Method Development and Validation for the Estimation of Azelnidipine in Bulk Form and Marketed Pharmaceutical Dosage Form by Using Rp-HPLC
Corresponding Author(s) : Gade Sammaiah
bhargavsynpharma@gmail.com
International Journal of Allied Medical Sciences and Clinical Research,
Vol. 11 No. 2 (2023): 2023 Volume -11 - Issue 2
Abstract
The present work includes a simple, economic, rapid, accurate and precise isocratic RP-HPLC method development for estimation of Azelnidipine in bulk form and its marketed formulation. Estimation was done at 286nm which was found to be ?max of Azelnidipine. The simple, selective, isocratic RP-HPLC method for Azelnidipine was developed on Phenomenex Luna (C18) RP Column; 250 mm x 4.6 mm, 5µm with a mobile phase of Phosphate Buffer (pH-4.6) and Methanol were taken in the ratio of 65:35% v/v at a flow rate of 1.0 ml/min and detection wavelength 286nm. The developed method was validated successfully according to ICH Q2 (R1) guidelines. The chromatographic methods showed a good linear response with r2 values of 0.9995. The percentage relative standard deviation for method was found to be less than two, indicating that the methods were precise. The mean percentage recovery was for RP-HPLC method was 100.437%. From the results it could be concluded that both the developed method was specific, selective and robust. The method could be successfully applied for analysis of Bulk form and Marketed formulation of Azelnidipine.
Keywords
Azelnidipine, RP-HPLC, Method Development, Validation, ICH Guidelines.
1.
Yamuna Puchhakayala, Gade Sammaiah. Method Development and Validation for the Estimation of Azelnidipine in Bulk Form and Marketed Pharmaceutical Dosage Form by Using Rp-HPLC. Int. J. of Allied Med. Sci. and Clin. Res. [Internet]. 2023 May 29 [cited 2026 Apr. 15];11(2):181-9. Available from: https://ijamscr.com/ijamscr/article/view/1324
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References
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35. Gore MG, Pratap S. Dabhade, RP-HPLC method development and validation of azelnidipine, Gore and Dabhade, IJPSR. Vol. 7(12); 2016. p. 5111-4.
36. Prabhakar D, Sreekanth J, Jayaveera KN. Method development and validation of azelnidipine by RP-HPLC. Int J ChemTech Res. 2017;10(10):418-23.
37. Ubale S, Dr. Kalshetti MS, Habib B, Mittha J, Adlinge S. Development and validation of RP-HPLC method for quantification of azelnidipine in tablet. Int J Creat Res Thoughts (IJCRT). 2021;9 (7, July): 797-802.
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References
1. Available from: https://go.drugbank.com/drugs/DB09230.
2. Available from: https://pubchem.ncbi.nlm.nih.gov/compound/Azelnidipine.
3. Available from: https://en.wikipedia.org/wiki/Azelnidipine. Wikipedia.
4. Available from: https://medicaldialogues.in/generics/azelnidipine-2722518.
5. Skoog, Holler and Nieman, Chapter 28. Principles of instrumental analysis. 5th ed, Harcourt Publishes Int Company. p. 726-66.
6. Neue D, Wiley VC. HPLC columns. Theor Technol Pract Uwe. https://www.wiley.com/en-gl/HPLC+Columns:+Theory,+Technology,+and+Practice-p-9780471190370
7. Handbook of HPLC. Vol. 78, by Elena Katz et al. Marcel Dekker Inc. 1999. https://www.semanticscholar.org/paper/Handbook-of-HPLC-%E2%80%93-Chromatographic-Science-Series-Lloyd-Kennedy/5446ebc6108a8594de1657929583a2e785841b53
8. Ewing GW. Instrumental methods of chemical analysis. 5th ed. McGraw-Hill Book Company; 1988.
9. HPLC in pharmaceutical industry. Fong and long, Marcel Dekker Series. 1991. http://libraryopac.bits-hyderabad.ac.in/cgi-bin/koha/opac-detail.pl?biblionumber=15742
