HIGH THROUGHPUT LC-MS/MSMETHOD FOR THE QUANTITATION OF LINAGLIPTIN IN HUMAN PLASMA BY SOLID PHASE EXTRACTION USING 96 WELL PLATE FORMATAbstract
High-throughput Liquid chromatography–mass spectrometry method has been developed and validated for the quantiﬁcation of Linagliptin in human plasma using Linagliptin D4 as an internal standard (ISTD). Following solid phase extraction (SPE) in 96 well plate format, the analyte and ISTD were run on phenyl hexyl, 100A 100 X 4.6mm, 2.6µusing an isocratic mobile phase consisting of 10mM Ammonium formate buffer (pH 6.5 ± 0.5): Methanol 15:85 v/v. The precursor and productions of the drugs were monitored on a triple quadrupole instrument operated in the positive ionization mode. The method was validated over a concentration range of 99.532-10045.049pg/mL with relative recoveries ranging from 69.9 to 77.1%. The inter batch precision (%CV) across three validation runs was≤ 2.9%.The Inter batch accuracy determined at four QC levels (LLOQ, LQC, MQC and HQC) was between 95.2–102.7%. According to the validated results, the proposed method was found to be specific, accurate, precise and high throughput method and could be used for the estimation of Linagliptin in human plasma and can be applied for the routine analysis.
Tangudu Nagabhusana Rao*, Guntuku Girija Sankar and Lade Jyothi Rani
Sr. Scientist II Nektar Therapeutics (India) Pvt Ltd. Sy Nos. 101/2, Genome Valley, Lalgadi Malakpet, Shameerpet Mandal, Hyderabad, R.R. District, Telangana - 500078, India
30 September, 2015
04 December, 2015
25 February, 2016
01 March, 2016