Premium
A new stability indicating reverse phase high performance liquid chromatography method for the determination of enantiomeric purity of a DPP‐4 inhibitor drug linagliptin
Author(s) -
Salapaka Appalacharyulu,
Bonige Kishore Babu,
Korupolu Raghu Babu,
T Chandrasekhar Reddy,
K Chandrasekhar Reddy,
N Sreenivas,
Sharma Hemant Kumar,
Ray Uttam Kumar
Publication year - 2019
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.201800502
Subject(s) - chromatography , enantiomer , chemistry , elution , analyte , high performance liquid chromatography , resolution (logic) , acetonitrile , detection limit , analytical chemistry (journal) , stereochemistry , artificial intelligence , computer science
A simple, sensitive, and stability indicating isocratic reverse phase high performance liquid chromatography method has been developed, optimized and validated for the separation and quantification of S ‐enantiomer in linagliptin ( R ‐enantiomer) drug substance. Enantiomeric separation was achieved on a Cellulose tris(4‐chloro‐3‐methylphenylcarbamate) stationary phase. Mobile phase consists of aqueous diammonium hydrogen phosphate buffer and acetonitrile in the ratio of 35:65 v/v. Isocratic elution was performed at a flow rate of 1.0 mL/min, the column oven temperature was set at 40°C and detection was at 226 nm. The resolution between R and S enantiomers is found to be more than 4.0. The impact of mobile phase composition, pH of buffer and temperature on the resolution has been studied. The detector response is found to be linear over the concentration range of 0.17–1.7 μg/mL. LOD and LOQ levels of S ‐enantiomer are found to be 0.057 and 0.172 μg/mL respectively. The recovery of S ‐enantiomer is 99.8% w/w. The proposed method is validated for specificity, precision, linearity, accuracy and robustness.