Development and validation of a method for the determination of total fatty acid esters of chloropropanols in edible vegetable oils by gas chromatography-mass spectrometry
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(Wuhan Institute for Food and Cosmetic Control,Hubei Wuhan 430012,China)

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    Abstract:

    To establish a method for the simultaneous determination of total fatty acid esters of 4 chloropropanols including 3-monochloropropane-1,2-diol (3-MCPD esters), 2-monochloropropane-1,3-diol (2-MCPD esters), 1,3-dichloropropan-2-ol (1,3-DCP esters) and 2,3-dichloropropan-1-ol (2,3-DCP esters) in edible vegetable oils by gas chromatography-mass spectrometry (GC-MS).Methods The edible vegetable oil samples were dissolved in tert-butyl methyl ether/acetic ether, followed by ester cleavage reaction using sodium methylate/methanol as the reagent. The solution was neutralized with acetic acid and cleaned up with hexane, then purified by matrix solid-supported liquid-liquid extraction using diatomaceous earth as the sorbent. After being derivatized with heptafluoro butyrylimidazole (HFBI), the analytes were detected by GC-MS and quantified by the multi-isotopic internal standards. Results Validated by five inspection and research institutes, a good linear relationship between peak area and concentrations was obtained within the range of 0.02-0.4 mg/L with correlation coefficients(r2) above 0.999 for 4 kinds of chloropropanols esters(calculated as dissociated chloropropanols). Recoveries ranged from 78.5% to 109.8% at spiked levels ranging from 0.2 to 2 mg/kg, and the relative standard deviations (RSDs) were in the range of 2.2%-18.8%. The limits of detection were 0.1 mg/kg for all the chloropropanols esters.Conclusion The collaborative validate test results validated by five inspection and research institutes and proficiency test results of the official Food Analysis Performance Assessment Scheme (FAPAS) indicated that the method presented a good linear relationship, and is low-cost, accurate and sensitive, suitable for the determination of total fatty acid esters of chloropropanols in edible vegetable oils.

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GONG Rui, MIAO Hong, JIN Shao-ming, JIANG Xiao-ming, HOU Jing, YANG Yong, LU Yue-peng. Development and validation of a method for the determination of total fatty acid esters of chloropropanols in edible vegetable oils by gas chromatography-mass spectrometry[J].中国食品卫生杂志,2016,28(3):333-339.

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  • Received:August 21,2015
  • Revised:
  • Adopted:
  • Online: June 02,2016
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