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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

: Berger-Preiß, E.; Gerling, S.; Apel, E.; Lampen, A.; Creutzenberg, O.


Analytical and bioanalytical chemistry 398 (2010), Nr.1, S.313-318
ISSN: 1618-2642 (Print)
ISSN: 1618-2650 (Online)
Fraunhofer ITEM ()
biomonitoring; 3-chloropropane-1,2-diol; negative chemical ionization; rat; blood; Urine; gas chromatography; mass spectrometry

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.