高效液相色谱法测定大鼠血浆中的二氯二茂钛

Determination of titanocene dichloride in rat plasm by reversed-phase high-performance liquid chromatography

目的建立反相高效液相色谱法测定大鼠血浆中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(250×4.6mm,5m),V(甲醇)∶V(醋酸铵)=55∶45,pH2.5为流动相,流速为1.0ml/min,紫外检测波长254nm,柱温室温,氨基比林为内标进行测定。血浆中生物样品采用液-液萃取法进行提取。结果二氯二茂钛在大鼠血浆中的线性范围为10～120μg/ml,回归方程为Y=57.83X-0.6042(r=0.9991,n=7),方法精密度RSD为1.8%(n=6),平均回收率为RSD=1.63%(n=9)。结论方法简单快速,专属性强,可用于测定大鼠血浆中二氯二茂钛的含量,为该类药物的体内血药浓度检测和动力学研究提供了实验依据。

Objective A method for the determination of a novel organometallic antitumor crude drug titanocene dichloride in rat plasm by reversed-phase high-performance liquid chromatography was established. Methods A Shimadzu VP-ODS column （250 nun × 4. 6 nun,5 μm）was used. The mobile phase was consisted of methanol and ammonium acetate（55： 45, v/v） at a flow rate of 1.0 ml/min. The UV detction wavelength was set at 254 nm and the column temperature was room temperature. Aminopyrine was selected as an internal standard to determine. Samples of plasm were separated with liquid-liquid extraction method. Results The linear range of ti- tanocene dichloride in rat plasm was 10 - 120μg/ml, and the regression equation was Y = 57. 83X-0. 6042, （r = 0. 9991, n = 7）. The RSD of precision was 1.8% （ n = 6）, and the RSD of average reproducibility was 0. 63% （n = 9）. Conclusion The analytical method was simple, quick, accurate and seletive for the analysis of the content of novel organometallic antitumor crude drug titanocene dichloride in rat plasm. The study provides experimental evidence for detection of concentration of drug in plasm and kinetics study.