Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design
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, fu...
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MDPI AG
2016-10-01
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| Series: | Scientia Pharmaceutica |
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| Online Access: | http://www.mdpi.com/2218-0532/84/4/671 |
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| author | Sushant B. Jadhav Rahul M. Mane Kalyanraman L. Narayanan Popatrao N. Bhosale |
| author_facet | Sushant B. Jadhav Rahul M. Mane Kalyanraman L. Narayanan Popatrao N. Bhosale |
| author_sort | Sushant B. Jadhav |
| collection | DOAJ |
| description | 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. |
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| last_indexed | 2024-12-10T08:21:49Z |
| publishDate | 2016-10-01 |
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| series | Scientia Pharmaceutica |
| spelling | doaj.art-ec6fa3ebd6af48f284fbae9c55818f1a2022-12-22T01:56:20ZengMDPI AGScientia Pharmaceutica2218-05322016-10-0184467168410.3390/scipharm84040671scipharm84040671Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial DesignSushant B. Jadhav0Rahul M. Mane1Kalyanraman L. Narayanan2Popatrao N. Bhosale3Department of Chemistry, Shivaji University, Kolhapur 416-004, Maharashtra, IndiaDepartment of Chemistry, Shivaji University, Kolhapur 416-004, Maharashtra, IndiaResearch and Development, Integrated Product Development, Dr. Reddy’s Laboratories Ltd., Bachupally, Hyderabad 500-090, Telangana, IndiaDepartment of Chemistry, Shivaji University, Kolhapur 416-004, Maharashtra, IndiaA 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.http://www.mdpi.com/2218-0532/84/4/671S-isomerenantiomerdesign of experiments (DoE)developmentlinagliptin and metformin hydrochloride |
| spellingShingle | Sushant B. Jadhav Rahul M. Mane Kalyanraman L. Narayanan Popatrao N. Bhosale Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design Scientia Pharmaceutica S-isomer enantiomer design of experiments (DoE) development linagliptin and metformin hydrochloride |
| title | Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design |
| title_full | Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design |
| title_fullStr | Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design |
| title_full_unstemmed | Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design |
| title_short | Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design |
| title_sort | analytical enantio separation of linagliptin in linagliptin and metformin hcl dosage forms by applying two level factorial design |
| topic | S-isomer enantiomer design of experiments (DoE) development linagliptin and metformin hydrochloride |
| url | http://www.mdpi.com/2218-0532/84/4/671 |
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