高效液相色谱-质谱联用法测定人血浆中奥昔布宁的浓度

Determination of oxybutynin 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奥昔布宁血药浓度的方法。方法 以 0 .0 1mol/L乙酸铵水溶液 甲醇 ( 15∶85 )为流动相 ,盐酸非洛普为内标 ,血浆样品经用环己烷萃取后上样 ,经C18柱分离后 ,以质谱为检测器 ,采用选择性离子检测 (SIM)测定人体血浆中奥昔布宁的浓度。结果 线性范围 0 .2～ 5 0ng/mL(r=0 .994 8) ,平均相对回收率在 90 %～ 110 %之间 ,日内和日间精密度的RSD均小于 10 % ,奥昔布宁的定量限为 0 .2ng/mL ,提取回收率大于 90 %。 结论 该方法快速、准确、灵敏 ,可用于奥昔布宁的药代动力学研究。

OBJECTIVE To develop a HPLC ESI MS method for determination of oxybutynin in human plasma. METHOD The mobile phase was composed of 0.01mol/L ammonium acetate/water: methanol(15:85),phenoprolamine hydrochloride was used as internal standard. Plasma samples were extracted with cyclohexane and separated by C 18 column. The single quadrapole MS was used as detector. SIM was used for determination of oxybutynin in human plasma.RESULTS Standard curve was linear in the range of 0.2 to 50 ng/mL( r =0.9948),the relative recovery was between 90%～110%. RSD of intra day and inter day assays were all less than 10%. The limit of detection was 0.2ng/mL. The extraction recovery was more than 90%.CONCLUSION The method developed is stable and reliable for determination of oxybutynin in human plasma as well as for pharmacokinetic studies.