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Analytical Enantio-Separation of Linagliptin in Linagliptin and Metformin HCl Dosage Forms by Applying Two-Level Factorial Design
- Source :
- Scientia Pharmaceutica, Vol 84, Iss 4, Pp 671-684 (2016), Scientia Pharmaceutica, Volume 84, Issue 4, Pages 671-684
- Publication Year :
- 2016
- Publisher :
- Österreichische Apotheker-Verlagsgesellschaft m. b. H., 2016.
-
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.
- Subjects :
- Pharmaceutical Science
lcsh:RS1-441
S-isomer
030209 endocrinology & metabolism
Linagliptin
01 natural sciences
Dosage form
Article
design of experiments (DoE)
lcsh:Pharmacy and materia medica
03 medical and health sciences
chemistry.chemical_compound
0302 clinical medicine
Impurity
Phase (matter)
enantiomer
medicine
linagliptin and metformin hydrochloride
development
Chromatography
Chemistry
Silica gel
010401 analytical chemistry
Factorial experiment
0104 chemical sciences
Methanol
Enantiomer
medicine.drug
Subjects
Details
- Language :
- English
- ISSN :
- 22180532
- Volume :
- 84
- Issue :
- 4
- Database :
- OpenAIRE
- Journal :
- Scientia Pharmaceutica
- Accession number :
- edsair.doi.dedup.....86659766fecab99a0ff9b59edb2985f6