Heptad green metrics and quality by design tool evaluated chromatography method for content determination of Bexagliflozin in formulation product

The study created an eco-friendly, rapid, sensitive, cost-efficient, stability-assessing method for analyzing Bexagliflozin in pharmaceuticals using a RP-UPLC approach. The method's specificity was achieved using an XBridge analytical column (100 mm x 2.1 mm, 3.5 µm) with a mobile phase consist...

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Main Authors: Satyajit Raj Nethekar, Phani Raja Kanuparthy, Leela Prasad Kowtharapu, Vishnuvardhana Kishore Polisetti, Pankaj Kumar Lahoti, Sreekantha B Jonnalagadda, Naresh Kumar Katari
Format: Article
Language:English
Published: Elsevier 2025-06-01
Series:Green Analytical Chemistry
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Online Access:http://www.sciencedirect.com/science/article/pii/S277257742500076X
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author Satyajit Raj Nethekar
Phani Raja Kanuparthy
Leela Prasad Kowtharapu
Vishnuvardhana Kishore Polisetti
Pankaj Kumar Lahoti
Sreekantha B Jonnalagadda
Naresh Kumar Katari
author_facet Satyajit Raj Nethekar
Phani Raja Kanuparthy
Leela Prasad Kowtharapu
Vishnuvardhana Kishore Polisetti
Pankaj Kumar Lahoti
Sreekantha B Jonnalagadda
Naresh Kumar Katari
author_sort Satyajit Raj Nethekar
collection DOAJ
description The study created an eco-friendly, rapid, sensitive, cost-efficient, stability-assessing method for analyzing Bexagliflozin in pharmaceuticals using a RP-UPLC approach. The method's specificity was achieved using an XBridge analytical column (100 mm x 2.1 mm, 3.5 µm) with a mobile phase consisting of 10 mM Ammonium acetate and Methanol in a ratio of 55:45 (v/v). The flow rate is 0.2 mL/min, the injection volume is 1 µL, and the UV detection wavelength is 220 nm. The total run time is 2.5 minutes. The technique was meticulously validated, strictly adhering to the ICH criteria, and demonstrated specificity, linearity, ruggedness, robustness, and accuracy. The technique robustness analysis was carried out by using the QbD tool to build DoE's and assess their robustness. The methodology exhibited a linear trend as the concentration level increased from 5µg/mL to 30ug/mL. The recovery process ranged from 50% to 150%, with the average recovery considered adequate. Method stability indicating nature proved by forced degradation study. Analytical Eco-scale value found 81. NEMI showing the three quadrants showing the green, Modified NEMI has only one red quadrant. GAPI have five green, 5 yellow and 5 red parts. Complex GAPI have 12 green, 7 yellow and 6 red parts in the whole pictogram. AGREE shown the quantitative value 0.64 and pictogram shown 7 green parts, three yellow parts and 2 red parts. Green metric tools NEMI, modified NEMI, GAPI, complex GAPI Eco-scale, AGREE, and AGREEprep are used to express the method's greenness.
