Popis: |
The food contaminants including 3-chloro-1,2-propanediol (3-MCPD) and 3-MCPD fatty acid esters have been a matter of great concern in the past few years due to their toxicity and their occurrence in numerous foods. Recently, significant amounts of the isomeric compounds 2-chloro-1,3-propanediol (2-MCPD) fatty acid esters have been detected in refined oil samples. Gas Chromatography (GC) coupled with mass spectroscopy (MS) was used for the quantification of fatty acid esters of 2-Chloro-1,3-propandiol (2-MCPD), 3-Chloro-1,2- propandiol (3-MCPD) and glycidol in oil. Internal standards including 3-MCPD-ester-d5 (rac 1,2-bis-palmitoyl-3-chloropropanediol-d5), 2-MCPD-ester-d5 (1,3-Distearoyl-2- chloropropanediol-d5) and Glycidyl sterate-d5 were added to samples. Spiked samples were, then, incubated in NaBr/H2SO4 and H2SO4/MeOH solutions. They were, eventually, extracted with ethyl acetate and n-hexane solvents in order to convert Glycidyl esters to free MCPD and glycidol in samples before using phenylboronic acid derivative. The limit of quantitation was of 0.1 ppm (mg/kg). The recoveries at the concentration of 0.1 mg/kg ranged from 80 to 120% and the repeatability and reproducibility were less than 10%. |