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

2019 ◽  
Vol 82 (8) ◽  
pp. 1377-1383 ◽  
Author(s):  
LIJUAN MA ◽  
WENZHE TONG ◽  
LIPING DU ◽  
SHIYONG HUANG ◽  
JINYAN WEI ◽  
...  

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.

1995 ◽  
Vol 230 (2) ◽  
pp. 254-258 ◽  
Author(s):  
C. Guermant ◽  
J. Brygier ◽  
D. Baeyensvolant ◽  
M. Nijs ◽  
J. Vincentelli ◽  
...  

2001 ◽  
Vol 84 (6) ◽  
pp. 1818-1827 ◽  
Author(s):  
Angelo Visconti ◽  
Michelangelo Pascale ◽  
Gianluca Centonze ◽  
E Anklam ◽  
A M Betbeder ◽  
...  

Abstract The accuracy, repeatability, and reproducibility characteristics of a liquid chromatographic method for the determination of ochratoxin A (OTA) in white wine, red wine, and beer were established in a collaborative study involving 18 laboratories in 10 countries. Blind duplicates of blank, spiked, and naturally contaminated materials at levels ranging from ≤0.01 to 3.00 ng/mL were analyzed. Wine and beer samples were diluted with a solution containing polyethylene glycol and sodium hydrogen carbonate, and the diluted samples were filtered and cleaned up on an immunoaffinity column. OTA was eluted with methanol and quantified by reversed-phase liquid chromatography with fluorometric detection. Average recoveries from white wine, red wine, and beer ranged from 88.2 to 105.4% (at spiking levels ranging from 0.1 to 2.0 ng/mL), from 84.3 to 93.1% (at spiking levels ranging from 0.2 to 3.0 ng/mL), and from 87.0 to 95.0% (at spiking levels ranging from 0.2 to 1.5 ng/mL), respectively. Relative standard deviations for within-laboratory repeatability (RSDr) ranged from 6.6 to 10.8% for white wine, from 6.5 to 10.8% for red wine, and from 4.7 to 16.5% for beer. Relative standard deviations for between-laboratories reproducibility (RSDR) ranged from 13.1 to 15.9% for white wine, from 11.9 to 13.6% for red wine, and from 15.2 to 26.1% for beer. HORRAT values were ≤0.4 for the 3 matrixes.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Sabah Shiri ◽  
Tahere Khezeli ◽  
Shahram Lotfi ◽  
Sina Shiri

A novel, simple, and more sensitive spectrophotometric procedure has been developed for the determination of brilliant blue FCF in water and food samples by an aqueous two-phase system (ATPS). In this method, adequate amount of polyethylene glycol/ sodium carbonate (PEG-4000/Na2CO3) was added to aqueous solution for formation of a homogeneous solution. To the mixture solution, suitable amount ofNa2CO3was added, the mixture solution was shaken until the salt was dissolved, and then it was separated into two clear phases easily and rapidly. The target analyte in the water sample was extracted into the polyethylene glycol phase. After extraction, measuring the absorbance at 634 nm was done. The effects of different parameters such as polyethylene glycol (type and concentration), pH, salt (type and amount), centrifuge time, and temperature on the ATPS of dye was investigated and optimum conditions were established. Linear calibration curves were obtained in the range of 0.25–750 ng/mL for brilliant blue FCF under optimum conditions. Detection limit based on three times the standard deviation of the blank (3Sb) was 0.12 ng/mL. The relative standard deviation (RSD) for 400 ng/mL was 3.14%. The method was successfully applied to the determination of brilliant blue FCF in spiked samples with satisfactory results. The relative recovery was between 96.0 and 102.2%.


2021 ◽  
Vol 267 ◽  
pp. 02010
Author(s):  
Rui Wang ◽  
Xueqin Zhang ◽  
Qian Zhou

Moringa leaves were used as raw materials, ethanol and ammonium sulfate were used to construct a aqueous two-phase system to extract the flavonoids from Moringa leaves. The solid-liquid ratio, ethanol content, ultrasonic extraction time, and ultrasonic extraction temperature were selected as single factors, and the extraction process of flavonoids was optimized through single-factor experiments and orthogonal experiments. The optimal process was: 1:110 of solid-liquid ratio, 45 % of ethanol concentration, 15 minutes of ultrasonic extraction time, 70 °C of ultrasonic extraction temperature. Under this condition, the extraction rate of Moringa leaf flavonoids reached 8.37 %.


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