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%.
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Wang, XQ., Xiang, Z., Yu, XM. et al. LC–MS–MS Determination of Nikethamide in Human Plasma. Chroma 69, 1067–1071 (2009). https://doi.org/10.1365/s10337-009-1041-z
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DOI: https://doi.org/10.1365/s10337-009-1041-z