反相高效液相色谱法测定抗癌原料药二氯二茂钛的含量

Determination of organometallic antitumor crude drug titanocene dichloride by reversed-phase high-performance liquid chromatography

目的建立了反相高效液相色谱法测定有机金属抗癌原料药二氯二茂钛的含量。方法采用Shimadzu VP-ODS色谱柱(250mm×4.6mm,5μm),V(甲醇):V(醋酸铵)=55:45,为流动相,流速为1.0ml/min,紫外检测波长254nm,室温检测,以氨基比林为内标进行测定。结果二氯二茂钛线性范围为10～140μg/ml,回归方程为f=0.0173c+0.0086,r=0.9994(n=8),方法精密度RSD为0.91%(n=6),重复性的RSD为0.82%(n=9)。结论方法简单快速,专属性强,可用于测定二氯二茂钛的含量。

Objective A method for the determination of a novel organometallic antitumor crude drug titanocene dichloride by reversed-phase high-performance liquid chromatography was established. Methods A Shimadzu VP-ODS column（ 250 mm × 4.6 mm,5 μm）was used. The mobile phase was consisted with methanol and ammonium acetate（55： 45, v/v） at a flow rate of 1.0 ml/min. The UV detction wavelength was set at 254nm and the column temperature was room temperature. Aminopyrine was select as an internal standard to determine. Results The linear range wae 10 - 140 μg/ml,and the regression equation was f = 0. 0173c ＋ 0. 0086, r = 0.9994 （ n = 8 ）. The RSD of precision was 0.91% （ n = 6 ） , and the RSD of reproducibility was 0. 82% （n = 9 ）. Conclusions The analytical method was simple, quick, accurate and seletive for the analysis of the content of novel organometallie antitumor crude drug titanocene dichloride.