Quality by design approach in HPLC method development and validation for simultaneous determination of abiraterone acetate and prednisolone with greenness assessment
DOI:
https://doi.org/10.56782/pps.369Keywords:
Abiraterone acetate, Prednisolone, Quality by Design (QbD), High-Performance Liquid Chromatography (HPLC), GreennessAbstract
A
A Quality by Design (QbD) approach was employed to develop and optimize a novel and robust Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for the simultaneous estimation of abiraterone acetate (ABTA) and prednisolone (PDS) in the pharmaceutical dosage form. The optimized method parameters were determined using a Central Composite Design (CCD) and included a run time of 8 minutes, the flow rate of 0.8 mL//min, and a column temperature of 25°C. The mobile phase comprised methanol and acetonitrile (90:10v/v) with detection at 260 nm. Retention times of 5.23 minutes for ABTA and 3.335 minutes for PDS were achieved, ensuring efficient separation with high resolution and minimal tailing. Method validation confirmed precision, accuracy, linearity, robustness, and system suitability in compliance with ICH guidelines, establishing the method’s reliability for routine use. Green analytical chemistry assessment using GAPI, AGREE, HPLC-EAT, and BAGI tools highlighted the method’s environmental sustainability, practicality, and safety. The development of this method supports efficient quality control by providing a precise, eco-friendly analytical solution for simultaneous drug analysis. Additionally, its adaptability for future pharmaceutical applications makes it a valuable tool for enhancing process efficiency and meeting sustainability goals.
Downloads
References
1. Jena, B. R.; Panda, S. P.; Kulandaivelu, U.; Alavala, R. R.; Rao, G. S. N. K.; Swain, S.; Pattnaik, G.; Ghose, D. AQbD Driven Development of an RP-HPLC Method for the Quantitation of Abiraterone Acetate for Its Pharmaceutical Formulations in the Presence of Degradants. Turk. J. Pharm. Sci. 2021, 18 (6), 718–729. DOI: 10.4274/tjps.galenos.2021.74150
2. Bashar, T.; Apu, M. N. H.; Mostaid, M. S.; Islam, M. S.; Hasnat, A. Pharmacokinetics and Bioavailability Study of a Prednisolone Tablet as a Single Oral Dose in Bangladeshi Healthy Volunteers. Dose Response 2018, 16 (3), Art. No: 1559325818783932. DOI: 10.1177/1559325818783932
3. Attard, G.; Murphy, L.; Clarke, N. W.; Cross, W.; Jones, R. J.; Parker, C. C.; Gillessen, S.; Cook, A.; Brawley, C.; Amos, C. L.; Atako, N.; Pugh, C.; Buckner, M.; Chowdhury, S.; Malik, Z.; Russell, J. M.; Gilson, C.; Rush, H.; Bowen, J.; Lydon, A.; Pedley, I.; O’Sullivan, J. M.; Birtle, A.; Gale, J.; Srihari, N.; Thomas, C.; Tanguay, J.; Wagstaff, J.; Das, P.; Gray, E.; Alzoueb, M.; Parikh, O.; Robinson, A.; Syndikus, I.; Wylie, J.; Zarkar, A.; Thalmann, G.; de Bono, J. S.; Dearnaley, D. P.; Mason, M. D.; Gilbert, D.; Langley, R. E.; Millman, R.; Matheson, D.; Sydes, M. R.; Brown, L. C.; Parmar, M. K. B.; James, N. D.; Systemic Therapy in Advancing or Metastatic Prostate cancer: Evaluation of Drug Efficacy (STAMPEDE) investigators. Abiraterone Acetate and Prednisolone with or without Enzalutamide for High-Risk Non-Metastatic Prostate Cancer: A Meta-Analysis of Primary Results from Two Randomised Controlled Phase 3 Trials of the STAMPEDE Platform Protocol. Lancet 2022, 399(10323), 447–460. DOI: 10.1016/S0140-6736(21)02437-5
4. Chandra Reddy, B. J.; Sarada, N. C. Development and Validation of a Novel RP-HPLC Method for Stability-Indicating Assay of Abiraterone Acetate. J. Liq. Chromatogr. Relat. Technol. 2016, 39 (7), 354–363. DOI: 10.1080/10826076.2016.1163500
5. Beg, S.; Malik, A. K.; Afzal, O.; Altamimi, A. S. A.; Kazmi, I.; Al-Abbasi, F. A.; Almalki, W. H.; Barkat, M. A.; Kawish, S. M.; Pradhan, D. P.; Rahman, M. Systematic Development and Validation of a RP-HPLC Method for Estimation of Abiraterone Acetate and Its Degradation Products. J. Chromatogr. Sci. 2021, 59 (1), 79–87. DOI: 10.1093/chromsci/bmaa080
6. Sankar, P. R.; Eswarudu, M. M.; Siva, P.; Viswanath, A. Optimized and Validated RP-HPLC Method for Quantification of Abıraterone Acetate (an Antı-Prostate Cancer Drug) in Pharmaceutıcal Dosage Form. High Technol. Lett. 2021, 27 (7), 21-32.
