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建立了液相色谱-串联质谱法拆分并测定大鼠血浆中SIPI6360的立体异构体。采用Daicel Chiralpak IA手性柱,以甲醇为流动相,采用ESI源正离子模式、多反应监测进行定量分析。结果显示,(R)-(+)-SIPI6360与(S)-(-)-SIPI6360立体异构体分离良好,在0.5~100 ng/ml浓度范围内线性关系良好。方法回收率为94.0%~102.8%,批内和批间RSD小于5.2%和11.4%。
A liquid chromatography-tandem mass spectrometry (LC-MS / MS) method was developed to separate and determine the stereoisomers of SIPI6360 in rat plasma. Daicel Chiralpak IA chiral column was used with methanol as the mobile phase, ESI source positive ion mode and multiple reaction monitoring. The results showed that (R) - (+) - SIPI6360 was well separated from the (S) - (-) - SIPI6360 stereoisomer and had a good linearity in the range of 0.5-100 ng / ml. The method recoveries ranged from 94.0% to 102.8%. Intra-assay and inter-assay RSD were less than 5.2% and 11.4%, respectively.