Determination of the Enantiomeric Purity of Trelagliptin by Pre-Column Derivatization and Liquid Chromatography on a Chiral Stationary Phase |
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Authors: | Wang Qi Chen Xiuli Zhang Cuiwei Liao Mengya Hu Mingxing Lin Shuo Xie Yongmei Yin Wenya Zhang Yiwen |
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Institution: | 1.State Key Laboratory of Biotherapy and Cancer Center, West China Hospital, Sichuan University, and Collaborative Innovation Center for Biotherapy, Chengdu, 610041, China ;2.Department of Nutrition, Food Safety and Toxicology, West China School of Public Health, Sichuan University, 16#, Section 3, Renmin South Road, Chengdu, 610041, China ;3.Department of Pathology, The Affiliated Hospital of Luzhou Medical College, Luzhou, 646000, China ;4.Chengdu University of Traditional Chinese Medicine, Chengdu, 610075, China ; |
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Abstract: | A precise and sensitive LC method for determination
of enantiomeric purity of trelagliptin has been developed and validated. Pre-column derivatization was performed before separation. Baseline separation with a resolution factor >2.5 was accomplished within 10 min by use of a Chiralpak AD column (250 × 4.6 mm; particle size 5 µm) and n-hexane–2-propanol (90:10 v/v) as mobile phase at a flow rate of 1 mL min?1. Eluted analytes were monitored by UV detection at 260 nm. The effects of mobile phase composition and temperature on enantiomeric selectivity and on resolution of enantiomers were thoroughly investigated. Calibration curves were plotted within the concentration range 0.005–2 mg mL?1 (n = 12), and recoveries between 98.23 and 101.34 % were obtained, with relative standard deviation (RSD) <1.39 %. LOD and LOQ for the trelagliptin derivative were 1.51 and 5.03 µg mL?1; those for its enantiomer were 1.49 and 4.94 µg mL?1, respectively. The method was evaluated and validated by analysis of bulk samples of trelagliptin of different enantiomeric purity. It was demonstrated that the method was accurate, robust, and sensitive, and enabled practical analysis of real samples. |
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