Sensitive and selective liquid chromatography–mass spectrometry method for the quantification of rosiglitazone in human plasma

• Published in: Journal of pharmaceutical and biomedical analysis Vol. 43; no. 2; pp. 580 - 585
• Main Authors: He, J., Hu, Y.F., Duan, L.F., Tan, Z.R., Wang, L.S., Wang, D., Zhang, W., Li, Z., Liu, J., Tu, J.H., Yao, Y.M., Zhou, Hong-Hao
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 17.01.2007; Elsevier Science
• Subjects: Administration, Oral; Adult; Analysis; Analytical, structural and metabolic biochemistry; Biological and medical sciences; Biological Availability; Chromatography, High Pressure Liquid - methods; Chromatography, High Pressure Liquid - standards; Drug Monitoring - methods; Fundamental and applied biological sciences. Psychology; General pharmacology; HPLC–ESI–MS–MS; Human plasma; Humans; Hypoglycemic Agents - administration & dosage; Hypoglycemic Agents - blood; Hypoglycemic Agents - pharmacokinetics; Male; Medical sciences; Pharmacology. Drug treatments; Reference Standards; Reference Values; Reproducibility of Results; Rosiglitazone; Sensitivity and Specificity; Spectrometry, Mass, Electrospray Ionization - methods; Spectrometry, Mass, Electrospray Ionization - standards; Tandem Mass Spectrometry - methods; Tandem Mass Spectrometry - standards; Thiazolidinediones - administration & dosage; Thiazolidinediones - blood; Thiazolidinediones - pharmacokinetics; HPLC–ESI–MS–MS; Rosiglitazone; Human plasma; Human; Biological fluid; Hypoglycemic agent; HPLC-ESI-MS-MS; Thiazolidinedione derivatives; Electrospray; Quantitative analysis; Blood plasma
• ISSN: 0731-7085; 1873-264X
• DOI: 10.1016/j.jpba.2006.07.010

A sensitive and selective high-performance liquid chromatography–electrospray ionisation–tandem mass spectrometry (HPLC–ESI–MS–MS) method for determination of rosiglitazone in human plasma has been developed. After the addition of the internal standard, plasma samples were precipited by acetonitrile. The compounds were separated on a proC18 column using a mixture of ammonium acetate buffer (0.02 M, pH 6.5) and acetonitrile (in the ratio of 47:53, v/v) as mobile phase. A Finnigan LCQdeca plus ion trap mass spectrometer connected to a Finnigan Surveyor HPLC was used to develop and validate the method. Linearity was established for the range of concentrations 1–1000 ng/ml with a coefficient of determination ( r 2) of 0.999. The intra-day accuracy for rosiglitazone ranged from 110.0 to 99.2% at low, medium and high levels. The inter-day accuracy was less than 15%. The lower limit of quantitation (LLOQ) was identified reproducible at 1.0 ng/ml with a precision of 5.7%. After validation, the method was used to study the pharmacokinetic profile of rosiglitazone in five healthy volunteers after administration of a single oral dose (4.0 mg). The proposed method enabled the unambiguous evaluation and quantitation of rosiglitazone for pharmacokinetic, bioavailability or drug–drug interaction studies. A possible chromatography peak ( m/ z 121, its parent ion m/ z 344) of N-demethyl rosiglitazone was observed at 3.49 min during determining rosiglitazone. This may be also a potential method for simultaneous determination of rosiglitazone and its metabolite N-demethyl rosiglitazone concentrations in plasma.