Direct identification and quantitation of prednisone in the presence of overlapping hydrocortisone by liquid chromatography with electrospray and atmospheric-pressure chemical-ionisation mass spectrometry.
The paper describes the application of liquid chromatography interfaced to a triple quadrupole mass spectrometer utilising the multiple reaction monitoring (MRM) mode. The technique was shown to provide detection limits lower than 0.01% for the analysis of prednisone in the presence of hydrocortisone. Prednisone was mixed in concentrations from 0.500 to 0.0005 ppm (corresponding to 1% to 0.001% of the hydrocortisone concentration). These solutions were assayed using MRM observing the product ion transitions of 359.2-->147.1 and 359.2-->171.2 and was shown to be capable of detecting co-eluting impurities at concentrations of less than 0.001% of the major component. The assay of prednisone was shown to be linear over the range 0.500-0.0005 ppm with a correlation coefficient of 0.999 and a precision of 6.9% at the concentration of 0.005 ppm. The analysis was carried out using both atmospheric pressure chemical ionisation (APCI) and electrospray ionisation (ESI) as an interface. However, for these compounds APCI provided significantly more sensitive data compared to ESI.
Mulholland
M
M
Department of Chemistry, Materials and Forensic Science, University of Technology, Sydney, Australia, NSW.
Whelan
T J
TJ
Rose
H
H
Keegan
J
J
D001274:Atmospheric Pressure; D002853:Chromatography, Liquid / Q000379:methods*; D006854:Hydrocortisone / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D011241:Prednisone / Q000032:analysis*; D012680:Sensitivity and Specificity
D011241:Prednisone; D006854:Hydrocortisone