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Determination of 4 Kinds of Chloropropanols in Foods by Gas Chromatography-Mass Spectroscopy Coupled with Multi-Isotopic Internal Standard Technique

WU Shao-ming，FU Wu-sheng，FU Hai-qing，FANG Qin-mei，HUA Juan   

  1. 1. Fujian Provincial Key Laboratory of Zoonosis Research, Center for Disease Control and Prevention, Fuzhou 350001, China；
    2. Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China；
    3. College of Jinshan, Fujian Agriculture and Forestry University, Fuzhou 350002, China；
    4. Biotechnology Research Institute, Fujian Academy of Agricultural Sciences, Fuzhou 350003, China；
    5. College of Food Science, Fujian Agriculture and Forestry University, Fuzhou 350002, China
  • Online:2013-09-25 Published:2013-09-27

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Abstract:

An analytical method was developed to determine 4 kinds of chloropropanols in foods using gas
chromatography mass spectrometer coupled with the multi-isotopic internal standard technique. The performance
difference between different brands of HFBI as a derivativization reagent and internal standard selection for quantification
were discussed. Under the optimal conditions, the limits of detection (LOD) were 2.5–10 μg/kg for 4 kinds of
chloropropanols. According to the internal standard calibration, an excellent linearity between 100 ng and 2000 ng of
chloropropanols (R² ＞ 0.9990) was obtained. When chloropropanols were spiked at levels of 100, 200, 400 mg/kg in
soy sauce and seasoning powder of instant noodles, the average recovery rates were 90.1%–107%, with relative standard
deviation (RSD) of 3.37%–10.4% (n = 6). The application of only 2 kinds of internal standards (chloropropane-1,2-diol-d5
or 2-chloropropane-1,3-diol-d5 and 1,3-dichloro-2-propanol-d5) can reveal accurate and precise determination for 4 kinds
of chloropropanols. When 3-chloropropane-1,2-diol (3-MCPD) was used to calibrate 2-MCPD in foods, the level of
2-chloropropane-1,3-diol (2-MCPD) was only 52.1%–77.8% of the real content.

Key words: food, chloropropanol, dispersion matrix solid-phase extraction, isotopic internal standard technique, gas chromatography-mass spectrometer (GC-MS)