Comparison of the Analytical Method for 3-Monochloropropane-l,2-diol in Food

摘要

The studies for the derivatization of 3-monochloropropane-l,2-diol (3-MCPD) were performed mainly as acylation with HFBI (heptafluorobutyrylimidazole), alkylation with PB A (phenylboric acid) and silylation with BSTFA (N,O-bis[trimethylsilyl]trifluoroacetamide). Also silylation with MTBSTFA(N-methyl-N-ttert.-butyldimethylsilyl] trifluoro-acetamide) 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 ug/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 toeliminate 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 l,2-dibromo-3-chloropropane, respectively. The limit of detectionfor PB-MCPD and TMS-MCPD were 10.16 and 7.06 ug/kg on GC/MSD, respectively. HFB-MCPD derivative showed the lowest detection limits 2.98 and 5.32 fig/kg by GC/ECD and GC/MSD, respectively.