固相萃取-高效液相色谱法测定排石颗粒中马兜铃酸A的含量

Determination aristolochic acid A inPaishi granule by SPE-HPLC

目的 建立排石颗粒中马兜铃酸A的限量检测方法.方法 样品经固相萃取小柱进行处理,采用高效液相色谱法,色谱柱为Phenomenex Luna C18柱（4.6 mm×250 mm,5μm）,以乙腈-0.2%碳酸铵溶液（稀盐酸调节pH值为7.5）为流动相,采用梯度洗脱,流速1.0 ml/min,柱温35℃,检测波长250 nm.结果马兜铃酸A在0.029～0.580μg/ml浓度范围内有良好线性关系（r=0.999 9）,检测限（S/N=3）为0.9 ng/ml,定量限（S/N=10）为3.0 ng/ml,平均加样回收率为96.4%.结论本方法灵敏度高、准确、重复性好、专属性强,可用于排石颗粒中马兜铃酸A的限量测定.

Objective To establish a method for the determination of aristolochic acid A inPaishi granule.Methods The HPLC system consisted of the Phenomenex Luna C18（4.6 mm×250 mm, 5μm）column, the mobile phase consisted of acetonitrile and 0.01% HAc, gradient elution flow rate was 1.0 ml/min, the column temperature was 35℃, The UV detector was set at 250 nm.Results The linear response range was 0.029-0.580μg/ml （r=0.999 9）. The detection limit and quantitation limit of aristolochic acid A inPaishi granule were 0.9 and 3.0 ng/ml. The average recovery of aristolochic acid A was 96.4%.Conclusion The method is high sensitivity, accurate, repeatable and high specificity,and can be used as an inspection method for safe use of Paishi granule.