Increasing thermospray response for cortisol by derivatization
| Autor: | Jan Paulson, Claes Lindberg |
|---|---|
| Rok vydání: | 1991 |
| Předmět: |
Detection limit
Chromatography Hydrocortisone Organic Chemistry Thermospray Acetylation General Medicine Mass spectrometry Biochemistry Gas Chromatography-Mass Spectrometry Mass Spectrometry Analytical Chemistry chemistry.chemical_compound Acetic anhydride chemistry Selected ion monitoring Gas chromatography–mass spectrometry Derivatization Triethylamine hormones hormone substitutes and hormone antagonists Chromatography Liquid |
| Zdroj: | Journal of chromatography. 554(1-2) |
| Popis: | The 21-hydroxyl group of cortisol was selectively acetylated under mild conditions without affecting the more sterically hindered 11 beta- and 17 alpha-hydroxyl groups. The reaction was performed with a mixture of acetic anhydride and triethylamine in acetonitrile and was complete in less than 15 min at room temperature. The thermospray mass spectrum of cortisol 21-acetate showed minimal fragmentation with the [M + H]+ ion as the base peak. High sensitivity was achieved for acetylated cortisol during selected ion monitoring, the signal-to-noise ratio being increased by a factor of about 4, compared to underivatized cortisol. The limit of detection of cortisol 21-acetate was estimated at 0.24 pmol injected, making thermospray liquid chromatography-mass spectrometry competitive with gas chromatography-mass spectrometry for the determination of cortisol in biological fluids. |
| Databáze: | OpenAIRE |
| Externí odkaz: |
|