【摘要】 目的:建立一种用于同时检测大鼠血浆中没食子酸和芍药苷的准确、灵敏的超高液相色谱-串联质谱分析方法,并研究没食子酸、芍药苷在大鼠体内的药代动力学。方法:大鼠静脉注射赤芍提取物后,采用乙腈沉淀血浆蛋白,通过BEH C18(2.1 mm×50 mm,1.7μm)柱分离,0.1%甲酸乙腈-0.1%甲酸水梯度洗脱,流速0.35 mL·min-1,1μL进样分析,采用电喷雾离子化三重四极杆串联质谱,以多反应监测(MRM)方式进行负离子模式检测。用于定量分析的二级碎片离子分别为m/z169.0→125.0(没食子酸)和m/z 525.1→449.1(芍药苷)。结果:没食子酸、芍药苷分别在0.056~41.2 mg·L和0.36~265.1mg·L线性关系良好,日内、日间精密度(RSD)均<10.5%,低、中、高浓度下没食子酸的回收率分别为87.5%,103.3%,89.5%,芍药苷的回收率为88.5%,105.0%,107.4%。两种成分在大鼠体内的平均滞留时间均较短在37 min以内。结论:方法快速、专属性强、灵敏度高,适用于赤芍提取物的临床前药代动力学研究。更多还原

【Abstract】 Objective: To develop a sensitive and reliable ultra performance liquid chromatography tandem mass sepctrometry( UPLC-MS-MS) method for simultaneous determination and pharmacokinetics of gallic acid and paeoniflorin in rat plasma. Method: Following a protein precipitation with acetonitrile for plasma samples after iv Paeoniae Radix Rubra extract to rat. The analysis was achieved by BEH C 18( 2. 1 mm ×50 mm,1. 7 μm) column and the mobile phase was consisted of acetonitrile and water( both 0. 1% formic acid included) follow step gradient elution. A TQD tandem mass spectrometry equipped with electrospray ionization source was used as detector and operated by multiple reaction monitoring( MRM) negative ion mode of the transitions m / z 169. 0 → 125. 0,m / z 525. 1 →449. 1 for gallic acid and paeoniflorin,respectively. Result: Good linearity was achieved with concentration over the range of 0. 056-41. 2,0. 36-265. 1 mg·L- 1for gallic acid and paeoniflorin,the intraand inter-day precisions were lower than 10. 5%,while the low,mid and high concentration levels extraction recoveries were 87. 5%,103. 3%,89. 5%,and 88. 5%,105. 0%,107. 4% for gallic acid and paeoniflorin, respectively. The MRT of the two compounds were all blow 37 min in rats. Conclusion: The method was proved tobe suitable for the pharmacokinetics of Paeoniae Radix Rubra extract,which offers advantages of rapid,high sensitivity and selectivity.更多还原