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.
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.
Berger-Preiss
Edith
E
Fraunhofer Institute for Toxicology and Experimental Medicine, Nikolai-Fuchs-Strasse 1, 30625 Hannover, Germany. edith.berger-preiss@item.fraunhofer.de
Gerling
Susanne
S
Apel
Elisabeth
E
Lampen
Alfonso
A
Creutzenberg
Otto
O
D000818:Animals; D008401:Gas Chromatography-Mass Spectrometry; D005990:Glycerol / Q000031:analogs & derivatives* / Q000097:blood / Q000652:urine; D051381:Rats; D054928:Validation Studies as Topic; D000517:alpha-Chlorohydrin
D000517:alpha-Chlorohydrin; D005990:Glycerol