• Gokul S. Sanap Sanjivani College of Pharmaceutical Education and Research, Kopargaon, Dist-Ahmednagar
  • Nilesh S. Zarekar Sanjivani College of Pharmaceutical Education and Research, Kopargaon, Dist-Ahmednagar
  • Sarita S. Pawar Sanjivani College of Pharmaceutical Education and Research, Kopargaon, Dist-Ahmednagar


Qualitative, Quantitative, Force degradation, Method development, Stability, ICH


High performance liquid chromatography is most accurate methods widely used for the qualitative and quantitative analysis of drug product. Analytical method development and validation play important roles in the Drug discovery, Drug development and Manufacture of pharmaceuticals. It involves detection of the purity and toxicity of a drug substance. A number of chromatographic parameters have been evaluated in order to optimize the methods in the analysis of method development in HPLC. An appropr- iate mobile phase, column, column tempe- rature, wavelength and gradient are develop- ped. Force degradation studies are helpful in development and validation of stability-indicating studies, determination of degrad- ation pathways of drug substances and drug products. Validation of an analytical procedure is to demonstrate that it is suitable for its intended purpose. The parameters described here are according to ICH guidelines and include accuracy, precision, specificity, limit of detection, limit of quantitation, linearity, range, ruggedness and robustness. The objective of this paper is to review the method development, optimize method parameters and validation of method for drug product from developm- ental stage of formulation to commercial batch of product.


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Skoog D. A. and West D. M., Fundamentals of Analytical Chemistry, 3rd Edn, 643-649(1995).

Columns from http://www.waters. com/watersdivision/pdf/Ic3AC.pdf.

Beckett A.H., Stenlake J.B., Practical Pharmaceutical chemistry, Univer- sity of London., Vol. I, 14th Edn. (1962).

Gurdeep R. Chatwal, Sham Anand, Instrumental Methods of Chemical Analysis, Himalaya publishing house Pvt Ltd., 185-190.

Kazakevich Y., Lobrutto R., HPLC for Pharmaceutical Scientists, John Wiley & Sons, New Jersey, (2007).

B.V. Rao, G.N. Sowjanya1, A. Ajitha, V.U.M. Rao, Review on stability indicating HPLC method develop-ment, World Journal of Pharmacy and Pharmaceutical Sciences.2015; 4(8): 405-423.

M. S. Charde, A. S. Welankiwar, J. Kumar, Method development by liquid chromatography with valida- tion, International Journal of Phar- mceutical Chemistry. 2014; 04(02): 57-61.

S. Sood, R. Bala, N.S. Gill, Method development and validation using HPLC technique – A review, Journal of Drug Discovery and Therapeutics. 2014; 2 (22):18-24.

Snyder L.R., Kirkland J.J and Glajch J. L., Practical HPLC Method Deve- lopment, 2nd Edn, John Wiley and Sons Inc. Canada.(1997).

Principles and Methods, Amesham Biosciences of Reversed Phase Chromatography, 6-8.

A report by Jay Breaux, Kevin Jones and Pierre Boulas, Analytical Method Development and Valida- tion, AAI Development Services, United States.

Bliesner D.M., Validating Chromato- graphic Methods, John Wliey & sons, Inc. 88-92, (2006).

Sethi PD, HPLC Quantitative Anal-ysis of Pharmaceutical Formulations. 1st Edn., New Delhi: CBS Publishers & Distributors (2001).

Breaux J, Jones K, Boulas P., Understanding and implementing efficient analytical methods develop- ment and validation. Pharm Technol Anal Chem Test. 2003; 5:6-13.

FDA Guidance for Industry, Analytical Procedures and Methods Validation (draft guidance), August 2000.

K. Huynh-Ba, Development of Stability indicating methods, Handbook of Stability Testing in Pharmaceutical Development, Sprin- ger. 2009; 153.

Christain GD, Analytical Chemistry, 6th Edn. USA: John Wiley & Sons Inc, (2001).

Columns from http://www.waters. com/watersdivision/pdf/Ic3AC.pdf.

Columns from

Columns from www.phenomenex. com.

B. Prathap, G.H.S. Rao, G. Devdass, A. Dey, N. Harikrishnan, Review on Stability Indicating HPLC Method Development, International Journal of Innovative Pharmaceutical Research. 2012; 3(3): 229-237.

M.W. Dong, Modern HPLC for prac- ticing scientists, John Wiley & Sons, New Jersey, (2006).

Separations Solutions: Mobile Phase pH, U.D. Neue, American Labora- tory, March 60.1, (1999).

How do I Develop an HPLC Method.

Vibha G et al., Development and validation of HPLC method a review. International Research Jour- nal of Pharmaceutical and Applied Sciences. 2012; 2(4):22-23.

N. Toomula, A. Kumar, S. D. Kumar, V.S. Bheemidi, Develop- ment and Validation of Analytical Methods for Pharmaceuticals, J. Anal. Bioanal. Techniques. 2011; 2(5): 1-4.

B. Nigovic, A. Mornar, M. Sertic, Chromatography-The Most Versatile Method of Chemical Analysis, Intech. 385-425 (2012).

K. Kardani, N. Gurav, B. Solanki, P. Patel, B. Patel, RP-HPLC Method Development and Validation of Gallic acid in Polyherbal Tablet Formulation, Journal of Applied Pharmaceutical Science. 2013; 3(5): 37-42.

International Conference on Harmonization, Draft Guidance on specifications, Test procedures and acceptance criteria for new drug substances and products, Chemical Substances. Fed. Regist. 2000; 3(5): 83041-63.

Putheti RR, Okigbo RN, Patil SC, Advanapu MS, Leburu R. Method development and validations, Characterization of critical elements in the development of pharma- ceuticals. Int J Health Res. 2008; 1:11-20.

Wood R. How to Validate Analytical Methods. Trends Analyt Chem. 2005; 54: 149-58.

Vessman J. Selectivity or specifi- city? Validation of analytical methods from the perspective of an analytical chemist in the pharmaceutical industry. J Pharm Biomed Analyt, 1996; 14:867-9.

Hearn Perkin Elmer RA., A Guide to Validation in HPLC Based on the Work of G. M. Holland.

Lindner W, Wainer IW, Require- ments for initial assay validation and publication in J Chromatltography B. J Chromatogr. 2006; 707: 1.2.

Validation of Compendial Proce- dures, United State Pharmacopeia, USP 36 NF, 27 (2) (2010).

Validation of Analytical Procedures: Text and Methodology, International Conferences on Harmonization, Draft Revised (2005), Q2 (R1).

Boulanger B, Chiap P, Dewe W, Crommen J, Hubert P. An analysis of the SFSTP guide on validation of chromatographic bioanalytical meth- ods: progress and limitations. J Pharm Biomed Anal. 2003; 32:753-65.


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How to Cite

Gokul S. Sanap, Nilesh S. Zarekar, and Sarita S. Pawar. “REVIEW ON METHOD DEVELOPMENT AND VALIDATION”. International Journal of Pharmaceutics and Drug Analysis, vol. 5, no. 5, May 2017, pp. 177-84,



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