10. Instrumental Method of Chemical Analysis. Chatwal Anand, Himalaya Publishing House, p. no. 615-623.
11. Dr. Kealey, Haines PJ. Analytical chemistry. 1st ed. Bios Publisher; 2002. p. 1-7.
12. Practical pharmaceutical chemistry. 4th ed. part 2, by Beckett and Stenlake, CBS Publishers and Distributors, 2005; P.No.157-174. Available from: https://www.jpsr.pharmainfo.in/Documents/Volumes/vol11issue11/jpsr11111910.pdf
13. Govt of India, Ministry of Health and Family Welfare. Delhi: publication by controller of publication. Indian Pharmacopoeia. 2007;2:484-554.
14. British Pharmacopoeia. Published on the recommendation of the medicines commissions pursuant to Medicines Act 1968. international ed. Vol. 1; 1993. p. 429, 483.
15. United States Pharmacopoeia 29 NF;24, Published on the Recommendation of the Medicines Commissions Pursuant to Medicines, page no. 587.
16. Skoog, West, Holler, Crouch. Fundamentals of analytical chemistry. 8th ed. New Delhi: Cengage learning India Pvt ltd, Page no. 271-280; 2009 (Indian edition).
17. Kasture AV, Mahadik KR, Wadodkar SG, More HN. A textbook of pharmaceutical analysis, Instrumental methods. Nirali Prakashan. 9th ed, page no. 5-7;2:28-30.
18. Settle FA. Handbook of instrumental techniques for analytical chemistry. 1st ed. Singapore: Pearson Education Inc; 2004.
19. Willard HH, Dean AJ. Instrumental methods of analysis. CBS Publishers and distributors. 7th ed; 1986. p. 513-5.
20. Connors AK. In: Wiley A, editor. A text book of pharmaceutical analysis. 3rd ed. Interscience Publication; 2005. p. 373-400.
21. In AS. High pressure liquid chromatography of comprehensive analytical chemistry. Elsevier Publications; 2006.
22. Principles and methods. In: Amesham biosciences of reversed phase chromatography. 1999. p. 6-8. Available from: https://books.google.com/books/about/Reversed_Phase_Chromatography.html?id=4Q3eQgAACAAJ
23. Synder LR, Kirkland JJ, Glajch JL. Practical HPLC method development. 2nd ed. Canada: John Wiley & Sons Inc; 1997.
24. Mohammad T et al. HPLC method development and validation for pharmaceutical. Int Pharm Sci. 2012;2(3):14 Analysis-A [review].
25. Snyder LR, Kirkland JJ, Glajch JL. Practical HPLC method development. 2nd ed; 2001.
26. Vibha G et al. Development and validation of HPLC method – a review. Int Res J Pharm Appl Sci. 2012;2(4):22-3.
27. Bliesner DM. Validating chromatographic methods. John Wiley & sons Inc; 2006. p. 88-92.
28. Validation of analytical procedures: methodology. ICH-guidelines Q2B. Geneva. 1996, 11. (CPMP/ICH/281/95).
29. Gupta V et al. Development and validation of HPLC method – a review. Int Res J Pharm Appl Sci. 2012;2(4):17-25.
30. A review: HPLC method development and validation. Santosh Kumar Bhardwaj et al. International Journal of Analytical and Bioanalytical Chemistry, accepted 20 November 2015.
31. Method Development: A Guide to Basics Quantitative & Qualitative HPLC, LC, GC Chromacademy. Available from: https://www.waters.com/webassets/cms/support/docs/715003355_dev_meth.pdf
32. Sonawane LV. Bioanalytical method validation and its pharmaceutical application- A review pharmaceutica analytical. Acta. 2014;5:3 Center for Drug Evaluation and Research (CDER) Reviewer Guidance. https://www.researchgate.net/publication/269538705_Bioanalytical_Method_Validation_and_Its_Pharmaceutical_Application-_A_Review
33. ICH, Topic Q. 2 (R1) validation of analytical procedures: text and methodology. Available from: https://www.ema.europa.eu/en/documents/scientific-guideline/ich-q-2-r1-validation-analytical-procedures-text-methodology-step-5_en.pdf
34. Patil SD, Bachhav RS, Udavant PB, Ahirrao SP. Deepak S.bhambere4, Development and Validation of Stability Indicating RP-HPLC Method for Azelnidipine for bulk drug. Natl Volatiles Essent Oils. 2021;8(5):11151-7.
