Abstract
Application of gas chromatography-mass spectrometry (GC-MS) can significantly improve trace analyses of compounds in complex matrices from natural environments compared to gas chromatography only. A GC-MS/MS technique for determination of poly-β-hydroxybutyrate (PHB), a bacterial storage compound, has been developed and used for analysis of two soils stored for up to 319 d, fresh samples of sewage sludge, as well as a pure culture of Bacillus megaterium. Specific derivatization ¶of β-hydroxybutyrate (3-OH C4 : 0) PHB monomer units by N-tert-butyl-dimethylsilyl-N-methyltrifluoracetamide (MTBSTFA) improved chromatographic and mass spectrometric properties of the analyte. The diagnostic fragmentation scheme of the derivates tert-butyldimethylsilyl ester and ether of β-hydroxybutyric acid (MTBSTFA-HB) essential for the PHB identification was shown. The ion trap MS was used, therefore the scan gave the best sensitivity and with MS/MS the noise decreased, so the S/N was better and also with second fragmentation the amount of ions increased compared to SIM. The detection limit for MTBSTFA-HB by GC-MS/MS was about 10–13 g μL–1 of injected volume, while by GC (FID) and GC-MS (scan) it was around 10–10 g μL–1 of injected volume. Sensitivity of GC-MS/MS measurements of PHB in arable soil and activated sludge samples was down to 10 pg of PHB g–1 dry matter. Comparison of MTBSTFA-HB detection in natural soil sample by GC (FID), GC-MS (scan) and by GC-MS/MS demonstrated potentials and limitations of the individual measurement techniques.
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Received: 25 September 1999 / Revised: 2 December 1999 / Accepted: 10 December 1999
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Elhottová, D., Tříska, J., Petersen, S. et al. Analysis of poly-β-hydroxybutyrate in environmental samples by GC-MS/MS. Fresenius J Anal Chem 367, 157–164 (2000). https://doi.org/10.1007/s002160051617
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DOI: https://doi.org/10.1007/s002160051617