TITLE:
A New and Enantioselective Chromatographic Method for Linagliptin on Amylose Coated Chiral Stationary Phase
AUTHORS:
Cholleti Vijay Kumar, Pasula Aparna, Pavan Kumar Vasa, Y. Ravindra Kumar, Nitin Haridas Dhekale
KEYWORDS:
Enantiomers, Amylose Based Stationary Phase, Method Development, Method Validation, Specificity
JOURNAL NAME:
American Journal of Analytical Chemistry,
Vol.7 No.7,
July
20,
2016
ABSTRACT: A new and enantioselective liquid chromatographic
method was developed for estimation of S-Linagliptin in Linagliptin (LINA)
drug substances. The desired enantiomeric separation was achieved on Chiralpak
AD-H (250*4.6
mm*5 μm)
column with the mobile phase composition of ethanol, methanol and diethylamine
in a ratio of 90:10:0.1 (v/v/v) with flow rate of 0.5 mL·min-1 and column oven temperature 30°C and the eluted compounds were monitored at 225
nm. In the proposed chiral method, USP resolutions between both the enantiomers
were more than 5.0. Limit of detection and Limit of quantitation of S-LINA was
found to be 0.03 μg·mL-1 and
0.10 μg·mL-1 respectively. Linearity study was conducted from LOQ to 150% and correlation
coefficient found to be 0.9997. Accuracy was within the range of 98.6% to
101.5%. To prove selectivity power of the method specificity study was
conducted by subjecting drug substance to acid, base, hydrolysis, oxidation and
photolysis and ensured the peak purity of analyte in degraded samples.
Moreover, the method has been fully validated as per ICH guidelines. The
proposed method is precise, accurate, linear, rugged, robust and suitable for
accurate quantification of S-LINA in LINA drug substance.