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Validation of on-line solid- phase extraction coupled with high-performance liquid chromatography–mass spectrometry assays for the determination of indacaterol, a potent β-adrenoceptor agonist in human serum

Emotte, Corinne and Deglave, Fanny and Picard, Franck and Chaturvedi, Animesh and Majumdar, Tapan and Agarwal, Ashish and Kretz, Olivier (2012) Validation of on-line solid- phase extraction coupled with high-performance liquid chromatography–mass spectrometry assays for the determination of indacaterol, a potent β-adrenoceptor agonist in human serum. Journal of chromatography B, 895/89. pp. 1-9. ISSN 1570-0232

Abstract

Adequate sample preparation is a key aspect of quantitative bioanalysis and can often be the cause of bottlenecks for the development of sensitive and high-throughput LC-MS/MS methods. Here, we have developed a highly sensitive method for the determination of indacaterol in human blood serum. Indacaterol is currently under development for the treatment of asthma and chronic obstructive pulmonary disease (COPD). The method involved was as follows: direct injection of the acidified serum into an on-line solid-phase extraction system with ion exchange MCX cartridge (Symbiosis™, Spark, Holland) followed by chromatography of indacaterol along with its stable isotope labeled internal standard on an analytical column, and analysis using LC–MS/MS (API 5000, Applied Biosystems, USA), in multiple reaction monitoring mode, with electron spray ionization. The results of assessments intended for validation viz., specificity, carry over, reproducibility of three days of validation, accuracy, precision, dilution effect, relative recovery and stability are presented. In addition, a second validation method with another cartridge (Hysphere C18 HD) was also studied. The methods were specific and selective for indacaterol in human serum and suitable for supporting clinical trials with indacaterol and allowed performing pharmacokinetic studies of indacaterol in humans.

Item Type: Article
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Additional Information: author can archive post-print (ie final draft post-refereeing); Publisher's version/PDF cannot be used
Keywords: Indacaterol, On-line SPE, LC-MS/MS and Validation.
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Date Deposited: 13 Oct 2015 13:15
Last Modified: 13 Oct 2015 13:15
URI: https://oak.novartis.com/id/eprint/5118

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