7. Ashok, R.; Prakash, P. P.; Selvan, T. Development and Validation of Analytical Method for Estimation of Prednisolone in Bulk and Tablets Using UV-Visible Spectroscopy. Int. J. Pharm. Pharm. Sci. 2011, 3 (4), 184–186.
8. Optimization and Validation of Spectrophotometric Methods for the Determination of Prednisolone in Chitosan Nanoparticles. J. Hunan Univ. Nat. Sci. 2024, 51 (4), 83-91. DOI: 10.55463/issn.1674-2974.51.4.10.
9. Ghosh, S.; Kumar, D. S.; Sahu, A.; Banji, D.; Harani, A.; Chaitanya, C. K.; Kalapana, M. Development and Validation for Prednisolone in Tablet Dosage Form by Reverse Phase-HPLC. Asian J. Chem. 2011, 23 (11), 5092–5094.
10. Razzaq, S. N.; Khan, I. U.; Mariam, I.; Razzaq, S. S. Stability Indicating HPLC Method for the Simultaneous Determination of Moxifloxacin and Prednisolone in Pharmaceutical Formulations. Chem. Cent. J. 2012, 6 (1), Art. No: 94. DOI: 10.1186/1752-153X-6-94
11. S. Chitlange, S.; K. Chaturvedi, K.; B. Wankhede, S. Development and Validation of Spectrophotometric and HPLC Method for the Simultaneous Estimation of Salbutamol Sulphate and Prednisolone in Tablet Dosage Form. J. Anal. Bioanal. Tech. 2011, 2, Art. No: 19. DOI: 10.4172/2155-9872.1000117
12. Potnuri, N. R.; Rao, D. G.; Prasad, R. Y. A Novel Stability Indicating RP-HPLC Method for the Simultaneous Estimation of Moxifloxacin and Prednisolone in Bulk and Their Combined Dosage Form. Int. J. Pharm. Sci. Res. 2015, 6 (5), 1965-1973. DOI: 10.13040/IJPSR.0975-8232.6(5).1965-73
13. Solanki, T. D.; Patel, S. K.; Patel, B. K. Development and Validation of Stability Indicating Method for Simultaneous Estimation of Ofloxacin and Prednisolone in Pharmaceutical Dosage Form. Pharm. Biol. Eval. 2016, 3, 256–263.
14. Saad, F.; Efstathiou, E.; Attard, G.; Flaig, T. W.; Franke, F.; Goodman, O. B., Jr; Oudard, S.; Steuber, T.; Suzuki, H.; Wu, D.; Yeruva, K.; De Porre, P.; Brookman-May, S.; Li, S.; Li, J.; Thomas, S.; Bevans, K. B.; Mundle, S. D.; McCarthy, S. A.; Rathkopf, D. E.; ACIS Investigators. Apalutamide plus Abiraterone Acetate and Prednisone versus Placebo plus Abiraterone and Prednisone in Metastatic, Castration-Resistant Prostate Cancer (ACIS): A Randomised, Placebo-Controlled, Double-Blind, Multinational, Phase 3 Study. Lancet Oncol. 2021, 22 (11), 1541–1559. DOI: 10.1016/S1470-2045(21)00402-2
15. Dewani, A. P.; Vekariya, H. J. Optimization of High-Performance Liquid Chromatographic Method Using Central Composite Design for the Simultaneous Estimation of Ciprofloxacin and Loteprednol. J. Chromatogr. Sci. 2023, 61 (3), 279–287. DOI: 10.1093/chromsci/bmac016
16. Kumar, N.; D, S. Analytical Method Development by Using QbD - an Emerging Approach for Robust Analytical Method Development. J. Pharm. Sci. Res. 2020, 12(10), 1298–1305.
17. Holm, P.; Allesø, M.; Bryder, M. C.; Holm, R. Q8(R2): Pharmaceutical Development. In ICH Quality Guidelines; John Wiley & Sons, Inc.: Hoboken, NJ, USA, 2017; pp 535–577.
