Journal : Acta Chromatographica
Article : Development and validation of stability-indicating high-performance thin-layer chromatography method for estimation of repaglinide in bulk and in pharmaceutical formulation

Authors :
Fatemi, M. H.
University of Mazandaran Laboratory of Chemometrics, Faculty of Chemistry Babolsar Iran, mhfatemi@umz.ac.ir,
Elyasi, M.
University of Mazandaran Laboratory of Chemometrics, Faculty of Chemistry Babolsar Iran,
Sowa, I.
Medical University of Lublin Department of Analytical Chemistry Chodźki 4a 20-093 Lublin Poland, i.sowa@umlub.pl,
Zajdel, D.
Medical University of Lublin Department of Analytical Chemistry Chodźki 4a 20-093 Lublin Poland,
Kocjan, R.
Medical University of Lublin Department of Analytical Chemistry Chodźki 4a 20-093 Lublin Poland,
Pizoń, M.
Medical University of Lublin Department of Analytical Chemistry Chodźki 4a 20-093 Lublin Poland,
Wójciak-Kosior, M.
Medical University of Lublin Department of Analytical Chemistry Chodźki 4a 20-093 Lublin Poland,
Hadad, G. M.
Suez Canal University Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy Ismailia 41522 Egypt, ghhadad@hotmail.com,
Abdel-Salam, R. A.
Suez Canal University Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy Ismailia 41522 Egypt, dr_rasalam@yahoo.com,
Abdel-Hameed, E. A.
Suez Canal University Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy Ismailia 41522 Egypt,
Liu, W.-Y.
China Pharmaceutical University Department of Pharmaceutical Analysis 24 Tongjiaxiang Nanjing 210009 China, liuwenyuan8506@163.com,
Xie, S.-L.
China Pharmaceutical University Department of Pharmaceutical Analysis 24 Tongjiaxiang Nanjing 210009 China,
Xu, X. Z.
China Pharmaceutical University Department of Pharmaceutical Analysis 24 Tongjiaxiang Nanjing 210009 China,
Wu, C. Y.
China Pharmaceutical University Department of Pharmaceutical Analysis 24 Tongjiaxiang Nanjing 210009 China,
Feng, F.
China Pharmaceutical University Department of Phytochemistry 24 Tongjiaxiang Nanjing 210009 China,
Maślanka, A.
Jagiellonian University Medical College, Pharmaceutical Faculty, Department of Inorganic and Analytical Chemistry Medyczna 9 30-688 Krakow Poland,
Hubicka, U.
Jagiellonian University Medical College, Pharmaceutical Faculty, Department of Inorganic and Analytical Chemistry Medyczna 9 30-688 Krakow Poland,
Krzek, J.
Jagiellonian University Medical College, Pharmaceutical Faculty, Department of Inorganic and Analytical Chemistry Medyczna 9 30-688 Krakow Poland, jankrzek@cm-uj.krakow.pl,
Walczak, M.
Jagiellonian University Medical College, Pharmaceutical Faculty, Department of Pharmacokinetics and Physical Pharmacy Medyczna 9 30-688 Krakow Poland,
Izworski, G.
Jagiellonian University Medical College, Pharmaceutical Faculty, Department of Inorganic and Analytical Chemistry Medyczna 9 30-688 Krakow Poland,
Suchy, D.
Medical University of Silesia Department of Internal Medicine and Clinical Pharmacology Medyków 18 PL 40752 Katowice Poland, dariuszsuchy@gmail.com,
Łabuzek, K.
Medical University of Silesia Department of Internal Medicine and Clinical Pharmacology Medyków 18 PL 40752 Katowice Poland,
Pierzchała, O.
Medical University of Silesia Department of Internal Medicine and Clinical Pharmacology Medyków 18 PL 40752 Katowice Poland,
Okopień, B.
Medical University of Silesia Department of Internal Medicine and Clinical Pharmacology Medyków 18 PL 40752 Katowice Poland,
Vamsi Krishna, M.
Alliance Institute of Advanced Pharmaceutical and Health Sciences Ameerpet, Hyderabad 500038 Andhra Pradesh India, marothu_vamsi@rediffmail.com,
Dash, R. N.
Alliance Institute of Advanced Pharmaceutical and Health Sciences Ameerpet, Hyderabad 500038 Andhra Pradesh India,
Jalachandra Reddy, B.
Alliance Institute of Advanced Pharmaceutical and Health Sciences Ameerpet, Hyderabad 500038 Andhra Pradesh India,
Venugopal, P.
Alliance Institute of Advanced Pharmaceutical and Health Sciences Ameerpet, Hyderabad 500038 Andhra Pradesh India,
Sandeep, P.
Alliance Institute of Advanced Pharmaceutical and Health Sciences Ameerpet, Hyderabad 500038 Andhra Pradesh India,
Madhavi, G.
Alliance Institute of Advanced Pharmaceutical and Health Sciences Ameerpet, Hyderabad 500038 Andhra Pradesh India,
Raghavi, K.
K.V.S.R Siddhartha College of Pharmaceutical Sciences Vijayawada 520010 AP India,
Sindhura, M.
K.V.S.R Siddhartha College of Pharmaceutical Sciences Vijayawada 520010 AP India,
Prashanthi, R.
K.V.S.R Siddhartha College of Pharmaceutical Sciences Vijayawada 520010 AP India,
Nalluri, B. N.
K.V.S.R Siddhartha College of Pharmaceutical Sciences Vijayawada 520010 AP India, buchinalluri@yahoo.com,
Jain, P. S.
R. C. Patel Institute of Pharmaceutical Education and Research Karwand Naka, Shirpur, Dist. Dhule 425 405 (M. S.) India, pritash79@yahoo.com,
Patel, M. K.
R. C. Patel Institute of Pharmaceutical Education and Research Karwand Naka, Shirpur, Dist. Dhule 425 405 (M. S.) India,
Surana, S. J.
R. C. Patel Institute of Pharmaceutical Education and Research Karwand Naka, Shirpur, Dist. Dhule 425 405 (M. S.) India,
Abstract : A simple, selective, precise, and stability-indicating high-performance thin-layer chromatographic method for analysis of repaglinide both in a bulk and in pharmaceutical formulation has been developed and validated. The method employed high-performance thin-layer chromatography (HPTLC) aluminum plates precoated with silica gel 60 RP-18 F254 as the stationary phase. The solvent system consisted of chloroform-methanol-ammonia (4.5:0.8:0.05, v/v). The system was found to give compact spot for repaglinide (RF value of 0.55 ± 0.03). Densitometric analysis of repaglinide was carried out in the absorbance mode at 288 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.998 ± 0.0015 with respect to peak area in the concentration range 600–1600 ng per spot. The mean value ± SD of slope and intercept were 3.38 ± 1.47 and 986.9 ± 108.78, with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantification were 22.64 and 68.84 ng per spot, respectively. Repaglinide was subjected to acid and alkali hydrolysis, oxidation, and thermal degradation. The drug undergoes degradation under acidic and basic conditions. This indicates that the drug is susceptible to acid and base. The degraded product was well resolved from the pure drug with significantly different RF value. Statistical analysis proves that the method is repeatable, selective, and accurate for the estimation of investigated drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of repaglinide in bulk drug and pharmaceutical formulation.

