[논문]가스크로마토그래피/질량분석기를 이용한 식품 중 클로로프로판올 화합물 분석

김은주; 박성국; 최동미

doi:10.5806/ast.2008.21.6.543

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 원문보기

분석과학 = Analytical science & technology, v.21 no.6, 2008년, pp.543 - 552

김은주 (식품의약품안전청 신종유해물질과) , 박성국 (식품의약품안전청 신종유해물질과) , 최동미 (식품의약품안전청 신종유해물질과)

초록
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식품 중 클로로프로판올 화합물인 3-MCPD (3-monochloropropane-1,2-diol, $C_3H_7ClO_2$, MW. 110) 및 1,3-DCP (1,3-dichloropropan-2-ol, $C_3H_6Cl_2O$, 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, $C_8F_{14}O_3$, 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($R^2{\geq}0.999$)이 좋았으며 평균회수율은 약 97%내외였다. 확립된 분석법을 이용하여 다양한 식품 중 클로로프로판올 화합물을 조사한 결과, 0.0~0.3 mg/kg (n=56/157) 수준으로 3-MCPD로 검출되었다.

Abstract ▼ AI-Helper

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.

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문제 정의

The improvements in detection of chloropropanols at low jig/kg level by modification of previous analytical methods and survey of chloropropanols in various foods were the objective of this research.

제안 방법

GC/MS analysis was carried out using a gas chromatograph equipped with mass spectrometer(1200 Triple Quadrupole GC/MS, Varian Co., Palo Alto, US) in the El mode at electron energy of 70 eV and source temperature of 230℃. The separation of chloropropanol derivatives was done on DB-5MS column(30 m x 0.
The analytical method was validated by determining the linearity, the limit of quantitation (LOQ), and recovery rate of chloropropanols (Table 3). The response of the calibration standards for both 3- MCPD and 1, 3-DCP were found to be linear at a concentration rage of 10~1000 ng/kg with correlation coefficients (R2) of 0.
There was no interference between peaks of targeted compounds as well as between peaks of targeted compounds and impurities. The targeted compounds were separated well in the order of 1, 3-DCP-刁5, 1, 3-DCP, 3-MCPD-刁5, and 3- MCPD, The spectra were analyzed by MS in El mode at the full scan range of m/z 50-550. There was no interfence noticed in the presented study although others16, 18 reported that interferences found at m/z 253 for 3-MCPD, The characteristic ions resulted from fragmentation of 3-MCPD and 1, 3- DCP derivatives were identical with fragment ions reported by Chung et aLe and Abu-El-Haj et al21 The major characteristic ions of each chloropropanol derivative were selected from each spectrum based on their relative response abundances to increase analytical sensitivity of measurements as described above (Fig.

성능/효과

The extraction capacity of chloropropanols was not significantly affected by dichloromethane volume. The 3-MCPD recovery (%) with 30 mL and 50 mL of dichloromethane extraction were 97」and 98.8%, respectively The 1D, C₃-P recovery (%) with different volume of dichloromethane were similar to those of 3-MCPD, which were 96.9% for 30 mL extraction and 97.3% for 50 mL extraction. It could be induced that 30 mL of dichloromethane was relatively sufficient to extract chloropropanols in samples.
The recovery rate of 3-MCPD and 1, 3-DCP were determined by analyzing various food (soy sauce, soup paste concentrate, and seasoning food powder) fortified with chcloropropanols at 50~400 ng/kg. The average recovery rates were 97.1% with 6.3% of RSD for 3-MCPD and 96.7% with 6.9% ofRSD for 1, 3-DCP.
in various food. The survey data showed that the detected level of 3-MCDP in foods was lower than that of standard in Food code.
The survey results of chloropropanols in various food items purchased from local grocery markets in Korea were summarized (Table 4). None of food tested was positive for 1, 3-DCP contamination.

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