Separation and determination of acetyl-glutamine enantiomers by HPLC-MS and its application in pharmacokinetic study.

Journal: Journal of pharmaceutical analysis
Published Date: Jun 13, 2017

Abstract

A high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) method was established for the separation and determination of acetyl-glutamine enantiomers (acetyl-L-glutamine and acetyl-D-glutamine) simultaneously. Baseline separation was achieved on Chiralpak AD-H column (250 mm × 4.6 mm, 5 µm). -Hexane (containing 0.1% acetic acid) and ethanol (75:25, v/v) were used as mobile phase at a flow rate of 0.6 mL/min. The detection was operated in the negative ion mode with an ESI source. [M-H] 187.0540 for enantiomers and [M-H] 179.0240 for aspirin (IS) were selected as detecting ions. The linear range of the calibration curve for each enantiomer was 0.05-40 µg/mL. The precision of this method at concentrations of 0.5-20 µg/mL was within 7.23%, and the accuracy was 99.81%-107.81%. The precision at LOQ (0.05 µg/mL) was between 16.28% and 17.56%, which was poor than that at QC levels. The average extraction recovery was higher than 85% for both enantiomers at QC levels. The pharmacokinetics of enantiomers was found to be stereoselective. There was not chiral inversion in vivo or in vitro between enantiomers.

Authors

  • Xiaoxiao Zhang
    Key Laboratory of Drug Quality Control&Pharmacovigilance (China Pharmaceutical University), Ministry of Education, Nanjing, China.
  • Lei Gao
    Microscopy Core Facility, Biomedical Research Core Facilities, Westlake University, Hangzhou, China.
  • Zunjian Zhang
    Key Laboratory of Drug Quality Control and Pharmacovigilance, China Pharmaceutical University, Ministry of Education, Nanjing, 210009, China.
  • Yuan Tian
    Department of Geriatrics, Union Hospital, Tongji Medical College, Huazhong University of Science and Technology, Wuhan, Hubei, China.

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