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目的:研究跳骨片中马兜铃酸A的限量测定方法。方法:色谱柱为Shimpack Vp-ods(4.6mm×15cm)C18柱,流动相为:甲醇-1%冰醋酸(51∶49);流速:1.0mL/min,检测波长为260nm。结果:进样量在20.04~1 282.5ng范围内与峰面积呈良好线性关系(r=0.999 98);平均回收率为98.50%,RSD为0.74%(n=6)。经HPLC含量测定,其马兜铃酸A的含量极低(2~20μg·g-1)。对10批成品进行检测,其含量均小于20ppm,参照ICH对氯仿残留的限定,浓度限定<60ppm,PED<0.6mg/d,本产品马兜铃酸A含量低于该限度。结论:该法简便准确,结果可靠,可用于测定跳骨片中马兜铃酸A的限量。
Objective: To study the method for the determination of aristolochic acid A in Jiao Gulian tablets. METHODS: The column was a Shimpack Vp-ods (4.6 mm × 15 cm) C18 column with a mobile phase of methanol-1% glacial acetic acid (51:49), a flow rate of 1.0 mL / min and a detection wavelength of 260 nm. Results: There was a good linear relationship between the injection volume and peak area in the range of 20.04-1 282.5 ng (r = 0.999 98). The average recovery was 98.50% and the RSD was 0.74% (n = 6). The content of aristolochic acid A was very low (2 ~ 20μg · g-1) as determined by HPLC. 10 batches of finished products were tested, the content of less than 20ppm, refer to ICH of chloroform residue limits, the concentration limit <60ppm, PED <0.6mg / d, the product of aristolochic acid A content below this limit. Conclusion: The method is simple and accurate, the results are reliable, and can be used to determine the limit of aristolochic acid A in Jiao Gou tablets.