LC-MS-MS研究氧化白藜芦醇在大鼠胆汁中的代谢

LC-MS-MS Method for Determination of Oxyresveratrol in Bile of Rats

目的：氧化白藜芦醇药理活性显著,研究其在体内的代谢过程有助于临床的开发利用.方法：采用液液萃取法对大鼠胆汁样品进行预处理,建立以卡马西平为内标的液相色谱-质谱联用（LC-MS-MS）检测方法.Agilent ZORBAX SB-C18色谱柱（2.1 mm×50mm,1.8 μm）,流动相为乙腈-0.2％甲酸水,以40∶60等度洗脱,流速为0.4mL· min-1,温度为35℃,进样量为10μL.MS测定条件：采用电喷雾离子源ESI＋,MS检测模式为MRM.脱溶剂气为高纯氮气,脱溶剂气温度350℃,脱溶剂气流速700L·h-1.气体流速10L·min-1,毛细管电压3.0kV,锥孔电压27V,离子源温度100℃,结果：给药后0.5-1h胆汁中的药物排泄量最高,12h基本排泄完.结论：该方法耗时短（每个样品仅用3 min）,专属性强,且准确度和精密度均可满足体内药物分析的要求.

Objective：An sensitive and selective liquid chromatography-tandem mass spectrometry （LC-MS-MS） method was developed and validated for the determination of oxyresveratrol in rat bile.Method：The analyte and the internal standard （carbamazepine） were extracted from bile samples using simple liquid-liquid extraction technique with ethyl acetate,seperated on a ZORBAX SB-C18 column （2.1 mm × 50 mm,1.8 μm） with mobile phase of acetonitrile and water containing 0.2％ formic acid.Detected by triple quadruple mass spectrometry with an positive electrosprayionization interface,and quantified using multiple reaction monitoring （MRM） mode.A guard column was used and the flow rate was 0.4 mL ·min-1 Result：It showed the highest biliary excretion at 0.5-1 h after administration.The biliary excretion rate of oxyresveratrol was 0.737％ within 12 hours.Conclusion：This analytical method is rapid （3 min for each sample）,selective,precise,accurate,and reliable for in vivo analysis of oxyresveratrol.