RP-HPLC柱前衍生化法测定白舒非血药浓度

目的建立测定人血浆中白舒非浓度的柱前衍生高效液相色谱法。方法以1,5-戊二醇二甲磺酸酯为内标,血浆样品经二乙基二硫代氨基甲酸钠衍生化处理后,以乙腈-0.7%冰醋酸水溶液(69∶31)为流动相,流速1.0mL·min-1,采用XterraP18色谱柱分离,在280nm波长下进行检测。结果白舒非线性范围为0.20～4.00mg·L-1,以加权最小二乘法计算得到回归方程为Y=2.56X+16.7(r=0.9993,n=7),提取回收率81.01%～82.72%,方法回收率96.50%～97.90%,日内、日间精密度(RSD)均小于10%。最低血浆检测质量浓度为0.080mg·L-1。结论柱前衍生高效液相色谱法准确、灵敏,适用于白舒非血浆浓度的测定及其药代动力学研究。

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Objective To develop a pre-column derivatization high performance liquid chromatography for determination of the plasma busulfan concentration. Methods 1,5-diol dimethyl sulfonate was used as internal standard, and plasma samples were processed by derivatization with sodium diethyldithiocarbamate, with acetonitrile -0.7% acetic acid (69∶31) as mobile phase, flow rate of 1.0 mL·min-1, and separated by XterraRP18 column (5μm, 4.6 mm×250 mm), then detected at 280 nm wavelength. Results The linear range of Busulfan plasma concentration was 0.20～4.00 mg·L-1. Computing with the weighted least squares, the regression equation was Y=2.56X+16.7 (r=0.9993, n=7). The extraction recovery was 81.01%～82.72% and the method recovery was 96.50%～97.90%. The intra-and inter-day RSD were less than 10%. The detected minimum plasma concentration was 0.080 mg·L-1. Conclusion This pre-column derivatization high performance liquid chromatography is accurate, sensitive and suitable for determination of Busulfan plasma concentration and pharmacokinetic studies.