A sensitive analytical method for determination of 3-monochloropropane-1,2-diol and 1,3-dichloropropan-2-ol in various foods by gas chromatography with mass spectrometer
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This paper described the relatively sensitive and simultaneous analytical method for 3-monochloropropane- 1,2-diol (3-MCDP, C3H7ClO2, MW. 110) as well as 1,3-dichloropropan-2-ol (1,3-DCP, C3H6Cl2O, MW. 128) in various foods. Food samples were homogenized in 5M NaCl solution, mixed with aluminum oxide and eluted with dichloromethane. The extracted chloropropanols were concentrated by rotary evaporator and N2 blow serially were derivatized with HFBA (Heptafluorobutyric anhydride, C8F14O3, MW. 410) and were determined by GC/MS using isotope dilution method. The characteristic molecular ions at m/z 253, 275, 289, 291, and 453 for HFBA derivatives of 3-MCPD (MW. 502) and 110, 275, and 277 for HFBA derivatives of 1,3-DCP (MW. 325) were chosen in selected ion mode. The method validation data showed sufficiently good properties of LOD (0.003 mg/kg), LOQ (0.010 mg/kg), linearity (R2≥0.999 at 0.010~1.000 mg/kg), and recovery rate ( 97%). The levels of chloropropanols in soy sauce, sauces, processed meat products, fishery products, and seasonings (n=56/157) determined by the presented method were 0.0~0.3 mg/kg.
Abstract
This paper described the relatively sensitive and simultaneous analytical method for 3-monochloropropane- 1,2-diol (3-MCDP, C3H7ClO2, MW. 110) as well as 1,3-dichloropropan-2-ol (1,3-DCP, C3H6Cl2O, MW. 128) in various foods. Food samples were homogenized in 5M NaCl solution, mixed with aluminum oxide and eluted with dichloromethane. The extracted chloropropanols were concentrated by rotary evaporator and N2 blow serially were derivatized with HFBA (Heptafluorobutyric anhydride, C8F14O3, MW. 410) and were determined by GC/MS using isotope dilution method. The characteristic molecular ions at m/z 253, 275, 289, 291, and 453 for HFBA derivatives of 3-MCPD (MW. 502) and 110, 275, and 277 for HFBA derivatives of 1,3-DCP (MW. 325) were chosen in selected ion mode. The method validation data showed sufficiently good properties of LOD (0.003 mg/kg), LOQ (0.010 mg/kg), linearity (R2≥0.999 at 0.010~1.000 mg/kg), and recovery rate ( 97%). The levels of chloropropanols in soy sauce, sauces, processed meat products, fishery products, and seasonings (n=56/157) determined by the presented method were 0.0~0.3 mg/kg.
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