Abstract
We have developed a highly selective and sensitive method using gas chromatography-mass spectrometry with negative chemical ionization for measuring 3-chloropropane-1,2-diol (3-MCPD) in rat blood and urine. Samples were adsorbed on silica gel, extracted with ethyl acetate, and derivatized by chemical derivatization with heptafluorobutyric acid anhydride. For quantification, matrix-based calibration curves and 3-MCPD-d 5, as an isotope-labeled internal standard, were used. The relative recoveries of 3-MCPD were between 80 and 110% in most cases and the relative standard deviations were typically less than 10%, with some exceptions. The limit of quantification of the method was found to be about 2 ng/mL. In conclusion, a valuable, robust, and sensitive method for detection of 3-MCPD is now available for biokinetics studies.
Typical ion chromatogram of spiked rat urine (25 ng/mL 3-MCPD)
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Acknowledgements
We would like to thank the German Federal Ministry of Food, Agriculture and Consumer Protection (BMELV) for financing this work and the Federal Institute for Risk Assessment (BfR) for its scientific advice.
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Berger-Preiß, E., Gerling, S., Apel, E. et al. Development and validation of an analytical method for determination of 3-chloropropane-1,2-diol in rat blood and urine by gas chromatography-mass spectrometry in negative chemical ionization mode. Anal Bioanal Chem 398, 313–318 (2010). https://doi.org/10.1007/s00216-010-3928-9
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DOI: https://doi.org/10.1007/s00216-010-3928-9