35. Gore MG, Pratap S. Dabhade, RP-HPLC method development and validation of azelnidipine, Gore and Dabhade, IJPSR. Vol. 7(12); 2016. p. 5111-4.
36. Prabhakar D, Sreekanth J, Jayaveera KN. Method development and validation of azelnidipine by RP-HPLC. Int J ChemTech Res. 2017;10(10):418-23.
37. Ubale S, Dr. Kalshetti MS, Habib B, Mittha J, Adlinge S. Development and validation of RP-HPLC method for quantification of azelnidipine in tablet. Int J Creat Res Thoughts (IJCRT). 2021;9 (7, July): 797-802.
38. Jadhav, Lokhande, Narwade, Mahananda V. Ghodke, Rutuja. S. Desai and Prerna R. Mote, Method development & validation of stability indicating Rp-HPLC method for simultaneous estimation for azelnidipine & telmisartan in bulk & pharmaceutical dosage form, world. J Pharm Med Res Wjpmr. 2022;8(3):216-22.
2. Available from: https://pubchem.ncbi.nlm.nih.gov/compound/Azelnidipine.
3. Available from: https://en.wikipedia.org/wiki/Azelnidipine. Wikipedia.
4. Available from: https://medicaldialogues.in/generics/azelnidipine-2722518.
5. Skoog, Holler and Nieman, Chapter 28. Principles of instrumental analysis. 5th ed, Harcourt Publishes Int Company. p. 726-66.
6. Neue D, Wiley VC. HPLC columns. Theor Technol Pract Uwe. https://www.wiley.com/en-gl/HPLC+Columns:+Theory,+Technology,+and+Practice-p-9780471190370
7. Handbook of HPLC. Vol. 78, by Elena Katz et al. Marcel Dekker Inc. 1999. https://www.semanticscholar.org/paper/Handbook-of-HPLC-%E2%80%93-Chromatographic-Science-Series-Lloyd-Kennedy/5446ebc6108a8594de1657929583a2e785841b53
8. Ewing GW. Instrumental methods of chemical analysis. 5th ed. McGraw-Hill Book Company; 1988.
9. HPLC in pharmaceutical industry. Fong and long, Marcel Dekker Series. 1991. http://libraryopac.bits-hyderabad.ac.in/cgi-bin/koha/opac-detail.pl?biblionumber=15742
10. Instrumental Method of Chemical Analysis. Chatwal Anand, Himalaya Publishing House, p. no. 615-623.
11. Dr. Kealey, Haines PJ. Analytical chemistry. 1st ed. Bios Publisher; 2002. p. 1-7.
12. Practical pharmaceutical chemistry. 4th ed. part 2, by Beckett and Stenlake, CBS Publishers and Distributors, 2005; P.No.157-174. Available from: https://www.jpsr.pharmainfo.in/Documents/Volumes/vol11issue11/jpsr11111910.pdf
13. Govt of India, Ministry of Health and Family Welfare. Delhi: publication by controller of publication. Indian Pharmacopoeia. 2007;2:484-554.
14. British Pharmacopoeia. Published on the recommendation of the medicines commissions pursuant to Medicines Act 1968. international ed. Vol. 1; 1993. p. 429, 483.
15. United States Pharmacopoeia 29 NF;24, Published on the Recommendation of the Medicines Commissions Pursuant to Medicines, page no. 587.
16. Skoog, West, Holler, Crouch. Fundamentals of analytical chemistry. 8th ed. New Delhi: Cengage learning India Pvt ltd, Page no. 271-280; 2009 (Indian edition).
17. Kasture AV, Mahadik KR, Wadodkar SG, More HN. A textbook of pharmaceutical analysis, Instrumental methods. Nirali Prakashan. 9th ed, page no. 5-7;2:28-30.
