Issue 10, 2023

Determination and quantification of related substances and degradation products in bictegravir by full factorial design evaluated HPLC and mass spectrometry

Abstract

Determining and quantifying novel impurities and degraded impurities of a drug product is always a continuous challenge to enhancing the drug quality for patients' safety. Herein, our work deals with (i) developing a rapid, accurate, and reliable high-performance liquid chromatographic validation method to quantify the bictegravir drug (integrase inhibitors of antiretroviral drugs) and its novel related impurities at low levels, and (ii) the liquid chromatography-mass spectrometry (LC-MS) method to identify degraded impurities. Separation of bictegravir acid (impurity-I) and methyl bictegravir (impurity-II) impurities which are identified by LC-MS in the bictegravir drug was executed by developing a method and the same method performance evaluated by using full factorial design. This developed analytical technique gave a well-separated peak of bictegravir and related analytes such as bictegravir acid (impurity-I) and methyl bictegravir (impurity-II), adequate with the peak properties as per USP guidelines. The method's sensitivity and linearity are demonstrated by its detection and quantification limits at low levels with a correlation coefficient of 0.998. The method's repeatability, specificity, and accuracy suggest that this developed technique is a reliable determination strategy for the bictegravir drug substance and its related impurities (impurity-I and impurity-II) in a simple, feasible, and affordable way.

Graphical abstract: Determination and quantification of related substances and degradation products in bictegravir by full factorial design evaluated HPLC and mass spectrometry

Supplementary files

Article information

Article type
Paper
Submitted
29 Dec. 2022
Accepted
13 Febr. 2023
First published
14 Febr. 2023

Anal. Methods, 2023,15, 1274-1285

Determination and quantification of related substances and degradation products in bictegravir by full factorial design evaluated HPLC and mass spectrometry

S. R. J. Kumar, V. K. Rao, N. K. Katari, N. S. Jyothi and L. P. Kowtharapu, Anal. Methods, 2023, 15, 1274 DOI: 10.1039/D2AY02106D

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