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目的:建立辛芩胶囊中马兜铃酸Ⅰ的SPE-HPLC限量检查法。方法:采用超声、固相萃取法对制剂中马兜铃酸Ⅰ进行提取纯化,HPLC法对其含量进行检测。色谱柱为Agilent Zorbax SB-C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-水-冰醋酸(60∶39∶1),体积流量1.0 mL/min,检测波长390 nm。结果:马兜铃酸Ⅰ在进样量2.632 9~105.314 ng浓度范围内线性关系良好(r=0.999 9)。检测限为2.6 ng,平均回收率100.7%,RSD=2.81%(n=9)。结论:该法简捷,结果准确可靠,可用于辛芩胶囊中马兜铃酸Ⅰ的限量检查。
Objective: To establish a SPE-HPLC method for the determination of aristolochic acid Ⅰ in Xinqin Capsules. Methods: Aristolochic acid and solid phase extraction were used to extract and purify aristolochic acid I. The content of aristolochic acid Ⅰ was determined by HPLC. The column was an Agilent Zorbax SB-C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase of methanol-water-glacial acetic acid (60:39:1), a volume flow rate of 1.0 mL / min and a detection wavelength of 390 nm. Results: Aristolochic acid Ⅰ had a good linear relationship (r = 0.999 9) within the range of 2.632 9 ~ 105.314 ng of injection volume. The detection limit was 2.6 ng with an average recovery of 100.7% and RSD = 2.81% (n = 9). Conclusion: The method is simple, accurate and reliable, and can be used for the limited quantity of aristolochic acid Ⅰ in Xinqin Capsules.