高效液相色谱法测定西罗莫司血药浓度

 目的　采用HPLC测定西罗莫司血药浓度。方法　色谱柱为Supelcosil LC-18 DB(4.6mm×250mm,5μm),甲醇-水(75∶25)为流动相,柱温50℃,流速1.0mL·min^-1,检测波长 276nm。结果　西罗莫司血药浓度在2.5～70ng·mL^-1范围内,浓度与峰面积比有良好的线性关系(r=0.9998),最低检测浓度为0.8ng·mL^-1。平均方法回收率为( 99.0±4.7)%(n=15)。日内RSD≤3.2%,日间RSD≤6.7%。结论　本方法简单、快速、准确,可用于西罗莫司的临床药动学研究。

Determination of sirolimus in human whole blood by HPLC

OBJECTIVE To establish a HPLC method to measure the concentration of sirolimus in whole blood.METHODS A Supelcosil LC 18DB column(4.6mm×250mm,5μm) was used and the temperature was set at 50℃.The mobile phase was a mixture of methanol and water (75∶25) and the flow rate was 1.0 mL·min^-1.The detection wavelength was at 276 nm.RESULTS The linear calibration curves were obtained over the range 2.5 ng·mL^-1 to 70 ng·mL ^-1 of sirolimus in blood (r=0.999 8).The limit of detection was 0.8 ng·mL^-1.The recovery of the assay was (99.0±4.7)%(n=15).The coefficients of variation within a day and between days did not exceed 3.2% and 6.7%,respectively.CONCLUSION This method appeared to be simple,convenient and precise for clinical pharmacokinetics study of sirolimus.