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目的建立反相高效液相色谱法用于测定大鼠胰腺、肝脏、脾脏、肾脏、肺脏、心脏、腹直肌组织中吉西他滨的含量。方法采用phenomenex色谱柱,5-溴尿嘧啶为内标,流动相为乙腈-0.1%三氟乙酸溶液(3∶97,V/V),流速1.0 mL.min-1,检测波长268 nm,柱温45℃。组织样品经甲醇-乙腈(1∶9,V/V)蛋白沉淀处理后,55℃恒温水浴中氮气吹干,经流动相溶解后进样,进样量50μL。结果大鼠各脏器组织中吉西他滨在浓度1~100 mg.L-1内线性关系良好,方法回收率为93%~104%,提取回收率>70%,日内、日间RSD均<6%。结论本方法操作简单,重现性好,可用于大鼠多种组织中吉西他滨的含量测定。
Objective To establish an RP-HPLC method for the determination of gemcitabine in rat pancreas, liver, spleen, kidney, lung, heart and rectus abdominis. Methods The phenomenex column was used with 5-bromouracil as internal standard. The mobile phase consisted of acetonitrile-0.1% trifluoroacetic acid solution (3:97 V / V) at a flow rate of 1.0 mL · min- Temperature 45 ℃. Tissue samples were precipitated by methanol-acetonitrile (1: 9, V / V) protein and then dried in a constant temperature water bath at 55 ° C. After the sample was dissolved in the mobile phase, the sample was injected in an amount of 50 μL. Results The gemcitabine in various tissues of rats showed a good linearity in the range of 1 to 100 mg · L-1. The recovery rate was 93% -104% and the recovery rate was> 70%. The RSDs were both 6% . Conclusion The method is simple, reproducible, and can be used for the determination of gemcitabine in various tissues of rats.