Quality by Design (Qbd) Approach to Develop HPLC Method for Estimation of Gliclazide and its Impurity (Gliclazide Impurity A) in Bulk Drug

Author(s): Surendran Vijayaraj*, Narahari N. Palei, Thummala Katyayani

Journal Name: Current Pharmaceutical Analysis

Volume 15 , Issue 7 , 2019

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Graphical Abstract:


Background: Gliclazide Impurity A (GI-A) is one of the gliclazide impurities, as described in the European Pharmacopoeia.

Objective: The objective of this study was to develop and validate simple, robust and accurate Reverse- Phase High-Performance Liquid Chromatography (RP-HPLC) method for estimation of gliclazide along with GI-A in bulk by optimising chromatographic parameters using Box Behnken design in response surface methodology.

Methods & Results: Box Behnken design was employed for optimizing flow rate, injection volume and strength of the buffer in order to minimize retention time of both gliclazide and GI-A. The optimized strength of orthophosphoric acid buffer in a mixture of Acetonitrile (50:50 v/v), flow rate and injection volume were found to be 25mM, 1mL/min, 20 µL respectively. Linearity was observed in concentration range of 25-150 µg/mL (r2=0.999). The retention time of gliclazide and GI-A was found to be 5.799 minutes and 3.819 minutes, respectively. The limit of detection for Gliclazide and GI-A was found to be 0.0066, and 0.0075 µg/mL and the limit of quantification limit was found to be 0.0202, 0.0228 µg/mL, respectively. The developed method was validated as per the ICH guidelines.

Conclusion: The proposed method is useful for best analysis of Gliclazide and GI-A in pharmaceutical dosage forms. QbD approach was found to be an effective tool for optimising chromatographic conditions of the proposed method.

Keywords: Gliclazide, Impurity A, RP-HPLC, Box Behnken design, QbD, bulk drug.

Martindale. The Complete Drug Reference, 32nd ed; Pharmaceutical Press: London, 1999.
British Pharmacopoeia; The Stationery Office: United Kingdom, 1998.
European Pharmacopeia, Council of Europe, 9th ed.; France, 2016.
Wu, D.; Wang, X.; Pang, D.; Su, W.; Sun, Y. Gliclazide impurity F: N-[(perhydrocyclopenta[c]pyrrol-2-yl)aminocarbonyl]-o-toluenesulfonamide. Acta Crystallogr. Sect. E Struct. Rep. Online, 2012, 68(Pt 2), 446.
Brunton, L.L.; Lazo, J.S.; Parker, K.L. Goodman and Gillman’s The Pharmacological basis of therapeutics, 11th ed; Mcgraw-Hill: New York, 2005.
Tripathi, K.D. Essentials of Medical Pharmacology, 5th ed; Jaypee Brothers Medical Publishers: New Delhi, 2004.
Doomkaew, A.; Prutthiwanasan, B.; Suntornsuk, L. Stability indicating MEKC method for the determination of gliclazide and its specified impurities. J. Pharm. Biomed. Anal., 2015, 102, 119-128.
Doomkaew, A.; Prapatpong, P.; Buranphalin, S.; Vander Heyden, Y.; Suntornsuk, L. Fast and simultaneous analysis of combined anti-diabetic drugs by capillary zone electrophoresis. J. Chromatogr. Sci., 2015, 53(6), 993-999.
Hrichi, H.; Louhaichi, M.R.; Lotfi Monser, L.; Adhoum, N. Gliclazide voltammetric sensor based on electropolymerized molecularly imprinted polypyrrole film onto glassy carbon electrode. Sens. Actuators B Chem., 2014, 204, 42-49.
Krzek, J.; Dabrowska, M.; Hubicka, U. Identification and determination of Gliclazide and its impurities in various medicines by Thin-Layer Chromatography and densitometry. J. Planar Chromatog., 2001, 14, 183-187.
Frank, H.; Heinisch, G.; Neumayer, E. Identity control of formulated drugs by Thin layer chromatography Part 1: some selected tablets. Sci. Pharm., 1986, 54(4), 305-311.
El-Kousy, N. Colorimetric determination of the antidiabetic drug Gliclazide. J. Drug Res., 1991, 20(1-2), 157-162.
El-Kousy, N.; Ashoor, F. Colorimetric determination of two anti diabetic drugs using cobalt chloride. J. Drug Res., 1990, 19(1-2), 35-43.
Kamla, M.E.; Abdel-Maboud, I.M.; Hassan, F.A.; Ibrahim, A.D. Spectrophotometric determination of some pharmaceutical compounds using 2, 2-diphenyl-1-picrylhydrazyl. Anal. Lett., 1993, 26(11), 2385-2395.
Raul, S.K.; Spandana, B.; Sameera, P.; Vikitha, V.U.V. Spectrophotometric method development and validation for the estimation of gliclazide in bulk and pharmaceutical dosage form. Asian J. Pharm. Ana., 2016, 6(3), 143-146.
Hrichi, H.; Louhaichi, M.R.; Lotfi Monser, L.; Adhoum, N. Gliclazide voltammetric sensor based on electropolymerized molecularly imprinted polypyrrole film onto glassy carbon electrode. Sens. Actuators B Chem., 2014, 204, 42-49.
Krzek, J.; Czekaj, J.; Moniczewska, M.; Rzeszutko, W.O. Determination of gliclazide in pharmaceutical preparations by capillary gas chromatography with cool on-column injection and elimination of the matrix effect. J. AOAC Int., 2001, 84(6), 1695-1702.
Kuo, C.Y.; Wu, S.M. High-performance liquid chromatography with electrochemical detection for analysis of gliclazide in plasma. J. Chromatogr. A, 2005, 1088(1-2), 131-135.
Nadkarni, D.R.; Merchant, R.N.; Sundaresan, M.; Bhagwat, A.M. Isocratic separation and simultaneous estimation of four anti-diabetic members of the sulphonyl urea family by reverse phase HPLC. Indian Drugs, 1997, 34, 650-653.
Igaki, A.; Kobayashi, K.; Kimura, M.; Sakoguchi, T.; Matsuoka, A. Determination of serum sulfonyl ureas by High Performance Liquid Chromatography with flourimetric detection. J. Chromatogr. , 1989, 493(1), 222-229.
Sidhu, A.S.; Kennedy, J.M.; Deeble, S. General method for the analysis of pharmaceutical dosage forms by High-Performance Liquid Chromatography. J. Chromatogr. , 1987, 391(1), 233-242.
Peraman, R.; Bhadraya, K.; Padmanabha Reddy, Y. Analytical quality by design: A tool for regulatory flexibility and robust analytics. Int. J. Anal. Chem., 2015, 2015868727
U.S. Department of health and human services, food and drug administration, Centre for Drug Evaluation and Research (CDER), Centre for Biologics Evaluation and Research (CBER). Guidance for industry, Q2 (R1) Validation of Analytical Procedures: Methodology, International Conference on Harmonization, Geneva, November, 2005.
International Conference of Harmonization for Technical requirements for the Registration of Drugs for Human use. ICH, Q2B Validation of Analytical Procedure; Methodology, Geneva, Switzerland, May, 1997.
International Federation of Pharmaceutical Manufactures and Associations (IFPMA) Validation of analytical procedures: text and methodology. Proceedings of the International Conference on Harmonization, Methodology Q2 (R1) Geneva, Switzerland. ICH, Switzerland:, 1996.

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Article Details

Year: 2019
Published on: 14 October, 2019
Page: [716 - 723]
Pages: 8
DOI: 10.2174/1573412914666180523092012
Price: $65

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