蛍光検出高速液体クロマトグラフィーによる体液中Isofloxythepin の測定

概要

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A high sensitive method for the determination of isofloxythepin (IFT) in biological fluids by high-performance liquid chromatography (HPLC) with fluorometric detection is described. When IFT was treated with 1-anthroyl (AN) nitrile in the presence of triethylamine at 70℃, the condensation reaction occurred and was completed in 60 min, yielding the AN derivative (IFT-AN). The chromatographic separation of IFT-AN was achieved on YMC-PACK A-302-ODS with 0.2% ammonium bicarbonate-methanol-acetonitrile(1 : 4 : 9) as a mobile phase. A calibration curve was constructed by plotting the ratio of the peak height of IFT to that of internal standard against the amount of IFT, a linear response being observed in the range 0.15-12.89 ng. Clean-up of IFT in the plasma and urine of the dog was efficiently attained by extracting with n-hexane under basic conditions and derivatized with AN nitrile. The resulting product was extracted with hexane-benzene in the presence of acetonitrile under acidic conditions and subjected to HPLC. The quantitation limit of IFT in the canine plasma was estimated to be 0.6 ng/ml. The recovery rates of standard sample added to the canine plasma and urine were found to be 93.9 and 95.9%, respectively.
社団法人日本薬学会の論文
1988-05-25