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

Authors :
Mansoor, S.
Georgia Institute of Technology School of Chemical and Biomolecular Engineering Atlanta GA 30332-0100 USA,
Tas, C.
Georgia Institute of Technology School of Chemical and Biomolecular Engineering Atlanta GA 30332-0100 USA, ctas@gata.edu.tr,
Patel, D. S.
Pramukh Swami Science and H.D. Patel Arts College Chemistry Department Sarva Vidyalaya Campus Kadi 382 715 Gujarat India,
Sharma, N.
BA Research India Ltd. Bio-Analytical Laboratory Bodakdev, Ahmedabad 380054 Gujarat India,
Patel, M. C.
Pramukh Swami Science and H.D. Patel Arts College Chemistry Department Sarva Vidyalaya Campus Kadi 382 715 Gujarat India,
Patel, B. N.
BA Research India Ltd. Bio-Analytical Laboratory Bodakdev, Ahmedabad 380054 Gujarat India, bhavinpatel27@rediffmail.com,
Shrivastav, P. S.
Gujarat University Department of Chemistry, School of Sciences Navrangpura, Ahmedabad 380009 Gujarat India, pranav_shrivastav@yahoo.com,
Sanyal, M.
St. Xavier’s College Department of Chemistry Navrangpura, Ahmedabad 380009 Gujarat India,
Wang, G. Y.
Chinese Academy of Sciences Key Laboratory of Chemistry of Northwestern Plant Resources and Key Laboratory for Natural Medicine of Gansu Province, Lanzhou Institute of Chemical Physics Lanzhou 730000 P. R. China,
Shi, Y. P.
Lanzhou University of Technology School of Petroleum and Chemical Engineering Lanzhou 730050 P. R. China, shiyp@licp.cas.cn,
Akowuah, G. A.
UCSI University Faculty of Applied Sciences No. 1, Jalan Menara Gading, UCSI Heights 56000 Kuala Lumpur Malaysia, wuahmy@yahoo.com,
Okechukwu, P. N.
UCSI University Faculty of Pharmaceutical Sciences No. 1, Jalan Menara Gading, UCSI Heights 56000 Kuala Lumpur Malaysia,
Chiam, N. C.
UCSI University Faculty of Pharmaceutical Sciences No. 1, Jalan Menara Gading, UCSI Heights 56000 Kuala Lumpur Malaysia,
Raszewski, G.
Institute of Agricultural Medicine Department of Pathophysiology Lublin Poland, grasz@galen.imw.lublin.pl,
Juszczak, M.
Institute of Agricultural Medicine Department of Medical Biology Lublin Poland,
Lemieszek, M. K.
Institute of Agricultural Medicine Department of Medical Biology Lublin Poland,
Matysiak, J.
University of Life Sciences Department of Chemistry Lublin Poland,
Niewiadomy, A.
University of Life Sciences Department of Chemistry Lublin Poland,
Rzeski, W.
Maria Curie-Sklodowska University Department of Virology and Immunology, Institute of Microbiology and Biotechnology Lublin Poland,
Reddy, P. S.
IPDO Dr. Reddy’s Laboratories Ltd. Bachupally, Hyderabad 500072 A.P India, sunilpsr@yahoo.com,
Babu, K. S.
S. K. University Department of Chemistry Anantapur 515055 A.P. India,
Kumar, N.
IPDO Dr. Reddy’s Laboratories Ltd. Bachupally, Hyderabad 500072 A.P India,
Pareek, D.
Rajiv Gandhi Technological University School of Pharmaceutical Sciences Bhopal 462033 Madhya Pradesh India,
Jain, S.
Sagar Institute of Research and Technology Ayodhya bypass, Bhopal 462 041 MP India,
Basniwa, P. K.
Rajiv Gandhi Technological University School of Pharmaceutical Sciences Bhopal 462033 Madhya Pradesh India,
Jain, D.
Rajiv Gandhi Technological University School of Pharmaceutical Sciences Bhopal 462033 Madhya Pradesh India, deepti2515@yahoo.com,
Wróblewski, K.
Medical University of Lublin Department of Inorganic Chemistry 4a Chodźki Str. 20-093 Lublin Poland,
Petruczynik, A.
Medical University of Lublin Department of Inorganic Chemistry 4a Chodźki Str. 20-093 Lublin Poland,
Waksmundzka-Hajnos, M.
Medical University of Lublin Department of Inorganic Chemistry 4a Chodźki Str. 20-093 Lublin Poland, monika.hajnos@umlub.pl,
Jain, P. S.
R. C. Patel Institute of Pharmaceutical Education and Research Karwand Naka, Shirpur, Dist. Dhule 425 405 MS India, pritash79@yahoo.com,
Chaudhari, A. J.
R. C. Patel Institute of Pharmaceutical Education and Research Karwand Naka, Shirpur, Dist. Dhule 425 405 MS India,
Surana, S. J.
R. C. Patel Institute of Pharmaceutical Education and Research Karwand Naka, Shirpur, Dist. Dhule 425 405 MS India,
Abstract : A simple, selective, precise, and stability-indicating high-performance thinlayer chromatographic method for analysis of sitagliptin phosphate both in a bulk and in pharmaceutical formulation has been developed and validated. The method employed high-performance thin-layer chromatography (HPTLC) aluminium plates precoated with silica gel 60 RP-18 F254 as the stationary phase. The solvent system consisted of methanol-water-triethylamine (8:2:0.05 v/v). The system was found to give compact spot for sitagliptin phosphate (Rf value of 0.55 ± 0.03). Densitometric analysis of sitagliptin phosphate was carried out in the absorbance mode at 267 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 1000–6000 ng per spot. The mean value ± SD of slope and intercept was 0.723 ± 0.043 and 17.24 ± 18.78 with respect to peak area. The method was validated for precision, recovery, and robustness. The limits of detection and quantification were 85.80 and 265.42 ng per spot, respectively. Sitagliptin phosphate was subjected to acid and alkali hydrolysis, oxidation, and photo and thermal degradation. The drug undergoes degradation under acidic, basic, and oxidative conditions. This indicates that the drug is susceptible to acid and base, and oxidation. 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 sitagliptin phosphate in bulk drug and pharmaceutical formulation.

Keywords : sitagliptin phosphate (SITA), HPTLC, validation, stability, degradation,
Publishing house : University of Silesia in Katowice
Publication date : 2014
Number : Vol. 26, no. 2
Page : 309 – 319

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DOI :
Qute : Mansoor, S. ,Tas, C. ,Patel, D. S. ,Sharma, N. ,Patel, M. C. ,Patel, B. N. ,Shrivastav, P. S. ,Sanyal, M. ,Wang, G. Y. ,Shi, Y. P. ,Akowuah, G. A. ,Okechukwu, P. N. ,Chiam, N. C. ,Raszewski, G. ,Juszczak, M. ,Lemieszek, M. K. ,Matysiak, J. ,Niewiadomy, A. ,Rzeski, W. ,Reddy, P. S. ,Babu, K. S. ,Kumar, N. ,Pareek, D. ,Jain, S. ,Basniwa, P. K. ,Jain, D. ,Wróblewski, K. ,Petruczynik, A. ,Waksmundzka-Hajnos, M. ,Jain, P. S. ,Chaudhari, A. J. ,Surana, S. J. ,Surana, S. J. , Development and validation of stability-indicating high-performance thin-layer chromatography method for estimation of sitagliptin phosphate monohydrate in bulk and in pharmaceutical formulation. Acta Chromatographica Vol. 26, no. 2/2014
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