液相色谱-质谱联用法测定大鼠血浆中木通皂苷D的浓度  

Determination of aconitine in dog tissue homogenates by HPLC-MS/MS and its application to in vitro metabolic stability study

作　　者：吴诚[1] 李鹏飞[1] 王燕[1] 雷宁[1] 吕亚丽[1] 刘丽宏[1] 

机构地区：[1]第二炮兵总医院药剂科,北京100088

出　　处：《国际药学研究杂志》2012年第3期261-264,共4页Journal of International Pharmaceutical Research

摘　　要：目的建立液相色谱-质谱联用法(LC-MS/MS)测定大鼠血浆中木通皂苷D的浓度。方法选用XDB-C18色谱柱,以5 mmol/L乙酸铵水溶液(含0.1%甲酸)-甲醇溶液为流动相,采用梯度洗脱进行分离。样本经甲醇沉淀后进样,选用3200QTRAP型质谱仪的多重反应监测扫描方式进行检测。结果木通皂苷D线性范围为10～1000 ng/ml,最低定量限为10ng/ml。准确度与精密度结果显示方法日间、日内变异均小于15%,相对误差为-2.8%～4.6%,低、中、高3个浓度提取回收率为95.3%～108.1%。结论本研究所建立的方法快速、灵敏、专属性强、重现性好,可用于大鼠血浆中木通皂苷D浓度的测定和药代动力学研究。Objective To develop a LC-MS/MS method for the determination of the akebia saponin D in rat plasma. Methods After protein precipitation with methanol, the plasma sample was separated on a XDB-C1s column using 0. 1% ammonium acetate （ containning 0. 1% formic acid） water-methanol as mobile phase by gradient elution. Detection was carried out by multiple reaction monitoring on a 3200 QTrap LC-MS/MS system. Results The assay was linear over the range 10 - 1000 ng/ml with a lower limit of quantitation of 10 ng/m[. Intra- and inter-day precisions were less than 15% , respectively. The relative error was in the range -2. 8% -4. 6%. The recoveries of akebia saponin D were in the range of 95.3% - 108. 1%. Conclasion The LC-MS/MS method developed is rapid, sensitive, selective and reliable for the determination of akebia saponin D in rat plasma, and can be applied to the determination of akebia saponin D in rat plasma and the study on pharmacokinetics.

关 键 词：高效液相色谱-质谱联用法 木通皂苷D 药代动力学 

分 类 号：R285.5[医药卫生—中药学]