Analysis of derivatised steroids by matrix-assisted laser desorption/ionisation and post-source decay mass spectrometry.

Abstract:

:Neutral steroids are difficult to analyse using desorption ionisation methods coupled with mass spectrometry (MS). However, steroids with an unhindered ketone group can readily be derivatised with the Girard P (GP) reagent to give GP hydrazones. Steroid GP hydrazones contain a quaternary nitrogen atom and are readily desorbed in the matrix-assisted laser desorption/ionisation (MALDI) process, giving an improvement in sensitivity of two orders of magnitude. Steroids without a ketone group, but with a 3beta-hydroxy-Delta5 function, can be readily converted to 3-oxo-Delta4 steroids and subsequently derivatised to GP hydrazones for MALDI analysis. In addition to giving strong [M]+ ions upon MALDI, steroid GP hydrazones give informative post-source decay (PSD) spectra. By using the accurate mass of the precursor-ion measured by MALDI-MS, in combination with the structural information encoded in its PSD spectrum, steroid structures can readily be determined.

journal_name

Steroids

journal_title

Steroids

authors

Khan MA,Wang Y,Heidelberger S,Alvelius G,Liu S,Sjövall J,Griffiths WJ

doi

10.1016/j.steroids.2005.08.002

subject

Has Abstract

pub_date

2006-01-01 00:00:00

pages

42-53

issue

1

eissn

0039-128X

issn

1878-5867

pii

S0039-128X(05)00190-X

journal_volume

71

pub_type

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