高效液相色谱法测定杜仲壮骨丸中马兜铃酸A
庞逸辉，李岳，张宪
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
Determination of aristolochic acid A in Eucommia Ulmoides Strong Bone Pill by high performance liquid chromatography
PANG Yihui, LI Yue, ZHANG Xian
Beijing Institute for Drug Control, NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine (Traditional Chinese PatentMedicine), Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine, Beijing 102206, China
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 18 长为315 nm，柱温为35℃。马兜铃酸A的质量浓度在0.007 5～0.150μg/mL范围内与色谱峰面积线性关系良好，相关系数为0.999 8，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。
Abstract：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 chromatographic column(4.6 mm×250 mm, 5μm) 18 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 0.007 5-0.150μg/mL, the correlation coefficient was 0.999 8, 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
Keywords：Eucommia Ulmoides Strong Bone Pill; aristolochic acid A; high performance liquid chromatography
本文引用格式：
庞逸辉，李岳，张宪.高效液相色谱法测定杜仲壮骨丸中马兜铃酸A[J].化学分析计量，2022，31(6)：50.
PANG Yihui，LI Yue，ZHANG Xian. Determination of aristolochic acid A in Eucommia Ulmoides Strong Bone Pill by high performance liquid chromatography[J]. Chemical Analysis and Meterage，2022，31(6)：50.
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