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  • P-ISSN1225-0163
  • E-ISSN2288-8985
  • SCOPUS, ESCI, KCI

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  • P-ISSN 1225-0163
  • E-ISSN 2288-8985

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가스크로마토그래피/질량분석기를 이용한 식품 중 클로로프로판올 화합물 분석

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

분석과학 / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2008, v.21 no.6, pp.543-552
김은주 (식품의약품안전청)
박성국 (식품의약품안전청,신종유해물질팀)
최동미 (식품의약품안전청)
김은주, 박성국, & 최동미. (2008). 가스크로마토그래피/질량분석기를 이용한 식품 중 클로로프로판올 화합물 분석. 분석과학, 21(6), 543-552.
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초록

식품 중 클로로프로판올 화합물인 3-MCPD (3-monochloropropane-1,2-diol, <TEX>$C_3H_7ClO_2$</TEX>, MW. 110) 및 1,3-DCP (1,3-dichloropropan-2-ol, <TEX>$C_3H_6Cl_2O$</TEX>, MW. 128)를 분석하는 효과적인 방법을 확립하였다. 시료를 5M NaCl용액으로 균질화 한 후 알루미늄옥사이드와 섞어 유리컬럼에 충진하고 디클로로메탄으로 시료 중 클로로프로판올 화합물을 용출하였다. 용출된 클로로프로판올 화합물은 감압증류장치와 질소가스로 농축한 뒤 HFBA (Heptafluorobutyric anhydride, <TEX>$C_8F_{14}O_3$</TEX>, MW. 410)로 유도체화하여 GC/MS로 분석하였다. 3-MCPD-HFBA 유도체화 화합물(MW. 502)은 m/z 253, 275, 289, 291, 453를 선택이온으로 하고 1,3-DCP-HFBA 유도체화 화합물(MW. 325)은 110, 275, 277를 선택이온으로 설정하여 정성 정량 하였다. 확립된 분석법의 정량한계는 3-MCPD 및 1,3-DCP 모두 0.01 mg/kg이었고, 0.01~1.00 mg/kg의 농도범위에서 직선성(<TEX>$R^2{\geq}0.999$</TEX>)이 좋았으며 평균회수율은 약 97%내외였다. 확립된 분석법을 이용하여 다양한 식품 중 클로로프로판올 화합물을 조사한 결과, 0.0~0.3 mg/kg (n

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

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.

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


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