18. Settle FA. Handbook of instrumental techniques for analytical chemistry. 1st ed. Singapore: Pearson Education Inc; 2004.
19. Willard HH, Dean AJ. Instrumental methods of analysis. CBS Publishers and distributors. 7th ed; 1986. p. 513-5.
20. Connors AK. In: Wiley A, editor. A text book of pharmaceutical analysis. 3rd ed. Interscience Publication; 2005. p. 373-400.
21. In AS. High pressure liquid chromatography of comprehensive analytical chemistry. Elsevier Publications; 2006.
22. Principles and methods. In: Amesham biosciences of reversed phase chromatography. 1999. p. 6-8. Available from: https://books.google.com/books/about/Reversed_Phase_Chromatography.html?id=4Q3eQgAACAAJ
23. Synder LR, Kirkland JJ, Glajch JL. Practical HPLC method development. 2nd ed. Canada: John Wiley & Sons Inc; 1997.
24. Mohammad T et al. HPLC method development and validation for pharmaceutical. Int Pharm Sci. 2012;2(3):14 Analysis-A [review].
25. Snyder LR, Kirkland JJ, Glajch JL. Practical HPLC method development. 2nd ed; 2001.
26. Vibha G et al. Development and validation of HPLC method – a review. Int Res J Pharm Appl Sci. 2012;2(4):22-3.
27. Bliesner DM. Validating chromatographic methods. John Wiley & sons Inc; 2006. p. 88-92.
28. Validation of analytical procedures: methodology. ICH-guidelines Q2B. Geneva. 1996, 11. (CPMP/ICH/281/95).
29. Gupta V et al. Development and validation of HPLC method – a review. Int Res J Pharm Appl Sci. 2012;2(4):17-25.
30. A review: HPLC method development and validation. Santosh Kumar Bhardwaj et al. International Journal of Analytical and Bioanalytical Chemistry, accepted 20 November 2015.
31. Method Development: A Guide to Basics Quantitative & Qualitative HPLC, LC, GC Chromacademy. Available from: https://www.waters.com/webassets/cms/support/docs/715003355_dev_meth.pdf
32. Sonawane LV. Bioanalytical method validation and its pharmaceutical application- A review pharmaceutica analytical. Acta. 2014;5:3 Center for Drug Evaluation and Research (CDER) Reviewer Guidance. https://www.researchgate.net/publication/269538705_Bioanalytical_Method_Validation_and_Its_Pharmaceutical_Application-_A_Review
33. ICH, Topic Q. 2 (R1) validation of analytical procedures: text and methodology. Available from: https://www.ema.europa.eu/en/documents/scientific-guideline/ich-q-2-r1-validation-analytical-procedures-text-methodology-step-5_en.pdf
34. Patil SD, Bachhav RS, Udavant PB, Ahirrao SP. Deepak S.bhambere4, Development and Validation of Stability Indicating RP-HPLC Method for Azelnidipine for bulk drug. Natl Volatiles Essent Oils. 2021;8(5):11151-7.
35. Gore MG, Pratap S. Dabhade, RP-HPLC method development and validation of azelnidipine, Gore and Dabhade, IJPSR. Vol. 7(12); 2016. p. 5111-4.
36. Prabhakar D, Sreekanth J, Jayaveera KN. Method development and validation of azelnidipine by RP-HPLC. Int J ChemTech Res. 2017;10(10):418-23.
37. Ubale S, Dr. Kalshetti MS, Habib B, Mittha J, Adlinge S. Development and validation of RP-HPLC method for quantification of azelnidipine in tablet. Int J Creat Res Thoughts (IJCRT). 2021;9 (7, July): 797-802.
38. Jadhav, Lokhande, Narwade, Mahananda V. Ghodke, Rutuja. S. Desai and Prerna R. Mote, Method development & validation of stability indicating Rp-HPLC method for simultaneous estimation for azelnidipine & telmisartan in bulk & pharmaceutical dosage form, world. J Pharm Med Res Wjpmr. 2022;8(3):216-22.