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spelling doaj-art-603ba86128564c30a3c25a469f948d432025-08-20T03:22:23ZengElsevierGreen Analytical Chemistry2772-57742025-06-011310028010.1016/j.greeac.2025.100280Heptad green metrics and quality by design tool evaluated chromatography method for content determination of Bexagliflozin in formulation productSatyajit Raj Nethekar0Phani Raja Kanuparthy1Leela Prasad Kowtharapu2Vishnuvardhana Kishore Polisetti3Pankaj Kumar Lahoti4Sreekantha B Jonnalagadda5Naresh Kumar Katari6Department of Chemistry, GITAM School of Science, GITAM Deemed to be University, Hyderabad, Telangana 502329, IndiaDepartment of Chemistry, GITAM School of Science, GITAM Deemed to be University, Hyderabad, Telangana 502329, India; Corresponding authors.Department of Chemistry, GITAM School of Science, GITAM Deemed to be University, Hyderabad, Telangana 502329, IndiaResearch and Development, Appco Pharma IIc, 262 Old Newbrunswick Rd, Piscataway, New Jersey 08873, USAQuality Operations, Deloitte LLC, 5231, Giardino Dr, Mount Juliet, TN 37122, United StatesSchool of Chemistry & Physics, College of Agriculture, Engineering & Science, Westville Campus, University of KwaZulu-Natal, P Bag X 54001, Durban 4000, South AfricaSchool of Chemistry & Physics, College of Agriculture, Engineering & Science, Westville Campus, University of KwaZulu-Natal, P Bag X 54001, Durban 4000, South Africa; R&D, CHEMTEX Environmental Laboratories Inc., Port Arthur, Texas 77642, United States; Corresponding authors.The study created an eco-friendly, rapid, sensitive, cost-efficient, stability-assessing method for analyzing Bexagliflozin in pharmaceuticals using a RP-UPLC approach. The method's specificity was achieved using an XBridge analytical column (100 mm x 2.1 mm, 3.5 µm) with a mobile phase consisting of 10 mM Ammonium acetate and Methanol in a ratio of 55:45 (v/v). The flow rate is 0.2 mL/min, the injection volume is 1 µL, and the UV detection wavelength is 220 nm. The total run time is 2.5 minutes. The technique was meticulously validated, strictly adhering to the ICH criteria, and demonstrated specificity, linearity, ruggedness, robustness, and accuracy. The technique robustness analysis was carried out by using the QbD tool to build DoE's and assess their robustness. The methodology exhibited a linear trend as the concentration level increased from 5µg/mL to 30ug/mL. The recovery process ranged from 50% to 150%, with the average recovery considered adequate. Method stability indicating nature proved by forced degradation study. Analytical Eco-scale value found 81. NEMI showing the three quadrants showing the green, Modified NEMI has only one red quadrant. GAPI have five green, 5 yellow and 5 red parts. Complex GAPI have 12 green, 7 yellow and 6 red parts in the whole pictogram. AGREE shown the quantitative value 0.64 and pictogram shown 7 green parts, three yellow parts and 2 red parts. Green metric tools NEMI, modified NEMI, GAPI, complex GAPI Eco-scale, AGREE, and AGREEprep are used to express the method's greenness.http://www.sciencedirect.com/science/article/pii/S277257742500076XBexagliflozinGreen chemistryGreen metricsQuality by designUPLC
spellingShingle Satyajit Raj Nethekar
Phani Raja Kanuparthy
Leela Prasad Kowtharapu
Vishnuvardhana Kishore Polisetti
Pankaj Kumar Lahoti
Sreekantha B Jonnalagadda
Naresh Kumar Katari
Heptad green metrics and quality by design tool evaluated chromatography method for content determination of Bexagliflozin in formulation product
Green Analytical Chemistry
Bexagliflozin
Green chemistry
Green metrics
Quality by design
UPLC
title Heptad green metrics and quality by design tool evaluated chromatography method for content determination of Bexagliflozin in formulation product
title_full Heptad green metrics and quality by design tool evaluated chromatography method for content determination of Bexagliflozin in formulation product
title_fullStr Heptad green metrics and quality by design tool evaluated chromatography method for content determination of Bexagliflozin in formulation product
title_full_unstemmed Heptad green metrics and quality by design tool evaluated chromatography method for content determination of Bexagliflozin in formulation product
title_short Heptad green metrics and quality by design tool evaluated chromatography method for content determination of Bexagliflozin in formulation product
title_sort heptad green metrics and quality by design tool evaluated chromatography method for content determination of bexagliflozin in formulation product
topic Bexagliflozin
Green chemistry
Green metrics
Quality by design
UPLC
url http://www.sciencedirect.com/science/article/pii/S277257742500076X
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