Analysis of 11-dehydrothromboxane B2 in human urine improved by use of gas chromatography/high-resolution selected ion monitoring with18O2-labelled analogue as an internal standard
| Autor: | Michinao Mizugaki, Noriaki Harima, Yumiko Nakagawa, Masataka Ishibashi, Takanori Hishinuma |
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| Rok vydání: | 1994 |
| Předmět: |
Chromatography
Gas Chromatography Resolution (mass spectrometry) Chemistry Silica gel Spectrometry Mass Secondary Ion Urine Oxygen Isotopes Reference Standards respiratory system Mass spectrometry Biochemistry Thromboxane B2 chemistry.chemical_compound Molecular Medicine Indicators and Reagents lipids (amino acids peptides and proteins) Selected ion monitoring Gas chromatography Derivatization Spectroscopy Derivative (chemistry) circulatory and respiratory physiology |
| Zdroj: | Biological Mass Spectrometry. 23:612-620 |
| ISSN: | 1096-9888 1052-9306 |
| DOI: | 10.1002/bms.1200231003 |
| Popis: | Gas chromatography/high-resolution selected ion monitoring (GC/HR-SIM) for the determination of 11-dehydrothromboxane B2 (11-dehydro-TXB2) in human urine is described. Combined use of the lactone ring opening reaction and dimethylisopropylsilylation has been adopted for the analysis of 11-dehydro-TXB2, to give a new chemically stable derivative. The feasibility of using this derivative for the analysis of 11-dehydro-TXB2 in human urine has been evaluated. Following the addition of 18O2-labelled analogue, for use as an internal standard, the samples were extracted using chromatographic separation with Bond Elut C18 and silica gel. Derivatization of the extracted 11-dehydro-TXB2 was followed by GC/SIM at resolution of 5000. This method enables selective detection of 11-dehydro-TXB2 in human urine without serious interference from other endogenous substances. In 11 volunteers, the mean urinary excretions of 11-dehydro-TXB2 was 547.6 +/- 217.6 ng per day. |
| Databáze: | OpenAIRE |
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