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Analysis of poly-beta-hydroxybutyrate in environmental samples by GC-MS/MS
- Source :
- Fresenius' journal of analytical chemistry. 367(2)
- Publication Year :
- 2001
-
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-beta-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 beta-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 beta-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 microL(-1) of injected volume, while by GC (FID) and GC-MS (scan) it was around 10(-10) g microL(-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.
- Subjects :
- Detection limit
Analyte
Chromatography
Sewage
Chemistry
Polyesters
Hydroxybutyrates
Mass spectrometry
Biochemistry
Sensitivity and Specificity
Gas Chromatography-Mass Spectrometry
chemistry.chemical_compound
Bacillus megaterium
Soil Pollutants
Environmental Pollutants
Gas chromatography
Ion trap
Gas chromatography–mass spectrometry
Glycolipids
Derivatization
Sludge
Subjects
Details
- ISSN :
- 09370633
- Volume :
- 367
- Issue :
- 2
- Database :
- OpenAIRE
- Journal :
- Fresenius' journal of analytical chemistry
- Accession number :
- edsair.doi.dedup.....a9594e2083b2a9726370aef0904f03d4