Analytical and Bioanalytical Chemistry

, Volume 398, Issue 1, pp 313–318 | Cite as

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

  • Edith Berger-Preiß
  • Susanne Gerling
  • Elisabeth Apel
  • Alfonso Lampen
  • Otto Creutzenberg
Short Communication

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-d5, 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.

Figure

Typical ion chromatogram of spiked rat urine (25 ng/mL 3-MCPD)

Keywords

Biomonitoring 3-chloropropane-1,2-diol Rat Blood Urine Gas chromatography-mass spectrometry-negative chemical ionization 

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Copyright information

© Springer-Verlag 2010

Authors and Affiliations

  • Edith Berger-Preiß
    • 1
  • Susanne Gerling
    • 1
  • Elisabeth Apel
    • 1
  • Alfonso Lampen
    • 2
  • Otto Creutzenberg
    • 1
  1. 1.Fraunhofer Institute for Toxicology and Experimental MedicineHannoverGermany
  2. 2.Federal Institute for Risk AssessmentDepartment Food SafetyBerlinGermany

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