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Prednisolone measurement in human serum using liquid chromatography tandem mass spectrometry.
Ann Clin Biochem. 2005 Mar; 42(Pt 2):105-11.AC

Abstract

Prednisolone is a commonly prescribed corticosteroid used in the treatment of many diseases. Despite high doses of prednisolone, some patients appear to have subtherapeutic concentrations of the drug. It would be useful to measure prednisolone in this group to determine if they have poor absorption or compliance. Hence, we have developed a liquid chromatography-tandem mass spectrometry method for the determination of prednisolone in serum. Chromatography was performed using a C18 column, giving a retention time for both prednisolone and deuterated prednisolone (internal standard) of 1.6 min. Two transitions were monitored for both prednisolone and deuterated prednisolone. These were m/z 361.2 > 343.0 and m/z 361.2 > 146.9 for prednisolone, and m/z 367.2 > 349.0 and m/z 367.2 > 149.9 for the internal standard. The intra- and inter-batch imprecision was < 7% in both cases over a concentration range of 62.5-750 microg/L. The imprecision at the lower limit was 8%, the lower limit of quantitation was determined to be 30 microg/L and the method was linear up to 5000 microg/L. The method allows rapid prednisolone analysis because of a simplified sample extraction step, and has a cycle time of 3.5 min.

Authors+Show Affiliations

Owen LJ
Clinical Biochemistry Department, Wythenshawe Hospital, Southmoor Road, Wythenshawe, Manchester M23 9LT, UK. laura.owen@smuht.nwest.nhs.uk
Gillingwater S
No affiliation info available
Keevil BG
No affiliation info available

MeSH

Chromatography, High Pressure LiquidHumansPrednisoloneReproducibility of ResultsSensitivity and SpecificitySpectrometry, Mass, Electrospray Ionization

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

15829118

Citation

Owen, L J., et al. "Prednisolone Measurement in Human Serum Using Liquid Chromatography Tandem Mass Spectrometry." Annals of Clinical Biochemistry, vol. 42, no. Pt 2, 2005, pp. 105-11.
Owen LJ, Gillingwater S, Keevil BG. Prednisolone measurement in human serum using liquid chromatography tandem mass spectrometry. Ann Clin Biochem. 2005;42(Pt 2):105-11.
Owen, L. J., Gillingwater, S., & Keevil, B. G. (2005). Prednisolone measurement in human serum using liquid chromatography tandem mass spectrometry. Annals of Clinical Biochemistry, 42(Pt 2), 105-11.
Owen LJ, Gillingwater S, Keevil BG. Prednisolone Measurement in Human Serum Using Liquid Chromatography Tandem Mass Spectrometry. Ann Clin Biochem. 2005;42(Pt 2):105-11. PubMed PMID: 15829118.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Prednisolone measurement in human serum using liquid chromatography tandem mass spectrometry. AU - Owen,L J, AU - Gillingwater,S, AU - Keevil,B G, PY - 2005/4/15/pubmed PY - 2005/5/20/medline PY - 2005/4/15/entrez SP - 105 EP - 11 JF - Annals of clinical biochemistry JO - Ann Clin Biochem VL - 42 IS - Pt 2 N2 - Prednisolone is a commonly prescribed corticosteroid used in the treatment of many diseases. Despite high doses of prednisolone, some patients appear to have subtherapeutic concentrations of the drug. It would be useful to measure prednisolone in this group to determine if they have poor absorption or compliance. Hence, we have developed a liquid chromatography-tandem mass spectrometry method for the determination of prednisolone in serum. Chromatography was performed using a C18 column, giving a retention time for both prednisolone and deuterated prednisolone (internal standard) of 1.6 min. Two transitions were monitored for both prednisolone and deuterated prednisolone. These were m/z 361.2 > 343.0 and m/z 361.2 > 146.9 for prednisolone, and m/z 367.2 > 349.0 and m/z 367.2 > 149.9 for the internal standard. The intra- and inter-batch imprecision was < 7% in both cases over a concentration range of 62.5-750 microg/L. The imprecision at the lower limit was 8%, the lower limit of quantitation was determined to be 30 microg/L and the method was linear up to 5000 microg/L. The method allows rapid prednisolone analysis because of a simplified sample extraction step, and has a cycle time of 3.5 min. SN - 0004-5632 UR - https://www.unboundmedicine.com/medline/citation/15829118/Prednisolone_measurement_in_human_serum_using_liquid_chromatography_tandem_mass_spectrometry_ DB - PRIME DP - Unbound Medicine ER -