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作 者:祝坤赟 周成美 任鑫 李芳洁 胡晶红[1,2] 张永清 刘谦[1,2] ZHU Kun-yun;ZHOU Cheng-mei;REN Xin;LI Fang-jie;HU Jing-hong;ZHANG Yong-qing;LIU Qian(Shandong University of Traditional Chinese Medicine,Jinan 250355,China;Shandong Provincial Collaborative Innovation Center for Quality Control and TCM Whole Industry Chain Construction,Jinan 250355,China)
机构地区:[1]山东中医药大学,山东济南250355 [2]山东省质量控制与中药全产业链建设协同创新中心,山东济南250355
出 处:《中成药》2022年第7期2197-2201,共5页Chinese Traditional Patent Medicine
基 金:国家中医药管理局国家中药资源调查专项资金(GZY-KJS-2018-004);日照市重点研发计划项目(2021ZDYF010118);山东省高校中药质量控制与全产业链建设协同创新中心子课题(CYLXTCX2021-10)。
摘 要:目的 建立一测多评法同时测定蟾皮中华蟾酥毒基、日蟾毒它灵、蟾毒它灵、蟾毒灵、酯蟾毒配基、远华蟾蜍精、伪异沙蟾毒精的含量。方法 该药材甲醇提取液的分析采用Agilent ZORBAX SB-C_(18)色谱柱(250 mm×4.6 mm, 5μm);流动相乙腈-0.1%甲酸,梯度洗脱;体积流量1.0 mL/min;柱温30℃;检测波长296 nm。以华蟾酥毒基为内标,计算其他6种蟾毒内酯的相对校正因子,测定其含量。结果 7种蟾毒内酯在各自范围内线性关系良好(r≥0.999 0),平均加样回收率97.61%~100.83%,RSD 1.15%~2.69%,一测多评法与外标法所得结果接近。结论 该方法准确可靠,可用于蟾皮的质量控制。AIM To establish a quantitative analysis of multi-components by single-marker(QAMS)method for the simultaneous content determination of cinobufagin,gamabufalin,bufotaline,bufalin,resibufogenin,telocinobufagin and pseudobufarenogin in toad skin.METHODS The analysis of methanol extract of this medicinal material was performed on a 30℃thermostatic Agilent ZORBAX SB-C_(18) column(250 mm×4.6 mm,5μm),with the mobile phase comprising of water containing 0.1%formic acid-acetonitrile flowing at 1 mL/min in a gradient elution manner,and the detection wavelengths were set at 294 nm.cinobufagin was used as an internal standard to calculate the relative correction factors of the other six constituents,after which the content determination was made.RESULTS Seven constituents showed good linear relationships within their own ranges(r>0.9990),whose average recoveries were 97.52%-100.11%with the RSDs of 1.06%-2.20%.The result obtained by QAMS approximated those obtained by external standard method.CONCLUSION This stable and reliable method can be used for the quality control of toad skin.
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