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A high-performance liquid chromatographic (HPLC) method for the quantitative determination of 1-hexylcarbamoyl-5-fluorouracil (HCFU) and its metabolites using mu Bondapak C18 and mu Porasil has been developed. Two mobile phases containing PIC-B7 (consisting of acetic acid and 1-heptanesulphonic acid) were used for the separation, and good separations were obtained. With methanol-water (56:44) as the mobile phase, the separation of HCFU and its three metabolites was achieved within 4 min. With methanol-water (32:68) a new metabolite, 1-omega-carboxymethylcarbamoyl-5-fluorouracil, was revealed in human plasma. The recovery of each substance was 80% or greater and the sensitivity was at the nanograms per millilitre level. The coefficient of variation was less than 3.6% for each component.
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