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

가스크로마토그래피/질량분석기를 이용한 식품 중 클로로프로판올 화합물 분석

  • Kim, Eunju ;
  • Park, Sungkug ;
  • Choi, Dongmi
  • 김은주 ;
  • 박성국 ;
  • 최동미
  • Received : 2008.12.04
  • Accepted : 2008.12.12
  • Published : 2008.12.25

Abstract

This paper described the relatively sensitive and simultaneous analytical method for 3-monochloropropane-1,2-diol (3-MCDP, $C_3H_7ClO_2$, MW. 110) as well as 1,3-dichloropropan-2-ol (1,3-DCP, $C_3H_6Cl_2O$, 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 $N_2$ blow serially were derivatized with HFBA (Heptafluorobutyric anhydride, $C_8F_{14}O_3$, 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 ($R^2{\geq}0.999$ at 0.010~1.000 mg/kg), and recovery rate (${\approx}97%$). 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.

Keywords

3-monochloropropane-1,2-diol;1,3-dichloropropan-2-ol;Analytical method;Survey

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