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Sci. Pharm. 2016, 84(4), 671-684; doi:10.3390/scipharm84040671

Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design

1
Department of Chemistry, Shivaji University, Kolhapur 416-004, Maharashtra, India
2
Research and Development, Integrated Product Development, Dr. Reddy’s Laboratories Ltd., Bachupally, Hyderabad 500-090, Telangana, India
*
Authors to whom correspondence should be addressed.
Academic Editor: Thomas Erker
Received: 28 June 2016 / Accepted: 3 August 2016 / Published: 17 October 2016
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Abstract

A novel, stability indicating, reverse phase high-performance liquid chromatography (RP-HPLC) method was developed to determine the S-isomer of linagliptin (LGP) in linagliptin and metformin hydrochloride (MET HCl) tablets (LGP–MET HCl) by implementing design of experiment (DoE), i.e., two-level, full factorial design (23 + 3 centre points = 11 experiments) to understand the critical method parameters (CMP) and its relation with the critical method attribute (CMA), and to ensure robustness of the method. The separation of the S-isomer, LGP and MET HCl in the presence of their impurities was achieved on Chiralpak® IA-3 (Amylose tris (3, 5-dimethylphenylcarbamate), immobilized on 3 µm silica gel) stationary phase (250 × 4.6 mm, 3 µm) using isocratic elution and detector wavelength at 225 nm with a flow rate of 0.5 mL·min−1, an injection volume of 10 µL with a sample cooler (5 °C) and column oven temperature of 25 °C. Ethanol:Methanol:Monoethanolamine (EtOH:MeOH:MEA) in the ratio of 60:40:0.2 v/v/v was used as a mobile phase. The developed method was validated in accordance with international council for harmonisation (ICH) guidelines and was applied for the estimation of the S-isomer of LGP in LGP–MET HCl tablets. The same method also can be extended for the estimation of the S-isomer in LGP dosage forms. View Full-Text
Keywords: S-isomer; enantiomer; design of experiments (DoE); development; linagliptin and metformin hydrochloride S-isomer; enantiomer; design of experiments (DoE); development; linagliptin and metformin hydrochloride
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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MDPI and ACS Style

Jadhav, S.B.; Mane, R.M.; Narayanan, K.L.; Bhosale, P.N. Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design. Sci. Pharm. 2016, 84, 671-684.

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