VALIDATED LC-MS/MS METHOD FOR THE CONCOMITANT DETERMINATION OF AMOXICILLIN AND CLAVULANIC ACID FROM HUMAN PLASMA

József  BALÁZSI; Csaba  PAIZS; Florin-Dan  IRIMIE; Monica Ioana  TOŞA; László Csaba  BENCZE; Róbert  TŐTŐS

doi:10.24193/subbchem.2017.2.12

VALIDATED LC-MS/MS METHOD FOR THE CONCOMITANT DETERMINATION OF AMOXICILLIN AND CLAVULANIC ACID FROM HUMAN PLASMA

Authors

József BALÁZSI PharmacoKinetics SRL, Corunca, Mures county, Romania. Corresponding author: robert.totos@ubbcluj.ro.
Csaba PAIZS Faculty of Chemistry and Chemical Engineering, Hungarian Line of Study, Babes-Bolyai University, Cluj Napoca, Romania. Email: csaba.paizs@ubbcluj.ro. https://orcid.org/0000-0002-7403-7098
Florin-Dan IRIMIE Biocatalysis and Biotransformations Research Center, Babeş-Bolyai University, Faculty of Chemistry and Chemical Engineering, Cluj-Napoca, Romania. Email: irimie@chem.ubbcluj.ro. https://orcid.org/0000-0003-2093-0136
Monica Ioana TOŞA Department of Biochemistry and Biochemical Engineering, Faculty of Chemistry and Chemical Engineering , Babes-Bolyai University, Cluj Napoca, Romania. Email: monica.tosa@ubbcluj.ro. https://orcid.org/0000-0003-3240-706X
László Csaba BENCZE Biocatalysis and Biotransformations Research Center, Babeş-Bolyai University, Faculty of Chemistry and Chemical Engineering, Cluj-Napoca, Romania. Email: cslbencze@chem.ubbcluj.ro. https://orcid.org/0000-0003-0956-9749
Róbert TŐTŐS Biocatalysis and Biotransformations Research Group, Faculty of Chemistry and Chemical Engineering, Babeş-Bolyai University, Cluj-Napoca, Romania. Email: robert.totos@ubbcluj.ro. https://orcid.org/0000-0003-1743-3905

DOI:

https://doi.org/10.24193/subbchem.2017.2.12

Keywords:

amoxicillin, clavulanic acid, method validation, bioequivalence trial, LC-MS/MS

Abstract

The purpose of this study was the development and validation of an LC-MS/MS method, for the concomitant and rapid determination amoxicillin and clavulanic acid from human plasma. The sample workup involved a simple protein precipitation procedure. A core/shell type analytical column (50×2,1 mm, 2.6 Å) was used with PFP stationary phase. A mobile phase with high aqueous composition provided satisfactory separation with good accuracy and precision (stable ionization). The mass spectrometer was operated in positive electrospray ionization mode for both analytes and internal standard. The following parameters were evaluated for validation purpose: selectivity, sensitivity, matrix effect, anticoagulant effect, linearity, precision and accuracy, recovery, analyte/IS stability in solvent/matrix and carryover. The validated calibration range was 190-22222 ng/ml for amoxicillin, and 147-4908 ng/ml for clavulanic acid. The correlation coefficient R² was at least 0.99 for both analytes. The validated method has been successfully used for the evaluation bioequivalence of generic amoxicillin/potassium clavulanate formulations.

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STUDIA UBB CHEMIA, Volume 62 (LXII), No. 2, Tome I, June 2017

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Published

2017-06-01

How to Cite

BALÁZSI, J. ., PAIZS, C. ., IRIMIE, F.-D. ., TOŞA, M. I. ., BENCZE, L. C. ., & TŐTŐS, R. . (2017). VALIDATED LC-MS/MS METHOD FOR THE CONCOMITANT DETERMINATION OF AMOXICILLIN AND CLAVULANIC ACID FROM HUMAN PLASMA. Studia Universitatis Babeș-Bolyai Chemia, 62(2), 167–178. https://doi.org/10.24193/subbchem.2017.2.12