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KMID : 0380620070390040360
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Korean Journal of Food Science and Technology
2007 Volume.39 No. 4 p.360 ~ p.365
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Comparison of the Analytical Method for 3-Monochloropropane-1,2-diol in Food
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Oh Chang-Hwan
Yoo Seung-Seok
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Abstract
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The studies for the derivatization of 3-monochloropropane-1,2-diol (3-MCPD) were performed mainly as acylation with HFBI (heptafluorobutyrylimidazole), alkylation with PBA (phenylboric acid) and silylation with BSTFA (N,O-bis[trimethylsilyl]trifluoroacetamide). Also silylation with MTBSTFA(N-methyl-N-[tert.-butyldimethylsilyl] trifluoroacetamide) and acylation with MBTFA (N-Methyl-bis[trifluoro-acetamide]) were also considered. Except the TBDMS derivative of 3-MCPD, all the derivatives were detected well. The derivatives of 3-MCPD with HFBI, PBA and BSTFA showed below 10 μg/kg which was sensitive enough to satisfy Korea maximum residue limit 0.3 mg/kg. Among the tested adsorbents, Extrelut20 and Florisil were evaluated as the proper adsorbents to eliminate the soy sauce matrix for 3-MCPD. Ethyl acetate was the most efficient eluent with good recovery rate. The desired surrogate compound and internal standard were 1,2-butanediol and 1,2-dibromo-3-chloropropane, respectively. The limit of detection for PB-MCPD and TMS-MCPD were 10.16 and 7.06 μg/kg on GC/MSD, respectively. HFB-MCPD derivative showed the lowest detection limits 2.98 and 5.32 μg/kg by GC/ECD and GC/MSD, respectively.
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KEYWORD
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3-monochloropropane-1, 2-diol, derivatization, adsorbents, eluent, soy sauce, detection Limit
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