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Determination of the Enantiomeric Purity of Trelagliptin by Pre-Column Derivatization and Liquid Chromatography on a Chiral Stationary Phase

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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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Acknowledgments

We are grateful for financial support from the Youth Foundation of Sichuan University (no. 2015SCU11042) and the National Natural Science Foundation of China (no. 81302639).

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    Authors and Affiliations

    1. State Key Laboratory of Biotherapy and Cancer Center, West China Hospital, Sichuan University, and Collaborative Innovation Center for Biotherapy, Chengdu, 610041, China

      Qi Wang, Xiuli Chen, Mingxing Hu, Shuo Lin, Yongmei Xie & Yiwen Zhang

    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

      Wenya Yin

    3. Department of Pathology, The Affiliated Hospital of Luzhou Medical College, Luzhou, 646000, China

      Cuiwei Zhang

    4. Chengdu University of Traditional Chinese Medicine, Chengdu, 610075, China

      Mengya Liao

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    1. Qi Wang
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    2. Xiuli Chen
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    4. Mengya Liao
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    6. Shuo Lin
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    7. Yongmei Xie
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    8. Wenya Yin
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    9. Yiwen Zhang
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    Corresponding authors

    Correspondence to Wenya Yin or Yiwen Zhang.

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    Q. Wang and X. Chen contributed equally to this work.

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    Wang, Q., Chen, X., Zhang, C. et al. Determination of the Enantiomeric Purity of Trelagliptin by Pre-Column Derivatization and Liquid Chromatography on a Chiral Stationary Phase. Chromatographia 78, 1395–1400 (2015). https://doi.org/10.1007/s10337-015-2946-3

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    • DOI: https://doi.org/10.1007/s10337-015-2946-3

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