固本祛风颗粒中马兜铃酸Ⅰ的限量检查

Limit Detection of Aristolochic AcidⅠin Guben Qufeng Granules

目的:建立固本祛风颗粒中马兜铃酸Ⅰ的限量检查方法,保证临床用药安全。方法:采用高效液相色谱法。色谱柱为GL Inertsil ODS-SP(150mm×4.6mm,5μm),流动相为乙腈-0.05%磷酸(40∶60),流速为1mL·min-1,柱温为28℃,检测波长为320nm。结果:马兜铃酸Ⅰ的进样量在19.44～194.40ng范围内与峰面积积分值呈良好线性关系(r=0.9997);平均回收率为98.84%,RSD=0.90%(n=6);最低检测限为1.944ng。3批固本祛风颗粒中均未检出马兜铃酸Ⅰ。结论:该方法简便、专属性强、灵敏度高,可用于固本祛风颗粒中马兜铃酸Ⅰ的限量检查。

OBJECTIVE： To establish a method for the limit detection of aristolochic acid I in Guben qufeng granules and to guarantee the safety of drug use in the clinic. METHODS： HPLC method was adopted. The analytical column was GL Inertsil ODS-SP （150 mm×4.6 mm, 5μm） column with mobile phase consisted of acetonitrile-0.05%H3PO4（40：60） at the flow rate of 1 mL. min-1. The column temperature was set at 28℃ and the detection wavelength was at 320 nm. RESULTS： The Calibration curve was linear in the range of 19.44～194.40 ng （r=0.999 7） with an average recovery of 98.84% （RSD=0.90%, n=6）. The minimum limit of detection was 1.944 ng. In 3 batches of Guben qufeng granules, aristolochic acid I was undetectable. CONCLUSION： The method is simple, specific and sensitive, and it can be used for the limit detection of aristolochic acid I in Guben qufeng granules.