【摘要】 目的 :建立人血浆中格拉司琼浓度的反相高效液相色谱测定方法。方法 :液 液萃取法分离纯化血浆样品 ,采用荧光检测器 ,以甲醇 磷酸盐缓冲液 (pH 2 .2 ,0 .0 2mol·L- 1含 3 .0 %三乙胺 ) ( 6 3∶3 7)为流动相 ,色谱柱为Shim PackCLC ODS柱( 150mm× 6 .0mm) ,并阐述了血浆中格拉司琼色谱峰形变和分裂的可能机理。结果 :格拉司琼色谱峰对称、不拖尾 ,萃取回收率达 92 % ,空白血浆和代谢物不干扰测定 ,血药浓度线性范围为 0 .5～ 6 0 .0 μg·mL- 1(r =0 .9995) ,最低检测限 0 .3 μg·mL- 1,方法回收率为 98.43 %～ 10 0 .4% ,日内RSD 2 .3 %～ 3 .8% ,日间RSD 2 .9%～ 4.6 %。结论 :此法简便、准确 ,灵敏度高 ,选择性好。更多还原

【Abstract】 OBJECTIVE HPLC method was developed for the determination of granisetron in human plasma.METHODS The method involved isolation of granisetron from plasma by liquid liquid extraction prior to reversed phase chromatographic separation on a Shim Pack CLC ODS column(150 mm× 6.0 mm) equilibrated with an eluent mixture constituted of CH 3OH pH 2.2 , 0.02 mol·L -1 phosphate buffer containing 3.0% triethylamine (63∶37). The detection was performed using fluorescence detector at 301 nm for excitation and 365 nm for emission. Additionally the probable mechanism of peak deformation for granisetron in plasma was elucidated.RESULTS Granisetron peak was sharp and symmetric. Extraction recovery of granisetron from plasma was proved to be as high as 92%. Linear responses were observed for granisetron concentration in plasma ranging from 0.5 to 60.0 μg·mL -1 . The limit of quantification for granisetron in plasma was 0.3 μg·mL -1 . Assay recovery was 98.43% ～ 100.4% . Precision, expressed as RSD, was in the range of 2.3% ～ 3.8% in the within day assay, and 2.9% ～ 4.6% in the between day assay, respectively.CONCLUSIONS The proposed method is simple, accurate, reproducible, and highly sensitive and selective.更多还原