Citation: LI Shan, YI Qing, MIAO Hong, WU Yong-Ning. Determination of Total Fatty Acid Esters of Chloropropanols in Edible Vegetable Oils by Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(6): 893-900. doi: 10.11895/j.issn.0253-3820.150718 shu

Determination of Total Fatty Acid Esters of Chloropropanols in Edible Vegetable Oils by Gas Chromatography-Mass Spectrometry

Key Laboratory of Food Safety Risk Assessment, Ministry of Health, China National Center for Food Safety Risk Assessment, Beijing 100021, China

Received Date: 16 October 2015
Revised Date: 4 December 2015

Fund Project: This work was supported by the State Key Development Program for Basic Research of China (No.2012CB720804)

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A method was established for the simultaneous determination of the total fatty acid esters of chloropropanols in edible oils by gas chromatography-mass spectrometry combined with isotope dilution technology. The samples were hydrolyzed with sodium methylate-methanol, and then purified by diatomite cartridge. After being derivatized with heptafluorobutyrylimidazole (HFBI), the target analytes were determined by GC-MS with the deuteriumchloropropanols esters as the internal standards. An excellent linear correlation in the range of 0.050-2.000 mg/L was acquired for 3-monochloropropane-1,2-diol (3-MCPD) esters, 2-MCPD esters, dichloropropan-2-ol (1,3-DCP) esters and 2,3-dichloropropan-1-ol (2,3-DCP) esters, with all the correlation coefficients (r) higher than 0.9995. The limits of detection (LODs) for 3-MCPD esters, 2-MCPD esters, 1,3-DCP esters and 2,3-DCP esters were 0.015, 0.015, 0.030, and 0.030 mg/kg, respectively, and the limits of quantitation (LOQ) were 0.050, 0.050, 0.100, and 0.100 mg/kg, respectively. The average spike recoveries of the four kinds of chloropropanols esters in blank extra virgin olive oil matrix were typically in a range of 87.0%-110.5% with the relative standard deviations (RSDs) less than 10.1%. The detection rates of 3-MCPD esters, 2-MCPD esters, 1,3-DCP esters and 2,3-DCP esters in 74 edible oil samples were 94.6%, 63.5%, 5.4%, and 0%, respectively. The contamination levels of 3-MCPD esters, 2-MCPD esters and 1,3-DCP esters were in the range of not detected (ND) to 10.646 mg/kg, ND to 3.617 mg/kg and ND to 0.089 mg/kg, respectively. This method is accurate and rugged for the simultaneous determination of total fatty acid esters of chloropropanols in edible vegetable oils.
- Edible vegetable oil,
- Fatty acid esters of chloropropanols,
- Gas chromatography-mass spectrometry,
- Isotope dilution technology
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