Abstract

ANALYTICAL METHOD DEVELOPMENT, VALIDATION AND FORCE DEGRADATION STUDY FOR ESTIMATION OF AZELNIDIPINE USING LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

Unnati Naik*, Komal Sutaria and Bhavdip Hirapara

Abstract

A novel simple, rapid, sensitive and stability indicating LC-MS/MS method was developed and validated for the determination and identification of a degradation product for Azelnidipine. Shimadzu LC- 20 AT equipped with a mass spectrometer ABScix API 200 was used for LC-MS/MS. The chromatographic analysis was carried out using Agilent, Zorbax, C18 (150mm x 4.6mm, 5μm) column, using a 20:80 mixture of 10mM ammonium formate buffer in water having pH 4.0 and acetonitrile as a mobile phase. The flow rate was kept at 1 mL/min with a run time of 10 minutes and the sample injection volume was 20 μL. MRM scans for m/z products 583.400 (daughter ion 496.200) have been performed for Azelnidipine. A force degradation study has been performed using LC-MS for Azelnidipine at different stress levels (acidic, alkaline, oxidative, photolytic and thermal). Azelnidipine was unstable in acidic, basic as well as oxidation conditions, whereas it was stable in thermal and photo-degradation conditions. Validation parameters such as linearity, range, LOD and LOQ, accuracy, precision and robustness were evaluated as per ICH guidelines. The proposed LC-MS/MS method and its validation according to the ICH guidelines show that the developed method is sensitive, precise, accurate and simple for the determination of Azelnidipine.

Keywords: Azelnidipine, Force degradation, Liquid Chromatography-Mass Spectrometry, Method development, Method validation.