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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×50 mm,1.8μm),流动相为乙腈-0.2%甲酸水,以40∶60等度洗脱,流速为0.4 mL·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700 L·h-1。气体流速10 L·min-1,毛细管电压3.0 kV,锥孔电压27 V,离子源温度100℃,结果:给药后0.5~1 h胆汁中的药物排泄量最高,12 h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: Oxidation of resveratrol has significant pharmacological activity and its metabolism in the body is helpful for the clinical development and utilization. Methods: The rat bile samples were pretreated by liquid-liquid extraction and established by liquid chromatography-mass spectrometry (LC-MS-MS) with carbamazepine as internal standard. The Agilent ZORBAX SB-C18 column (2.1 mm × 50 mm, 1.8 μm) was used. The mobile phase consisted of acetonitrile-0.2% formic acid water and wasocratically eluted at 40:60 with a flow rate of 0.4 mL · min-1 at 35 ℃ , The injection volume of 10μL. MS measurement conditions: electrospray ionization ESI +, MS detection mode MRM. Desolvation gas is high purity nitrogen, desolvation gas temperature 350 ℃, desolvation gas flow rate 700 L · h-1. Gas flow rate was 10 L · min-1, capillary voltage was 3.0 kV, cone voltage was 27 V and ion source temperature was 100 ℃. The results showed that the drug excretion in bile was the highest at 0.5-1 h after administration, and was almost completely excreted after 12 h. CONCLUSION: This method is time-consuming (only 3 min for each sample), with high specificity and accuracy and precision to meet in vivo drug analysis requirements.