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. 2021 Sep 1;18(4):410-419.
doi: 10.4274/tjps.galenos.2020.70962.

Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Estimation of Bictegravir, Emtricitabine, and Tenofovir Alafenamide Fumarate

Tanuja Attaluri  1 , Ganapaty Seru  1 , Satya Narayana Murthy Varanasi  2
Affiliations

Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Estimation of Bictegravir, Emtricitabine, and Tenofovir Alafenamide Fumarate

Tanuja Attaluri et al. Turk J Pharm Sci. .

Abstract

Objectives: The focal intent of the current research work is to develop and validate a novel and reliable stability-indicating reverse-phase high performance liquid chromatographic method for the simultaneous estimation of a few anti-retrovirals, i.e., bictegravir, emtricitabine, and tenofovir alafenamide fumarate (AF).

Materials and methods: The novel method employs inertsil octyldecylsilyl C18 (4.6×250 mm, 5 mm) using 0.2% triethylamine buffer and methanol in a ratio of 40:60% (v/v) as the mobile phase to attain optimal elution. The detection wavelength was 260 nm with a 1.2 mL/min flow rate and a 20 μL injection volume.

Results: The linearity ranges for bictegravir, emtricitabine and tenofovir AF were 25-125 μg/mL, 100-500 μg/mL, and 12.5-62.5 μg/mL, respectively. The retention times for bictegravir, emtricitabine, and tenofovir AF were found to be 5.998 min, 2.805 min, and 4.537, min respectively. The percent recoveries of bictegravir, emtricitabine, and tenofovir AF were within the range of 98-102% w/w.

Conclusion: The novel method was successfully validated as per International Conference on Harmonization guidelines. In forced degradation studies, emtricitabine was found to be sensitive to thermal conditions; bictegravir and tenofovir AF, to oxidative conditions. The developed method is economical and reliable for routine analysis concerning all validated parameters.

Keywords: Bictegravir; RP-HPLC; emtricitabine; forced degradation studies; tenofovir AF; validation.

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Conflict of interest statement

Conflict of interest: No conflict of interest was declared by the authors. The authors are solely responsible for the content and writing of this paper.

Figures

Figure 1
Figure 1
Bictegravir
Figure 2
Figure 2
Emtricitabine
Figure 3
Figure 3
Tenofovir alafenamide fumarate
Figure 4
Figure 4
Optimized chromatogram showing the simultaneous elution of bictegravir, emtricitabine and tenofovir alafenamide fumarate
Figure 5
Figure 5
Assay chromatogram for marketed formulation of bictegravir, emtricitabine and tenofovir alafenamide fumarate
Figure 6
Figure 6
Linearity graph of emtricitabine
Figure 7
Figure 7
Linearity graph of tenofovir AF AF: Alafenamide
Figure 8
Figure 8
Linearity graph of bictegravir
Figure 9
Figure 9
Acidic degradation chromatogram of bictegravir, emtricitabine and tenofovir alafenamide fumarate AF: Alafenamide
Figure 10
Figure 10
Alkali degradation chromatogram of bictegravir, emtricitabine and tenofovir alafenamide fumarate
Figure 11
Figure 11
Thermal degradation chromatogram of bictegravir, emtricitabine and tenofovir alafenamide fumarate AF: Alafenamide
Figure 12
Figure 12
Oxidative degradation chromatogram of bictegravir, emtricitabine and tenofovir alafenamide fumarate AF: Alafenamide
Figure 13
Figure 13
Photolytic degradation chromatogram of bictegravir, emtricitabine & tenofovir alafenamide fumarate AF: Alafenamide
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