BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF LINAGLIPTIN IN PLASMA THROUGH LCMS/ MS

Author(s): Mahamad Shafi SS, Arifa Begum* and Saradhi NDVR

Abstract

The objective of the study was to develop and validate simple, selective, specific Liquid Chromatography - Tandem Mass Spectrometry (LC-MS/MS) method for the determination of Linagliptin in Human Plasma. The accuracy and precision data must fulfill the requirements for the quantification of analytes in biological matrices to produce data for bioavailability, bioequivalence, etc. The separation of the analyte was carried out on Waters, X-Bridge, C18, 5μm column having 4.6×50 mm internal diameter and the mobile phase containing acetonitrile and 0.1 % formic acid (90:10 v/v) at a flow rate of 0.6 mL/min. The retention times of Linagliptin and Telmisartan (Internal Standard ) were 1.45 min and 1.20 min simultaneously and the total run time was 3.0 min. Monitoring of the fragmentation of m / z 473.54 → 157.6 performed during MS/MS detection of Linagliptin and Internal Standard (I.S.) on the mass spectrometer. The overall recovery of Linagliptin and IS was 92.5 % and 89.9 % respectively. The matrix effect of Linagliptin and IS was 5.51 and 1.33 % respectively. The method was validated over the concentration range of 10ng/mL to 5000ng/mL. Multiple Reaction Monitoring (MRM) mode was used as an operating mode in the mass spectrometer. Ion spray was kept in positive mode for the detection of Analyte and IS during the production of ions. The method was validated for linearity, accuracy, precision, specificity, selectivity, inter and intraday precision, LQC, HQC.

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