Study of chloropropanols in soy sauce by gas chromatography-triple quadrupole mass spectrometry with coupled column separation without derivatisation.

A qualitative and quantitative determination method for chloropropanols in soy sauce was developed by GC-MS/MS with coupled column separation without derivatisation. The target compounds were 1,3-dichloropropan-2-ol (1,3-DCP), 2,3-dichloropropan-1-ol (2,3-DCP), 3-monochloropropane-1,2-diol (3-MCPD) and 2-monochloropropane-1,3-diol (2-MCPD). 3-MCPD-d(5) was used as an isotope internal standard for MCPDs and 1,3-DCP-d(5) for DCPs. After spiking with internal standards and mixed with 1 g of Extrelut™ NT, about 1 g of the sample was washed by 4 ml of hexane and the analytes were eluted with 15 ml of 95% (v/v) ethyl ether/hexane mixture. The concentrated extract was directly injected without derivatisation, separated by a coupled column - a 3 m Innowax (polyethylene glycol) combined with a 30 m DB-5 ms ((5%-phenyl)-methylpolysiloxane) by a quartz capillary column connector - and detected by GC-MS/MS. The limits of detection (LODs) in the sample matrix were 1.0, 2.5, 5.0 and 5.0 µg kg(-1) for the above chloropropanols, respectively. The relative proportions of 2-MCPD/3-MCPD ranged from 0.19 to 3.74 in soy sauce samples. 2,3-DCP and 2-MCPD were more stable than 1,3-DCP and 3-MCPD under alkaline condition. The levels of chloropropanols can be decreased by an alkaline treatment process.