高效液相色谱法测定杜仲壮骨丸中马兜铃酸A  

Determination of aristolochic acid A in Eucommia Ulmoides Strong Bone Pill by high performance liquid chromatography

作　　者：庞逸辉 李岳[1] 张宪[1] PANG Yihui;LI Yue;ZHANG Xian(Beijing Institute for Drug Control,NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine(Traditional Chinese Patent Medicine),Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing 102206,China)

机构地区：[1]北京市药品检验所,国家药品监督管理局中成药质量评价重点实验室,中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《化学分析计量》2022年第6期50-53,共4页Chemical Analysis And Meterage

摘　　要：建立反相高效液相色谱法测定杜仲壮骨丸中马兜铃酸A含量的方法。取50粒杜仲壮骨丸样品,碾细,称取样品粉末1.0 g至具塞锥形瓶中,加入40 mL甲醇溶液,称重并记录,超声40 min(功率为500 W,频率为40 kHz),冷却后再次称重,用甲醇溶液补足损失的重量,摇匀,用0.22μm过滤膜过滤,得样品溶液,采用Phenomenex Luna C_(18)色谱柱(4.6 mm×250 mm,5μm)为分离柱,流动相为水–甲醇溶液(体积比为1∶4),流量为1.0 mL/min,检测波长为315 nm,柱温为35℃。马兜铃酸A的质量浓度在0.0075~0.150μg/mL范围内与色谱峰面积线性关系良好,相关系数为0.9998,方法检出限为0.001μg/mL。测定结果的相对标准偏差为0.96%(n=6),样品加标平均回收率为99.27%。该方法专属性强,适用于杜仲壮骨丸中马兜铃酸A的含量测定及质量控制。The method for determining aristolochic acid A in Eucommia Ulmoides Strong Bone Pill by reversed phase high performance liquid chromatography was established.Took 50 samples of Eucommia Ulmoides Strong Bone Pill,ground them fine,1.0 g sample powder was weighed and put into a conical flask with a stopper,40 mL methanol solution was added in,weighed and recorded,and ultrasonication lasted for 40 min with the power of 500 W and the frequency of 40 kHz.Weighed again after cooling,made up the lost weight with methanol solution,shook well,and filtered with 0.22μm filter membrane to get the sample solution.The Phenomenex Luna C_(18) chromatographic column(4.6 mm×250 mm,5μm)was used as a separation column,the mobile phase was water–methanol solution(volume ratio was 1∶4)with the flow rate of 1.0 mL/min,the column temperature was 35℃,and the detection wavelength was 315 nm.The mass concentration of aristolochic acid A had a good linear relationship with the chromatographic peak area in the range of 0.0075–0.150μg/mL,the correlation coefficient was 0.9998,and the detection limit of the method was 0.001μg/mL.The relative standard deviation of determination results was 0.96%(n=6),and the average recovery of the samples was 99.27%.The method has strong specificity,and it is suitable for the determination and quality control of aristolochic acid A in Eucommia Ulmoides Strong Bone Pill.

关 键 词：杜仲壮骨丸 马兜铃酸A 高效液相色谱法 

分 类 号：O657.7[理学—分析化学]