ISSN print edition: 0366-6352 ISSN electronic edition: 1336-9075 Registr. No.: MK SR 9/7 Published monthly

Analysis of valsartan, clindamycin and mesalamine in human plasma by LC–MS/MS using different extraction methodologies to overcome matrix effect

Vikas Trivedi, Priyanka A. Shah, Pranav S. Shrivastav, and Mallika Sanyal

Kadi Sarva Viswavidyalaya, Ghandhinagar, India

E-mail: pranav_shrivastav@yahoo.com

Received: 14 November 2019  Accepted: 9 April 2020

Abstract:

Interference of endogenous components present in biological fluids has a profound effect on the performance of LC–MS/MS-based assays. The present work evaluates the effect of plasma matrix components during sample preparation for accurate and precise determination of valsartan, clindamycin and mesalamine by LC–ESI–MS/MS. The methods were thoroughly assessed using different approaches for sample preparation such as solid-phase extraction (SPE) with different cartridges for valsartan, conventional protein precipitation and Phree phospholipid removal cartridge for clindamycin and liquid–liquid extraction (LLE) with and without derivatization for mesalamine to minimize matrix interference. The extent of matrix effect was determined by post-column analyte infusion, post-extraction spike method and by calculation of slope of calibration lines for different plasma sources. The influence of matrix ion suppression/enhancement on the extraction recovery and sensitivity of the methods was identified and quantified. The mean recovery obtained was 96.8% for valsartan using SPE on Oasis MCX, 92.2% for clindamycin using Phree phospholipid cartridge and 96.5% for mesalamine using LLE following derivatization. The intra-batch and inter-day precision (% CV) was ˂4.0 for the methods and was validated as per the current regulatory guidance.

Keywords: Valsartan; Clindamycin; Mesalamine; Sample preparation; Matrix effect; LC–ESI–MS/MS

Full paper is available at www.springerlink.com.

DOI: 10.1007/s11696-020-01160-y

Chemical Papers 74 (12) 4365–4378 (2020)