Chromatographia

, Volume 69, Issue 9–10, pp 1067–1071 | Cite as

LC–MS–MS Determination of Nikethamide in Human Plasma

  • Xian-Qin Wang
  • Zheng Xiang
  • Xiao-Min Yu
  • Jian-Zhang Wu
  • Dan Lin
  • Fa-Qing Ye
Full Short Communication

Abstract

A sensitive LC–MS–MS method with electrospray ionization has been developed for determination of nikethamide in human plasma. After addition of atropine as internal standard, liquid–liquid extraction was used to produce a protein-free extract. Chromatographic separation was achieved on a 150 mm × 2.1 mm, 5 μm particle, Agilent Zorbax SB-C18 column, with 45:55 (v/v) methanol–water containing 0.1% formic acid as mobile phase. LC–MS–MS was performed in multiple reaction monitoring mode using target fragment ions m/z 178.8 → 107.8 for nikethamide and m/z 289.9 → 123.8 for the internal standard. Calibration plots were linear over the range of 20.0–2,000 ng mL−1. The lower limit of quantification was 20.0 ng mL−1. Intra-day and inter-day precisions were better than 4.2 and 6.1%, respectively. Mean recovery of nikethamide from human plasma was in the range 65.3–71.1%.

Keywords

Column liquid chromatography Tandem mass spectrometry Nikethamidein human plasma 

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Copyright information

© Vieweg+Teubner | GWV Fachverlage GmbH 2009

Authors and Affiliations

  • Xian-Qin Wang
    • 1
  • Zheng Xiang
    • 2
  • Xiao-Min Yu
    • 2
  • Jian-Zhang Wu
    • 2
  • Dan Lin
    • 1
  • Fa-Qing Ye
    • 1
  1. 1.Analytical and Testing CenterWenzhou Medical CollegeWenzhouPeople’s Republic of China
  2. 2.School of PharmacyWenzhou Medical CollegeWenzhouPeople’s Republic of China

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