Chemical Research in Chinese Universities ›› 2010, Vol. 26 ›› Issue (1): 33-37.

• Articles • Previous Articles     Next Articles

Development and Validation of a Reverse-phase High Performance Liquid Chromatography Method for Determination of Exenatide in Poly(lactic-co-glycolic acid) Microspheres

LIU Bin1,2, DONG Qing-guang1, SHI Lin1, WANG Meng-shu1, LI Chun1, WU Yong-ge1, YU Xiang-hui1, SHAN Ya-ming1, CHEN Yan1*, KONG Wei1,2* and SHEN Jia-cong2   

  1. 1. AIDS Vaccine National Engineering Lab,
    2. State Key Laboratory of Supramolecular Structure and Material, Jilin University, Changchun 130012, P. R. China
  • Received:2009-01-15 Revised:2009-04-08 Online:2010-01-04 Published:2010-03-29
  • Contact: CHEN Yan. E-mail: chen_yan@mail.jlu.edu.cn; KONG Wei. E-mail: weikong@mail.jlu.edu.cn
  • Supported by:

    Supported by the Key Projects in the National Science & Technology Pillar Program in the Eleventh Five-year Plan Period, China(No.2008ZX10001-012).

Abstract:

Exenatide(synthetic exendin-4), which has been approved by the Food and Drug Administration(FDA) for the adjunctive treatment of patients with type 2 diabetes, is an incretin mimetic agent. The development and validation of a RP-HPLC method for the quantification of the exenatide in poly(lactic-co-glycolic acid)(PLGA) microspheres is described. Separation was performed on a C4 column via a mobile phase consisting of ACN:KH2PO4(0.02 mol/L, pH=2.5) gradient elution from 30:70 to 45:55(volume ratio) in 30 min. Multi-diode array detection(DAD) appears to be most appropriate to evaluate the spectral purity of exenatide. The limits of detection and quantification of exenatide were 0.4 and 1.2 μg/mL, respectively. The calibration curve of exenatide was linear in a range of 0.025―0.2 mg/mL with a correlation coefficient of 0.9995. The results of validation study show that this method is specific, accurate(recovery>95%), precise(RSD<2.0%) and robust.

Key words: Exenatide; Quantification; RP-HPLC-DAD; PLGA; Microsphere