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Optimization of ultrasonic‐assisted extraction of 3‐monochloropropane‐1,2‐diol (MCPD) and analysis of its esters from edible oils by gas chromatography–mass spectrometry
Author(s) -
Ma Fei,
Li Peiwu,
Matthäus Bertrand,
Zhang Wen,
Zhang Qi
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200145
Subject(s) - chromatography , chemistry , detection limit , extraction (chemistry) , gas chromatography–mass spectrometry , mass spectrometry , gas chromatography , ethyl acetate , sample preparation , solvent , isotope dilution , organic chemistry
In this paper, ultrasonic‐assisted extraction of 3‐chloropropane‐1,2‐diol and its esters from edible oils was studied with isotope dilution GC‐MS. Effects of several experimental parameters, such as types and concentrations of extracting solvent, ratios of liquid to material, extraction temperature, time of ultrasonic treatment on the extraction efficiency of 3‐chloropropane‐1,2‐diol and its esters from edible oils and sample preparation for calibration were compared and optimized. The optimal extraction conditions were suggested as 66 mg oil sample in mixture of 0.5 mL MTBE/ethyl acetate (20% v/v) and 0.5 mL of sulfuric acid/ n ‐propanol (0.3% v/v), being extracted for 30 min at 45°C under ultrasonic irradiation. Good linearity was gained in the range of 0.020–5.000 μg/g with the limit of detection (LOD) of 0.006 μg/g ( S/N = 3) and the limit of quantification (LOQ) of 0.020 μg/g ( S/N = 10). The recoveries at five spiked concentrations were ranged from 91.9 to 109.3% with RSD less than 9.4%. The method was successfully applied to the determination of 3‐chloropropane‐1,2‐diol and its esters amounts in rapeseed, sesame, peanut, camellia, and soybean oils.