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Determination of stigmasterol hydroperoxides using high-performance liquid chromatography-mass spectrometry with atmospheric pressure chemical ionization

Author

Listed:
  • S. Kemmo

    (Department of Applied Chemistry and Microbiology, Division of Food Chemistry, University of Helsinki, Finland)

  • V. Ollilainen

    (Department of Applied Chemistry and Microbiology, Division of Food Chemistry, University of Helsinki, Finland)

  • A.-M. Lampi

    (Department of Applied Chemistry and Microbiology, Division of Food Chemistry, University of Helsinki, Finland)

  • V. Piironen

    (Department of Applied Chemistry and Microbiology, Division of Food Chemistry, University of Helsinki, Finland)

Abstract

A new specific method using high-performance liquid chromatography-mass spectrometry (HPLC-MS) for the detection of stigmasterol hydroperoxides was developed. Hydroperoxides of stigmasterol were obtained by photo-oxidation (90 min) in the presence of methylene blue as a sensitizer. The separation was performed using normal-phase chromatographic conditions. The MS detection was carried out with an ion-trap mass spectrometer using atmospheric pressure chemical ionization (APCI) and positive ion mode. Stigmasterol hydroperoxides were seen to produce no protonated molecular ions [M + H]+ but instead fragments representing loss of one or two water molecules [M - H2O + H]+, [M - 2H2O + H]+, loss of hydrogen peroxide [M - H2O2 + H]+ or loss of hydrogen peroxide and water [M - H2O2 - H2O + H]+. The results showed that positional isomers of hydroperoxides had different fragmentation patterns and relative ion abundances. On the other hand anomeric isomers had more similar fragmentation. As a conclusion the method developed showed to be a useful tool for investigation the oxidation mechanism of sterols.

Suggested Citation

  • S. Kemmo & V. Ollilainen & A.-M. Lampi & V. Piironen, 2004. "Determination of stigmasterol hydroperoxides using high-performance liquid chromatography-mass spectrometry with atmospheric pressure chemical ionization," Czech Journal of Food Sciences, Czech Academy of Agricultural Sciences, vol. 22(SpecialIs), pages 144-146.
    • Handle: RePEc:caa:jnlcjf:v:22:y:2004:i:specialissue:id:10639-cjfs
    DOI: 10.17221/10639-CJFS
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