高效液相色谱法测定人血浆中米托坦浓度

Determination of mitotane in human plasma by high performance liquid chromatography

目的建立测定人血浆中米托坦浓度的方法。方法以5%高氯酸为沉淀剂,血浆样本经蛋白沉淀处理,进高效液相分析,色谱柱:Shim-pak CLC-ODS(150×60 mm,5μm),流动相:水-乙腈=(15:85,v/v,磷酸调节pH至3.5),流速:1.0 mL·min^-1,柱温:35℃,紫外检测波长:230 nm。结果米托坦的标准曲线方程为y=1.800×10^-2 x-2.297×10^-3(r=0.999),线性范围为0.5~50μg·mL^-1。精密度在3.52%~7.00%之间,准确度在-8.63%~5.00%之间,平均提取回收率均大于70.69%,稳定性好。本方法灵敏度高,准确性好,简便快捷,适用于米托坦的血药浓度监测。

Objective To establish a method for the determination the concentration of mitotane in human plasma.Methods The clinical plasma samples were treated by protein precipitation using perchloric acid(5%)as a precipitant,and then were determined by high performance liquid chromatography.The separation was performed on a Shim-pak CLC-ODS(150×60 mm,5μm)at 35℃using water/acetonitrile(15∶85)(pH adjusted to 3.5 by H3 PO4)as mobile phase.The flow rate was 1.0 mL·min^-1 and the wavelength was 230 nm.Results The standard curve of mitotane was y=1.800×10^-2 x-2.297×10^-3(r2=0.999),the linear range was 0.5~50μg·mL^-1.The intra-run and inter-run RSDs were 3.52%~7.00%,the accuracy was-8.63%~5.00%,the average extraction recoveries were greater than 70.69%,and the stability was good.Conclusion The method was simple,sensitive and accurate,suitable for monitoring the concentrations of mitotane in human plasma.