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セミミクロカラム高速液体クロマトグラフィー-紫外吸収法を用いた簡便で高感度な, ヒト血液試料中の3種のオキシカム系非ステロイド性抗炎症薬(tenoxicam, piroxicam, lornoxicam)の定量法を開発した.血中の対象薬物及び内標準をジクロロメタンで抽出し, セミミクロODSカラム(250×1.5mm i.d., 5μm)で分離した.溶離液にアセトニトリル-酢酸緩衝液-メタノールの混液を用い, 検出は365nmで行った.内標準にはisoxicamを用いた.その結果, 血液成分に妨害されることなく, 30分以内に分離定量することができた.Tenoxicam, piroxicam及びlornoxicamの検出下限(signal-to-noise ratio=3)はそれぞれ血清で2.3, 4.2, 6.4ng/ml, 血しょうでは2.7, 4.7, 9.3ng/mlであった.本法をlornoxicam服用患者の血清試料に適用した.A simple and rapid semi-micro column high-performance liquid chromatographic (HPLC) method with UV detection was developed for the simultaneous detrmination of oxicam nonsteroidal anti-inflammatory drugs in human blood samples. Oxicams including isoxicam as an internal standard were extracted from buffered plasma samples (pH3) with dichloromethane, and the resulting extracts were subjected to HPLC analysis. The separation was performed with a C_<18> reversed-phase semi-micro column (250×1.5mm i.d., 5μm) at 35℃. The mobile phase used was a mixture of acetonitrile-0.1M acetate buffer (pH5.0)-methanol, and the detection wavelength was set at 365nm. Four oxicams were well-separated within 30min without interference by the blood components. The detection limits of tenoxicam, piroxicam, and lornoxicam were 2.3, 4.2, 6.4ng/ml in serum, and 2.7, 4.7, 9.3ng/ml in plasma at a signal-to-noise ratio of 3, respectively. The method was applied to the determination of lornoxicam in the sera of patients

Semi-Micro Column HPLC of Three Oxicam Non-Steroidal Anti-Inflammatory Drugs in Human Blood