Chromatographia

, Volume 78, Issue 21–22, pp 1395–1400 | Cite as

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

  • Qi Wang
  • Xiuli Chen
  • Cuiwei Zhang
  • Mengya Liao
  • Mingxing Hu
  • Shuo Lin
  • Yongmei Xie
  • Wenya Yin
  • Yiwen Zhang
Short Communication
First Online:
Received:
Revised:
Accepted:

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.

Keywords

Column liquid chromatography Chiral separation Enantiomeric purity Trelagliptin Pre-column derivatization 
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Notes

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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Copyright information

© Springer-Verlag Berlin Heidelberg 2015

Authors and Affiliations

  • Qi Wang
    • 1
  • Xiuli Chen
    • 1
  • Cuiwei Zhang
    • 3
  • Mengya Liao
    • 4
  • Mingxing Hu
    • 1
  • Shuo Lin
    • 1
  • Yongmei Xie
    • 1
  • Wenya Yin
    • 2
  • Yiwen Zhang
    • 1
  1. 1.State Key Laboratory of Biotherapy and Cancer CenterWest China Hospital, Sichuan University, and Collaborative Innovation Center for BiotherapyChengduChina
  2. 2.Department of Nutrition, Food Safety and ToxicologyWest China School of Public Health, Sichuan UniversityChengduChina
  3. 3.Department of PathologyThe Affiliated Hospital of Luzhou Medical CollegeLuzhouChina
  4. 4.Chengdu University of Traditional Chinese MedicineChengduChina

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