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The method was based on fluorescence labeling of both drugs with a fluorescent arylboronic acid 4\u2010(4,5\u2010diphenyl\u20101<jats:italic>H<\/jats:italic>\u2010imidazol\u20102\u2010yl)phenyl boronic acid followed by separation on silica column using a mobile phase consisting of acetonitrile and water (90:10, v\/v%) containing triethylamine and acetic acid. The labeling reaction conditions were optimized and the liquid\u2013liquid extraction method was successfully applied to extract the both drugs from serum. The linearity range was 0.025\u20132.00 \u00b5g\/mL for HZ and CZ. The limit of detection (S\/N = 3) was 10 and 5 ng\/mL for HZ and CZ, respectively. 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