YU Bin, LIANG Fang, HUANG Guang-yu, et al. LC-MS-MS Method for Determination of Oxyresveratrol in Bile of Rats[J]. Chinese journal of experimental traditional medical formulae, 2014, 20(21): 116-119.
DOI:
YU Bin, LIANG Fang, HUANG Guang-yu, et al. LC-MS-MS Method for Determination of Oxyresveratrol in Bile of Rats[J]. Chinese journal of experimental traditional medical formulae, 2014, 20(21): 116-119. DOI: 10.13422/j.cnki.syfjx.2014210116.
LC-MS-MS Method for Determination of Oxyresveratrol in Bile of Rats
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
1.8 μm)
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10 μL。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。
Abstract
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.
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