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目的:建立反相高效液相色谱法同时测定血浆中奥卡西平(OXC)及其活性代谢产物-10-单羟基代谢物(MHD)的浓度。方法:采用Waters X-TerraTM RP_(18)柱(150mm×3.9mm,5μm),柱温35℃,流速1.2ml·ml~(-1),流动相:甲醇-O.1%三氟乙酸(30:70),检测波长232nm。甲喹酮作为内标,血浆样品经蛋白沉淀法处理后直接进样测定。结果:OXC在0.625~37.50μg·ml~1,MHD在1.25~75.0μg·ml~(-1)的范围线性关系良好。OXC低、中、高三种浓度的提取回收率分别为109.9%,102.0%,104.1%。日内RSD为1.69%~3.61%,日间RSD为2.73%~7.45%;MHD低、中、高三种浓度的提取回收率分别为108.0%,107.3%,102.6%,日内RSD4.41%~5.75%,日间RSD 1.32%~7.06%。结论:该方法准确,简单,快速,可用于OXC临床治疗的药物浓度监测和药物动力学的研究。
OBJECTIVE: To establish a reversed-phase high performance liquid chromatography (HPLC) method for the simultaneous determination of oxaliplatin (OXC) and its active metabolite-10-monohydroxy metabolite (MHD) in plasma. METHODS: Waters X-TerraTM RP_ (18) column (150 mm × 3.9 mm, 5 μm) was used. The column temperature was 35 ℃ and the flow rate was 1.2 ml · ml -1. The mobile phase consisted of methanol-0.1% trifluoroacetic acid 30:70), detection wavelength 232nm. Methaqualone as an internal standard, plasma samples by protein precipitation method directly after injection determination. Results: The linear range of OXC was 0.625 ~ 37.50μg · ml ~ 1 and the MHD was in the range of 1.25 ~ 75.0μg · ml ~ (-1). OXC low, medium and high concentration of three extraction recovery rates were 109.9%, 102.0%, 104.1%. Day RSD was 1.69% ~ 3.61%, and daytime RSD was 2.73% ~ 7.45%. The recovery rates of MHD with low, medium and high concentrations were 108.0%, 107.3% and 102.6% respectively, and the intraday RSD was between 4.41% and 5.75% Day RSD 1.32% ~ 7.06%. Conclusion: This method is accurate, simple and rapid and can be used to monitor drug concentration and pharmacokinetics in OXC clinical treatment.