Pooja Avula, Rajitha Galla, Geetha Susmita Adepu, Hari Babu Vemanaboina, Sivaranjani Tyagarajan
Pooja Avula1, Rajitha Galla1*, Geetha Susmita Adepu1, Hari Babu Vemanaboina2, Sivaranjani Tyagarajan2
1Institute of Pharmaceutical Technology, Sri Padmavati Mahila Visvavidyalayam (Women’s University), Tirupati.
2Analytical Development (AR&D), Orchid Health Care, IKKT, Chennai.
Volume - 14,
Issue - 2,
Year - 2021
A simple, precise, stable and economical RP-HPLC method was developed for estimation of Roflumilast in tablet dosage form and validated according to the ICH guidelines. The chromatographic separation was achieved on an Inertsil ODS-3V column of dimensions 150mm x 4.6mm, 5µm, using a mobile phase mixture of 0.01M ammonium acetate buffer and organic mixture (methanol: acetonitrile in 1:1 ratio) in the ratio of 25: 75 (v/v) at a flow rate of 1.5ml/min and UV detection at 250nm. The injection volume was maintained at 80µl with 6 min run time. Retention time (RT) was found to be 2.92±0.01min. This developed method was validated as per the ICH guidelines. Linear plot was obtained with a correlation coefficient of 0.999 in the concentration range of 5-40 µg/ml. The optimized method was accurate with 100.1% recovery and precise with %RSD - 0.1 respectively. The method was found to be specific with no interference of drug from the excipients. Stress studies or forced degradation studies were carried out at different conditions like thermal, acidic, basic, photolytic, peroxide, humidity and the results revealed that the method was stable and it can be used for routine analysis in tablet dosage formulations.
Cite this article:
Pooja Avula, Rajitha Galla, Geetha Susmita Adepu, Hari Babu Vemanaboina, Sivaranjani Tyagarajan. Development and Validation of Stability indicating RP-HPLC Method for Estimation of Roflumilast in Tablet dosage form. Research J. Pharm. and Tech. 2021; 14(2):863-868. doi: 10.5958/0974-360X.2021.00153.0
2. Indian Pharmacopoeia.2014; 7thed, vol-3: pp. 2682-2683.
3. Ladani JJ et al. Method Development and Validation of Roflumilast in Tablet Dosage Form by UV Spectrophotometry. Journal of Atoms and Molecules. 2012; 2(5): 369-374.
4. Raveendra BG et al. UV Spectrophotometric Method for Estimation of Roflumilast in Human Serum. Pharmaceutical Analytical Acta. 2016;7(6): 1-4.
5. Ravvendra Babu G, Durga Bhavani M and Revathi Krishna B. Method Development and Validation of Roflumilast in Spiked Human Plasma by using UV Spectroscopy. International Journal of Chemical Sciences. 2016; 14(3): 1263-1271.
6. Patel Paresh U and Patel Ushma B. Development and Validation of Spectrophotometric Method for Simultaneous Determination of Roflumilast and Salmeterol in Synthetic Mixture. International Journal of Pharmacy and Pharmaceutical Research. 2016; 5(2): 68-77.
7. Thappali SRS et al. Simultaneous Quantification of IC87114, Roflumilast and its Active Metabolite Roflumilast N-oxide in Plasma by LC-MS/MS: Application for a Pharmacokinetic Study. Journal of Mass Spectrometry. 2012;47: 1612-1619.
8. Knebel NG et al. Sensitive Quantification of Roflumilast and Roflumilast N-oxide in Human Plasma by LC-MS/MS employing Parallel Chromatography and Electro spray Ionization. Journal of Chromatography B. 2012; 82-91.
9. Xinge CUI et al. Simultaneous Determination of Roflumilast and its Metabolites in Human Plasma by LC-MS/MS: Application for a Pharmacokinetic Study. 2016; 1-30.
10. Patel Ushma B and Patel Paresh U. Development and Validation of High Performance Thin Layer Chromatographic Method for Simultaneous Estimation of Roflumilast and Salmeterol in Synthetic Mixture. World Journal of Pharmaceutical Research. 2016; 5(5): 1107-1117.
11. Barhate VD and Priya Deosthalee. Validation of Rapid Chromatographic Method for the Determination of Roflumilast. Journal of Chemistry and Pharmaceutical Research. 2011;3(2): 770-775.
12. Fang Tan. Development and Validation of Stability Indicating HPLC Method for Roflumilast and Related Substances. Advanced Materials Research Vols 781-784. 2013; 781-784: 68-71.
13. Belal TS et al. Validated Stability-Indicating HPLC-DAD Method for Determination of the Phosphodiesterase (PDE-4) Inhibitor Roflumilast. Bulletin of Faculty of Pharmacy, Cairo University. 2014; 52: 79-89.
14. Ladani JJ et al. Analytical Method Development and Validation of RP-HPLC for Estimation of Roflumilast in Bulk Drugs and Tablet Dosage Form. International Journal for Pharmaceutical Research Scholars. 2012; 1(3): 28-32.
15. Rambabu. Kuchi et al. A Novel RP-HPLC Method for Quantification of Roflumilast in Formulations. International Journal of Science and Technology. 2013;7(2): 388-394.
16. Arpit D. Shah and Dr. Chhaganbhai N. Patel. Implementation of QbD Approach to the RP- HPLC Method Development and Validation of Roflumilast in Bulk and Tablet Dosage Form: An Application in Degradation Study. World Journal of Pharmacy and Pharmaceutical sciences. 2014; 3 (6): 2281-2307.
17. Pinheiro MS et al. Development and Validation of an RP-HPLC Method for Roflumilast and its Degradation Products. Journal of Liquid Chromatography & Related Technologies. 2018; 1-9.
18. International Conference on Harmonization (ICH) Q2 (R1): Validation of Analytical Procedures: Test and Methodology, Geneva, Switzerland, 2005.
19. Validation of Analytical Procedures: Methodology (Q2B), ICH Harmonized Tripartite Guidelines, Geneva, 1996.
20. ICH Stability Testing of New Drug Substance and Products Q1A (R2), International Conference on Harmonization, 2003.
21. ICH guidelines for impurities in new drug substances Text and methodology Q3A (R2), International Conference on Harmonization, 2006.
22. Harshad V. Paithankar. HPLC Method Validation for Pharmaceuticals: A Review. International Journal of Universal Pharmacy and Biosciences. 2013; 228-240.
23. Narendra Reddy Y, Sreeramulu J and Balaswami B. A new stability indicating RP-HPLC-PDA method for Simultaneous Estimation of Glecaprevir and Pibrentasvir in tablet dosage form. Research Journal of Pharmacy and Technology. 2019; 12(2): 625-631.