Keywords : repaglinide, HPTLC, validation, stability, degradation,
Publishing house : University of Silesia in Katowice
Publication date : 2013
Number : Vol. 25, no. 3
Page : 531 – 544

Bibliography
: 1 ICH, Stability testing of new drug substances and products Q1A (R2), International Conference on Harmonization, IFPMA, Geneva, 2003
2 Martindale, The Complete drug reference, 33rd edn., Council of Royal Pharmaceutical Society of Great Britain, 2007, pp. 334
3 Budavari, The Merck Index, 13th edn., Merck and Co. Inc., White House station, NJ, 2001, pp. 790
4 United States Pharmacopeia, Asian edn., USP Convention Inc., Rockville, MD, 2003, pp. 623
5 A.B. Ruzilawati, M.S. Wahab, A. Imran, Z. Ismail, and S.H. Gan, J. Pharm. Biomed. Anal., 43, 1831–1835 (2007)
6 M. Gandhimathi, T.K. Ravi, and S.K. Renu, Anal. Sci., 19, 1675–1677 (2003)
7 R.H. Khan, S. Talegaonkar, R.M. Singh, S.C. Mathur, R. Shiv, and G.N. Singh, Indian Drugs, 44, 428–433 (2007)
8 A. Goyal and I. Singhavi, Indian J. Pharm. Sci., 68, 656–657 (2006)
9 Gumieniczek, A. Berecka, and H. HopkaŁa, J. Planar Chromatogr., 18, 155–159 (2005)
10 G.Y. Swamy, K. Ravikumar, and L.K. Wadhwa, Acta Cryst., 61, 3608–3610 (2005)
11 P.D. Sethi, High Performance Thin Layer Chromatography (Quantitative Analysis of Pharmaceutical Formulations), CBS Publishers, New Delhi, 1996, 56–63
12 M. Bakshi and S. Singh, J. Pharm. Biomed. Anal., 28, 1011–1040 (2002)
13 S. Singh and M. Bakshi, Pharm. Tech., 24, 1–14 (2000)
14 ICH, Guidance on Analytical Method Validation, in: Proceedings of the International Convention on Quality for the Pharmaceutical Industry, Toronto, September 2002
15 ICH, Q2A Validation of Analytical Procedure, in: Methodology, International Conference on Harmonization, Geneva, October 1994
16 ICH Harmonised Tripartite Guideline: Validation of Analytical Procedures: Text and Methodology, Q2(R1) Geneva, 2005
17 M.C. Sharma and S. Sharma, Int. J. Chem. Tech. Res., 3, 210–216 (2011)
DOI :
Qute : Fatemi, M. H. ,Elyasi, M. ,Sowa, I. ,Zajdel, D. ,Kocjan, R. ,Pizoń, M. ,Wójciak-Kosior, M. ,Hadad, G. M. ,Abdel-Salam, R. A. ,Abdel-Hameed, E. A. ,Liu, W.-Y. ,Xie, S.-L. ,Xu, X. Z. ,Wu, C. Y. ,Feng, F. ,Maślanka, A. ,Hubicka, U. ,Krzek, J. ,Walczak, M. ,Izworski, G. ,Suchy, D. ,Łabuzek, K. ,Pierzchała, O. ,Okopień, B. ,Vamsi Krishna, M. ,Dash, R. N. ,Jalachandra Reddy, B. ,Venugopal, P. ,Sandeep, P. ,Madhavi, G. ,Raghavi, K. ,Sindhura, M. ,Prashanthi, R. ,Nalluri, B. N. ,Jain, P. S. ,Patel, M. K. ,Surana, S. J. ,Surana, S. J. , Development and validation of stability-indicating high-performance thin-layer chromatography method for estimation of repaglinide in bulk and in pharmaceutical formulation. Acta Chromatographica Vol. 25, no. 3/2013
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