利用超高效液相色谱-电喷雾三重四极杆质谱仪建立了中药中马兜铃酸A和B的定性定量分析方法.选取柴胡、生甘草、桔梗、龙胆泻肝丸、消胖丸、减肥茶等14种代表性样品,用甲醇-水(70∶30,v/v)溶液加热回流提取,经Oasis MAX固相萃取柱富集净化后,在Eclipse RP HD C18反相柱(150 mm×2.1 mm,1.8 μm)上进行分离;流动相为5 mmol/L乙酸铵水溶液(pH 7.5)-乙腈(75∶25,v/v).采用电喷雾离子源正离子模式(ESI+)和多反应监测模式(MRM)进行质谱分析.马兜铃酸A和B的线性范围分别为0.5～200 μg/L 和1～200 μg/L,相关系数(r2)均大于0.995;检出限(LODs)分别为5 μg/kg 和7.5 μg/kg;定量限(LOQs)分别为12.5 μg/kg 和25 μg/kg.在100 μg/kg 和500 μg/kg 添加水平下,马兜铃酸A和B的回收率(n=6)范围分别为60.3% ～96.4%和61.3% ～94.7%,相对标准偏差均不大于10.2%.该方法灵敏度高,重复性好,操作简便,适用于中药材、饮片及中成药中马兜铃酸A和B的痕量检测.
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