AQbD-driven development and validation of a robust UPLC method for lenacapavir in bulk and pharmaceutical dosage form

Lenacapavir, a novel long-acting human immunodeficiency virus (HIV) capsid inhibitor, represents a significant advancement in HIV therapy and prevention, creating a growing need for robust analytical methods to support quality control and regulatory requirements. Nevertheless, the reported methods are limited and lack systematic risk assessment, method understanding, and sustainability-oriented development. To address these gaps and ensure enhanced method robustness and reliability, an analytical quality by design (AQbD)-driven ultra-performance liquid chromatography (UPLC) method was developed for the quantification of lenacapavir. Method: An AQbD-driven strategy involving selection of Critical Operational Parameters (COPs) and Critical Analytical Attributes (CAAs), risk assessment, Plackett–Burman screening, and Central Composite Design (CCD)-based optimization was employed. Statistical evaluation was performed using ANOVA. Chromatographic separation was achieved on a phenomenex octadecylsilane stationary phase packed with 1.7 µm particles and dimensions of 50 × 2.1 mm, using ethanol and water (23.59:76.41, v/v) as the mobile phase at a solvent delivery rate of 0.56 mL/min with ultraviolet (UV) detection at 229 nm. Lenacapavir was eluted at 0.816 min within a total run time of 3 min. The method exhibited excellent linearity over 37.50–225.00 µg/mL (R2 = 0.9999), with a mean recovery of 100.1% and %RSD of 0.61. Validation was performed according to International conference of Harmonization (ICH) Q2(R1) guidelines, and stability-indicating capability was confirmed through forced degradation studies in accordance with ICH Q1A(R2) and Q1B. Environmental sustainability and analytical performance assessment using AGSA-Prep, CACI, and MA-tool metrics demonstrated the eco-friendly and efficient nature of the developed method. This study presents the first AQbD-driven green UPLC method for lenacapavir analysis. The developed method is rapid, robust, stability-indicating, and environmentally sustainable, making it suitable for routine quality control, stability studies, and regulatory applications in the pharmaceutical industry.

Authors

Publication Details

Journal
Analytical Chemistry Letters
Published
2026-10-13
DOI
https://doi.org/10.1080/22297928.2026.2730206
Primary Topic
Analytical Methods in Pharmaceuticals
Type
article
Field-Weighted Citation Impact
0.00
Controls
|||
ALL TIME
JAN
FEB
MAR
APR
MAY
JUN
JUL
AUG
SEP
OCT
article

AQbD-driven development and validation of a robust UPLC method for lenacapavir in bulk and pharmaceutical dosage form

Sandhya Madhuri Maddala, Vainda Shivani, T. Jayakrishna
Analytical Chemistry Letters
Analytical Methods in Pharmaceuticals
article

AQbD-driven development and validation of a robust UPLC method for lenacapavir in bulk and pharmaceutical dosage form

Sandhya Madhuri Maddala, Vainda Shivani, T. Jayakrishna
article en

Abstract

Lenacapavir, a novel long-acting human immunodeficiency virus (HIV) capsid inhibitor, represents a significant advancement in HIV therapy and prevention, creating a growing need for robust analytical methods to support quality control and regulatory requirements. Nevertheless, the reported methods are limited and lack systematic risk assessment, method understanding, and sustainability-oriented development. To address these gaps and ensure enhanced method robustness and reliability, an analytical quality by design (AQbD)-driven ultra-performance liquid chromatography (UPLC) method was developed for the quantification of lenacapavir. Method: An AQbD-driven strategy involving selection of Critical Operational Parameters (COPs) and Critical Analytical Attributes (CAAs), risk assessment, Plackett–Burman screening, and Central Composite Design (CCD)-based optimization was employed. Statistical evaluation was performed using ANOVA. Chromatographic separation was achieved on a phenomenex octadecylsilane stationary phase packed with 1.7 µm particles and dimensions of 50 × 2.1 mm, using ethanol and water (23.59:76.41, v/v) as the mobile phase at a solvent delivery rate of 0.56 mL/min with ultraviolet (UV) detection at 229 nm. Lenacapavir was eluted at 0.816 min within a total run time of 3 min. The method exhibited excellent linearity over 37.50–225.00 µg/mL (R2 = 0.9999), with a mean recovery of 100.1% and %RSD of 0.61. Validation was performed according to International conference of Harmonization (ICH) Q2(R1) guidelines, and stability-indicating capability was confirmed through forced degradation studies in accordance with ICH Q1A(R2) and Q1B. Environmental sustainability and analytical performance assessment using AGSA-Prep, CACI, and MA-tool metrics demonstrated the eco-friendly and efficient nature of the developed method. This study presents the first AQbD-driven green UPLC method for lenacapavir analysis. The developed method is rapid, robust, stability-indicating, and environmentally sustainable, making it suitable for routine quality control, stability studies, and regulatory applications in the pharmaceutical industry.

Analytical Chemistry Letters
Openalex Percentile: Top 19%
Analytical Methods in Pharmaceuticals
AI Navigator

Ask Laika to Summarize, Analyze, and Connect papers live on the map.

Summarize Papers & Methodologies

Extract key findings, datasets, and comparative methods across publications.

Benchmark Rankings & Visual Analytics

Rank top research institutions, authors, funders, topics, and journals by Field-Weighted Citation Impact (FWCI) and paper volume with instant charts.

Connect Distant Disciplines

Bridge topological clusters on the map to find hidden collaborative intersections.