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目的:建立微量马兜铃酸A的标准检测方法,并对目前合法使用的含马兜铃酸A的药材、易与含马兜铃酸药材相混淆的中药材及其中成药进行检测。方法:采用高效液相色谱法,Alltima C18色谱柱(4.6 mm×250 mm,5μm),甲醇-水-乙酸(68∶32∶1.5)为流动相,流速1.0 mL.min-1,检测波长390 nm。结果:马兜铃酸A在0.016~0.51μg线性关系良好,r=0.999 3,最低检测限为4 ng,平均加样回收率为101.2%。采用建立的标准限量检测方法,对11批市售细辛药材和15批中成药样品中马兜铃酸A进行分析;11批细辛中马兜铃酸A的质量分数在3.1~26.6μg.g-1,其中只有3批符合《中国药典》2010年版细辛药材项下的限量规定;15批中成药样品中只有1批检出了马兜铃酸A。结论:方法灵敏度高,重复性好,适合于含痕量马兜铃酸的药材及成药中马兜铃酸A的限量检测。
OBJECTIVE: To establish a standard test method for trace aristolochic acid A. To detect the Chinese medicinal herbs and proprietary Chinese medicines which are currently legally used, which contain the aristolochic acid A, and which are easily confused with the aristolochic acid-containing medicinal materials. Methods: Alltima C18 column (4.6 mm × 250 mm, 5 μm) and methanol-water-acetic acid (68:32:1.5) were used as mobile phase at a flow rate of 1.0 mL · min- nm. Results: The linear range of aristolochic acid A was 0.016 ~ 0.51μg, r = 0.999 3, the lowest detection limit was 4 ng, and the average recovery was 101.2%. The established standard limit test method was used to analyze the contents of aristolochic acid A in 11 batches of asarum and 15 Chinese patent medicines. The mass fraction of aristolochic acid A in 11 batches was 3.1 ~ 26.6 μg. g-1, of which only 3 batches in line with the “Chinese Pharmacopoeia” 2010 edition of the Xinshinarin under the limited provisions; 15 batches of proprietary Chinese medicines in only one batch detected the aristolochic A. Conclusion: The method has high sensitivity and repeatability, and is suitable for the limited detection of aristolochic acid A in herbs and medicines containing traces of aristolochic acid.