高效液相色谱-质谱法测定人血浆中双氯芬酸钾的浓度

Determination of diflofenac potassium in human plasma by HPLC-MS

目的 :建立一种用高效液相色谱 电喷雾离子化质谱联用技术测定双氯芬酸钾血药浓度的方法。方法 :以 0 .0 1mol·L-1 醋酸铵水溶液 甲醇 (2 8∶72 )为流动相 ,吉非罗齐为内标 ,血浆样品经醋酸乙腈沉淀蛋白后上清液上样 ,经C1 8柱分离后 ,以质谱为检测器 ,采用选择性离子检测 (SIM )测定人体血浆中双氯芬酸钾的浓度。结果 :线性范围 0 .0 2～ 5 .0mg·L-1 (r =0 .9992 ) ,平均相对回收率在 90 %～ 1 0 5 %之间 ,日内和日间精密度的RSD均小于 5 %,双氯芬酸钾的最低定量限为 0 .0 2mg·L-1 ,提取回收率大于 95 %。结论 :该方法快速、准确、灵敏 ,可用于双氯芬酸钾的药动学研究。

OBJECTIVE To establish an HPLC-ESI-MS method for determination of diflofenac potassium in human plasma.METHODS The mobile phase was composed of 0.01 mol·L -1 ammonium acetate/water-methanol(28∶72),gemfibrozil was used as internal standard. Plasma samples were precipitated with acetic acid/acetonitril and separated on C 18 column. The single quadrapole MS was used as detector. SIM was used for determination of diflofenac potassium in human plasma.RESULTS Standard curve was linear in the range of 0.02- 5.0 mg·L -1(r= 0.999 2),the relative recovery was between 90%-105%. RSD of intra-day and inter-day assays were all less than 5%. The quantitation limit was 0.02 mg·L -1. The extraction recovery was above 95%.CONCLUSION The method proves to be a stable and reliable for pharmacokinetic studies of diflofenac potassium.