Detection of corticosteroids by high-performance liquid chromatography/negative ion chemical ionization mass spectrometry using a particle beam interface

Abstract

A normal-phase high-performance liquid chromatographic/particle beam mass spectrometric (negative chemical ionization) method has been developed for the detection of Synthetic corticosteroids (SC). Characteristic and reproducible full-scan spectra were obtained for the SC analysed. The limit of detection using selected ion monitoring for the molecular anion of beclomethasone was 500 pg. Urine from an equine to which 9a-fluoroprednisolone acetate had been administered was extracted by immunoaftinity chromatography and analysed by high-performance liquid chromatography-ultraviolet detection/particle beam mass spectrometry. Full-scan spectral data from these extracts allowed positive identification of 9a-fluoroprednisolone (isoflupredone) in the equine urine up to % h post administration.

Rapid determination of corticosteroids in urine by combined solid phase microextraction/liquid chromatography/mass spectrometry

“…5 Combined liquid chromatography with mass spectrometry (LC/MS) has also frequently been applied to steroid and steroid conjugate analysis, using both the positive and negative ion modes of the mass spectrometer. For example, thermospray (TSP), [6][7][8][9] frit fast atom bombardment (FAB), 10 particle-beam (PB), 11 electrospray (ESI) 2,[12][13][14] and atmospheric-pressure chemical ionization (APCI) 15,16 have been successfully used, with detection limits in urine or serum in the lower ng/ mL range, sometimes down to the higher pg/mL range.…”

Effect of organic modifier and temperature on the resolution of betamethasone and dexamethasone using a porous graphitic carbon column: Application to their identification and confirmation in human urine by LC‐ESI‐MS/MS

“…Therefore, a selective and sensitive method is required for their unambiguous identification and their simultaneous quantification in human urine to prevent their use as anabolic agents. On the other hand, these two compounds differ only in the stereoisomery of their C-16 methyl group, which unfavourably affects their separation by LC techniques with either normal phase [2] or RP [3 -7]. Moreover, they have very similar mass spectra [3,5,6,8] leading to a difficult distinction between them.…”

Development of QuEChERS-based extraction and liquid chromatography–tandem mass spectrometry method for quantifying flumethasone residues in beef muscle

“…Although the method is sensitive, it seems to be somewhat impractical, as corticosteroids are slightly volatile and can be denatured with heat (Delahaut et al, 1997) or require time-consuming derivatization or oxidation steps (Bevalot, Gaillard, Lehermitte, & Pepin, 2000;Courtheyn et al, 1994;Rodchenkov, Vedenin, Uralets, & Semenov, 1991). The best alternative to GC-MS/MS is liquid chromatography (LC)-MS (Marquet & Lachatre, 1999;Stanley, Wilhelmi, & Rodgers, 1994), in particular, reversed-phase (RP)-LC-MS (Bevalot et al, 2000;Fiori, Pierdominici, Longo, & Brambilla, 1998). Additionally, LC-MS/MS is the best candidate to increase specificity (Antignac, Le Bizec, Monteau, Poulain, & Andrè, 2000;Rizea Savu, Silvestro, Haag, & Sorgel, 1996;Tolgyesi et al, 2011).…”