<abstract xmlns="http://www.w3.org/1999/xhtml">

A UPLC-MS method for the estimation of atazanavir sulfate was developed using the “analytical quality by design” approach. The critical chromatographic quality attributes identified were retention time, theoretical plates and peak tailing. The critical method parameters established were percent of organic modifier, flow rate and injection volume. Optimization performed using Box-Behnken Design (BBD) established 10 % organic modifier, 0.4 mL min−1 flow rate and 6-µL injection volume as the optimum method conditions. Atazanavir sulfate eluted at 5.19 min without any interference. Method validation followed international guidelines. The method has proven linearity in the range of 10–90 µg mL−1. Recovery was between 100.2–101.0 % and precision within the accepted limits (RSD 0.2–0.7 %). <italic>LOD</italic> and <italic>LOQ</italic> were 2.68 and 8.14 µg mL−1, resp. Stress testing stability studies showed atazanavir sulfate to degrade under acidic and basic conditions. The suggested technique is simple, rapid and sustainable. It is, therefore, suggested for routine analysis of atazanavir sulfate.
</abstract>

A UPLC-MS method for the estimation of atazanavir sulfate was developed using the “analytical quality by design” approach. The critical chromatographic quality attributes identified were retention time, theoretical plates and peak tailing. The critical method parameters established were percent of organic modifier, flow rate and injection volume. Optimization performed using Box-Behnken Design (BBD) established 10 % organic modifier, 0.4 mL min−1 flow rate and 6-µL injection volume as the optimum method conditions. Atazanavir sulfate eluted at 5.19 min without any interference. Method validation followed international guidelines. The method has proven linearity in the range of 10–90 µg mL−1. Recovery was between 100.2–101.0 % and precision within the accepted limits (RSD 0.2–0.7 %). LOD and LOQ were 2.68 and 8.14 µg mL−1, resp. Stress testing stability studies showed atazanavir sulfate to degrade under acidic and basic conditions. The suggested technique is simple, rapid and sustainable. It is, therefore, suggested for routine analysis of atazanavir sulfate.

Development and validation of a UPLC-MS method for determination of atazanavir sulfate by the “analytical quality by design” approach

Acta Pharmaceutica

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

A UPLC-MS method for the estimation of atazanavir sulfate was developed using the “analytical quality by design” approach. The critical chromatographic quality...

Development and validation of a UPLC-MS method for determination of atazanavir sulfate by the “analytical quality by design” approach

Publié en ligne: 01 nov. 2019

Pages: 17 - 33

Accepté: 20 mars 2019

DOI: https://doi.org/10.2478/acph-2020-0008

Mots clés
atazanavir sulfate, UPLC-MS, “analytical quality by design”

© 2020 Chandni Saha et al., published by Sciendo

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Development and validation of a UPLC-MS method for determination of atazanavir sulfate by the “analytical quality by design” approach

Publié en ligne: 01 nov. 2019

Pages: 17 - 33

Accepté: 20 mars 2019

DOI: https://doi.org/10.2478/acph-2020-0008

Mots clésatazanavir sulfate, UPLC-MS, “analytical quality by design”

© 2020 Chandni Saha et al., published by Sciendo

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Mots clés
atazanavir sulfate, UPLC-MS, “analytical quality by design”