmentioning

confidence: 99%

Rapid Quantification of Ethyl Carbamate in Spirits Using NMR Spectroscopy and Chemometrics

Monakhova

Kuballa

Lachenmeier

2012

ISRN Analytical Chemistry

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Ethyl carbamate (EC, urethane, C 2 H 5 OCONH 2 ) is a genotoxic carcinogen and is regularly found in fermented food products including alcoholic beverages. In this study, the rapid method of nuclear magnetic resonance (NMR) spectroscopy in combination with partial least squares (PLS) regression is applied for the first time to the analysis of ethyl carbamate in stone fruit spirits (n = 119) and unrecorded alcohols (n = 27) (analysis time only 15 min per sample). The PLS procedure was validated using an independent set of samples (n = 43, R 2 = 0.89, RMSE = 0.14 mg/L) in comparison to reference GC/MS/MS results. The NMR method was found to outperform other screening techniques based on NIR or FTIR regarding sensitivity and selectivity. The major advantage over GC/MS/MS, besides the reduced time of instrumental analysis, is that no sample preparation besides addition of buffer with internal standard is required, while for GC/MS/MS labour-intensive sample extraction is necessary prior to measurement.

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Multiple headspace solid‐phase microextraction using a new fiber for avoiding matrix interferences in the quantitative determination of ethyl carbamate in pickles

Lei

Zhang

Gao

et al. 2012

J of Separation Science

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Multiple headspace solid-phase microextraction (HS-SPME) using a novel fiber coated with anilino-methyl triethoxy silicane-methacrylic acid/terminated silicone oil has been introduced as a useful pretreatment technique coupled to gas chromatography-flame ionization detector for the detection of ethyl carbamate in pickles. Anilino-methyl triethoxy silicane and methacrylic acid are put into use simultaneously with the aim to increase the hydrogen interaction strength between ethyl carbamate and the coating. In addition, the new fiber exhibits high thermal stability, good reproducibility, and long lifetime. Extraction temperature, extraction time, amount of desiccant, and amount of sample were well optimized to guarantee the suitability of multiple HS-SPME. Significant matrix interference was observed among various types of pickles and the multiple HS-SPME procedure was proved to be effective in avoiding the matrix effect by a complete recovery of the analyte. The method showed satisfactory linearity (0.1-100 mg kg(-1)), precision (4.25%, n = 5), and detection limit (0.038 mg kg(-1)). The accuracy of the method was evaluated by comparison with standard addition method and the results were statistically equivalent. The study indicates that the multiple HS-SPME procedure is simple, convenient, accurate, and low-cost, and most of all, can be used for quantitative analysis in complex matrix without matrix effect.

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Determination of Ethyl Carbamate in Sake Using Headspace Solid Phase Microextraction

Cited by 18 publications

References 17 publications

Rapid determination of ethyl carbamate in Chinese rice wine using headspace solid-phase microextraction and gas chromatography-mass spectrometry

Rapid determination of ethyl carbamate in Chinese rice wine using headspace solid-phase microextraction and gas chromatography-mass spectrometry

Rapid Quantification of Ethyl Carbamate in Spirits Using NMR Spectroscopy and Chemometrics

Multiple headspace solid‐phase microextraction using a new fiber for avoiding matrix interferences in the quantitative determination of ethyl carbamate in pickles

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