大鼠血浆中利培酮及9-羟基利培酮的LC-MS/MS法测定

Determination of Risperidone and 9-Hydroxyrisperidone in Rat Plasma by LC-MS/MS

建立了LC-MS/MS法测定大鼠血浆中的利培酮和9-羟基利培酮。用蛋白沉淀法处理血样,采用C18色谱柱,以0.1%甲酸溶液-甲醇(40:60)为流动相,盐酸苯海拉明为内标,使用多反应监测,检测离子对分别为m/z411.3→191.4(利培酮)、m/z427.2→207.1(9-羟基利培酮)和m/z256.2→167.3(苯海拉明)。利培酮和9-羟基利培酮在0.5～1000ng/ml范围内线性关系良好,批内、批间RSD均小于5%,回收率为90%～110%。

A LC-MS/MS method was established for the simultaneous determination of risperidone and 9-hydroxyrispeirdone in rat plasma. The plasma samples were treated by protein precipitation. A C^8 column was used with the mobile phase of 0.1% formic acid solution-methanol （40 ： 60） and diphenhydramine hydrochloride as the internal standard. A multiple reaction monitoring （MRM） mode was chosen for the detection of m/z 411.3→191.4 （risperidone）, m/z 427.2→207.1 （9-hydroxyrispeirdone） and m/z 256.2→167.3 （diphenhydramine）. The calibration curves of risperidone and 9-hydroxyrisperidone were linear in the concentration range of 0.5 - 1 000 ng/ml. The intra- and inter-batch RSDs were less than 5 % and the recoveries for three concentration levels were 90 % - 110 %.