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


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.


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


  1. JECFA (Joint FAO/WHO Expert Committee on Food Additives) Prepared by the 57th meeting of the JECFA. WHO Food additives series, No. 48. WHO, Geneva, 401-432 (2002)
  2. S. Robjohns, R. Marshall, M. Fellows and G. Kowalczyk, Mutagenesis, 18, 401-404(2003) https://doi.org/10.1093/mutage/geg017
  3. C. Crews, G. LeBrun and P. Brereton, Food Additives and Contaminants, 19, 343-349(2002) https://doi.org/10.1080/02652030110098580
  4. P. Nyman, G. Diachenko and G. Perfetti, Food Additiv., Contamin. 20, 903-905(2003) https://doi.org/10.1080/02652030310001603783
  5. C. Crew, P. Brereton and A. Davies, Food Additiv. Contamin. 18, 271-280(2001) https://doi.org/10.1080/02652030120064
  6. G. J. Spyres, Chromatogr. A. 638 , 71-74(1993) https://doi.org/10.1016/0021-9673(93)85009-V
  7. D. Meierhans, S. Bruehlmann, J. Meili and C. Taeschler, J. Chromatogr. A. 802, 325-333 1998) https://doi.org/10.1016/S0021-9673(97)01188-6
  8. Food Standard Agency. Surveillance Information Sheet, No. 15/01 (2001)
  9. C. Crew, S. Hasnip, S. Chapman, P. Hough, N. Potter, J. Todd, P. Brereton and W. Matthews, Food Additv. Contamin. 20, 916-922(2003) https://doi.org/10.1080/02652030310001605989
  10. COC (Committee on Carcinogenicity of Chemicals in Food. Statement, COC/01/S1, January (2001)
  11. P. Nyman, G. Diachenko and G. Perfetti, Food Additiv. Contamin. 10, 909-915(2003)
  12. C. Hamlet, Food Addti. Contam. 15, 451-465(1998) https://doi.org/10.1080/02652039809374666
  13. K. Ushuima, Y. Deguchi, K. Kikukawa, T. Nomura and T. Adach, Shokushin Eiseigaku Zasshi, 36, 360-364 (1995) https://doi.org/10.3358/shokueishi.36.360
  14. L. E. Rodman and R. D. Ross, J. Chromatogr. A. 69, 97-103(1986)
  15. Food Standard Agency. Surveillance Information Sheet, No. 187 (1991)
  16. J. Valisek, K. Davidek, V. Kubelka, Z. Janicek, Z. Svobodova and Z. J. Simikova, Agric. Food Chem. 28, 1142-1144(1980) https://doi.org/10.1021/jf60232a022
  17. P. Collier, D. Cromie and A. J. Davies, Am. Oil Chem. Soc. 68, 785-790(1991) https://doi.org/10.1007/BF02662173
  18. W. J. Plantinga, W. G. Van Toorn and G. H. D. J. Stegen, Chromatogr. A. 555, 311-314(1991) https://doi.org/10.1016/S0021-9673(01)87196-X
  19. W. Chung, K. Hui and S. Cheng, J. Chrom. A., 952, 185-192(2002) https://doi.org/10.1016/S0021-9673(02)00062-6
  20. Food Standard Agency. Surveillance Information Sheet, No. 181 (1991)
  21. European Commision Directorate-General Health and Consumer Protection. http://europa.eu.int/comm/food/ food/chemicalsafety/contaminants/mcpd_en.htm
  22. P. Brereton, J. Kelly, C. Crews, S. Honour and R. J. Wood, AOAC Intl., 84, 455-465(2001)
  23. H Lee and C. Oh, The annual report of National Institute of Toxicological Research 1, 265-312(2002)
  24. E. J. Kissa, Chromatogr. 605, 134-138(1992) https://doi.org/10.1016/0021-9673(92)85038-U
  25. B. Lynch, D. Bryant, G. Hook, E. Nestmann and I. Munro, International Journal of Toxicology, 17, 47-76 (1998) https://doi.org/10.1177/109158189801700307
  26. S. Abu-El-Haj, M. Bogusz, Z. Ibrahim, H. Hassan and M. Tufail, Food control, 18, 81-90(2007) https://doi.org/10.1016/j.foodcont.2005.08.014
  27. Food Standard Agency. Surveillance Information Sheet, No. 14/01 (2001)
  28. C. Crews, P. Hough, P. Brereton, D. Harvey, R. MacArthur and W. Matthews, Food Additi. Contamin. 19, 22-27(2002) https://doi.org/10.1080/02652030110085395