Optimization of an Aqueous Two-Phase System for the Determination of Trace Ethyl Carbamate in Red Wine

Abstract

In this study, a novel method using gas chromatography–mass spectrometry coupled with ethanol and K2HPO4 aqueous two-phase system (ATPS) was established for the quantitative determination of trace ethyl carbamate (EC) in red wine. The parameters that influence EC extraction in an aqueous two-phase system, including extraction temperature, time, pH, and ethanol concentration, were optimized. Method validation results indicated that the regression coefficient of the proposed method was 0.9979 in the linear range of 10 to 100 μg/L, and the limits of detection and quantification were 2.8 and 9.2 μg/L, respectively. Four red wine samples made from different grape varieties were processed by the proposed method for the repeatability verification, and EC concentrations were between 15.8 and 37.3 μg/L, with the relative standard deviations ranging from 3.5 to 6.6%. Results of the precision assay showed the average recovery of EC in red wine at 95.4 to 107.1%, with the relative standard deviations ranging from 1.4 to 6.2%. This method proved to be simple and reliable for quantitative determination of trace EC in red wine and would give guidance for quality monitoring of various red wines in the production process.

Comparison of Extraction Methods and Extraction Optimization in Aqueous Two-Phase System for Ethyl Carbamate Analysis in Model Systems for Maesil Wine

“…This method is time-consuming, but it is more environmentally friendly and cost-effective because it is simple to operate and does not require an organic solvent. Furthermore, if the ethanol and salt concentrations are properly adjusted, a maximum extraction efficiency of about 90% or more can be achieved ( Ma et al, 2019 ).…”

“…IX). According to Ma et al (2019) , when the concentration of ethanol is about 55%, the extraction efficiency is highest (≥90%). In this experiment, after adjusting the ethanol concentration to 50%, the extraction efficiency of EC was about 90%.…”

Occurrence of Ethyl Carbamate in Foods and Beverages: Review of the Formation Mechanisms, Advances in Analytical Methods, and Mitigation Strategies

“…Sample preparation can be virtually eliminated with headspace solid-phase microextraction, which has been used to analyze both alcoholic beverages and solid foods (87,137,158,219). Additional approaches with potential to increase sample throughput include microextraction by packed sorbent, ultrasound-assisted microextraction, pressurized liquid extraction, and aqueous two-phase extraction systems (117,124,125,135).…”

Peptide-Based Molecularly Imprinted Polymer: A Visual and Digital Platform for Specific Recognition and Detection of Ethyl Carbamate

“…6 Ma et al also used GC−MS coupled with ethanol and K 2 HPO 4 aqueous two-phase system for EC detection with an LOD of 2.8 μg L −1 . 7 On the basis of GC− MS, the experimental scheme was improved, and the EC fluorescence recognition signal was given by derivatization pretreatment. Zhou et al used HPLC with fluorescence detection to detect EC with derivatization of 9-xanthydrol solution.…”

“…Leca et al used a rapid and sensitive GC–MS methodology for EC determination in fortified wines using microextraction by packed sorbents, and the limit of detection (LOD) was 1.5 μg L –1 . Ma et al also used GC–MS coupled with ethanol and K 2 HPO 4 aqueous two-phase system for EC detection with an LOD of 2.8 μg L –1 . On the basis of GC–MS, the experimental scheme was improved, and the EC fluorescence recognition signal was given by derivatization pretreatment.…”