18. Shamim, A.; Ansari, M. J.; Aodah, A.; Iqbal, M.; Aqil, M.; Mirza, M. A.; Iqbal, Z.; Ali, A. QbD-Engineered Development and Validation of a RP-HPLC Method for Simultaneous Estimation of Rutin and Ciprofloxacin HCl in Bilosomal Nanoformulation. ACS Omega 2023, 8 (24), 21618–21627. DOI: 10.1021/acsomega.3c00956
19. Patel, K. Y.; Dedania, Z. R.; Dedania, R. R.; Patel, U. QbD Approach to HPLC Method Development and Validation of Ceftriaxone Sodium. Futur. J. Pharm. Sci. 2021, 7, Art. No: 141. DOI: 10.1186/s43094-021-00286-4
20. The Application of Quality by Design to Analytical Methods. Pharmaceutical Technology 2007, 31(10). https://www.pharmtech.com/view/application-quality-design-analytical-methods (Accessed on 24-11-2024).
21. Borman, P.; Elder, D. Q2(R1) Validation of Analytical Procedures: Text and Methodology. In ICH Quality Guidelines; John Wiley & Sons, Inc.: Hoboken, NJ, USA, 2017; pp 127–166.
22. Nakov, N.; Acevska, J.; Brezovska, K.; Kavrakovski, Z.; Dimitrovska, A.. Green Strategies toward Eco-Friendly HPLC Methods in Pharma Analysis. High Performance Liquid Chromatography - Recent Advances and Applications 2023. DOI: 10.5772/intechopen.110035
23. Płotka-Wasylka, J. A New Tool for the Evaluation of the Analytical Procedure: Green Analytical Procedure Index. Talanta 2018, 181, 204–209. DOI: 10.1016/j.talanta.2018.01.013
24. Manousi, N.; Wojnowski, W.; Płotka-Wasylka, J.; Samanidou, V. Blue Applicability Grade Index (BAGI) and Software: A New Tool for the Evaluation of Method Practicality. Green Chem. 2023, 25 (19), 7598 –7604. DOI: 10.1039/d3gc02347h.
25. Fares, M. Y.; Hegazy, M. A.; El-Sayed, G. M.; Abdelrahman, M. M.; Abdelwahab, N. S. Quality by Design Approach for Green HPLC Method Development for Simultaneous Analysis of Two Thalassemia Drugs in Biological Fluid with Pharmacokinetic Study. RSC Adv. 2022, 12 (22), 13896–13916. DOI: 10.1039/d2ra00966h
26. Imam, M. S.; Batubara, A. S.; Gamal, M.; Abdelazim, A. H.; Almrasy, A. A.; Ramzy, S. Adjusted Green HPLC Determination of Nirmatrelvir and Ritonavir in the New FDA Approved Co-Packaged Pharmaceutical Dosage Using Supported Computational Calculations. Sci. Rep. 2023, 13 (1), Art. No: 137. DOI: 10.1038/s41598-022-26944-y
27. Pena-Pereira, F.; Wojnowski, W.; Tobiszewski, M. AGREE-Analytical GREEnness Metric Approach and Software. Anal. Chem. 2020, 92 (14), 10076–10082. DOI: 10.1021/acs.analchem.0c01887
28. Wejnerowska, G.; Narloch, I. A. Comprehensive Assessment of Sample Preparation Methods for the Determination of UV Filters in Water by Gas Chromatography–Mass Spectrometry: Greenness, Blueness, and Whiteness Quantification Using the AGREEprep, BAGI, and RGB 12 Tools. Applied Sciences 2024, 14(17), 7690–7690. DOI: 10.3390/app14177690
Downloads
Published
Issue
Section
License
Copyright (c) 2025 Priya Jagtap, Dr. Reshma Jadhav, Dr. Ashish Jain, Bhavesh Mahajan, Prapti Gawand, Prathamesh Chaudhari, Aishwarya Patil
This work is licensed under a Creative Commons Attribution 4.0 International License.
For all articles published in Prospects in Pharmaceutical Sciences copyright is retained by the authors. The journal publishes articles in the Open Access policy, within the CC BY 4.0 licence.
This is a human-readable summary of (and not a substitute for) the license. Disclaimer.
You are free to:
Share — copy and redistribute the material in any medium or format
Adapt — remix, transform, and build upon the material for any purpose, even commercially.
The licensor cannot revoke these freedoms as long as you follow the license terms.
Under the following terms:
Attribution — You must give appropriate credit, provide a link to the license, and indicate if changes were made. You may do so in any reasonable manner, but not in any way that suggests the licensor endorses you or your use.
No additional restrictions — You may not apply legal terms or technological measures that legally restrict others from doing anything the license permits.
Notices:
You do not have to comply with the license for elements of the material in the public domain or where your use is permitted by an applicable exception or limitation.
No warranties are given. The license may not give you all of the permissions necessary for your intended use. For example, other rights such as publicity, privacy, or moral rights may limit how you use the material.
How to Cite
