ABSTRACT: A procedure has been developed for the determination of a macrolide antibiotic roxythromycin (RX) in blood serum using HPLC
with mass spectrometric detection using clarithromycin (CL) as the internal standard. RX and CL have been extracted from the
samples by solid-phase extraction in a cartridge filled with a polar adsorbent, cyanopropylsilyl silica gel. The absolute
recoveries of RX and CL are 89.6 and 92.5%, respectively. Chromatographic separation has been performed on a Nucleodur C18 Isis column with the mobile phase composed as follows: water-methanol-acetonitrile-formic aid (499: 250: 250: 1 by volume).
Registration has been performed in the mode of selected ion monitoring with m/z 837.7 (RX) and m/z 748.7 (CL). The analytical range for RX is 0.097–14.81 μg/mL, the quantification limit is 0.097 μg/mL, the detection limit
is 0.03 μg/mL, and the intraday and interday relative standard deviation are 2–6 and 4–8% respectively. The procedure has
been applied to the pharmacokinetic studies of the Rulid pharmaceutical preparation.
Keywordsliquid chromatography–mass-spectrometric detection–roxythromycin
Journal of Analytical Chemistry 04/2012; 66(2):195-200. · 0.75 Impact Factor