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作 者:刘宗洋 赵文文[1] 武婧悦 吴霞[1] 陈筱清 昝珂[2] LIU Zong-yang;ZHAO Wen-wen;WU Jing-yue;WU Xia;CHEN Xiao-qing;ZAN Ke(Beijing Key Laboratory of Traditional Chinese Medicine Collateral Disease Theory Research, School of Traditional Chinese Medicine, Capital Medical University, Beijing 100069, China;National Institutes for Food and Drug Control, Beijing 100050, China)
机构地区:[1]首都医科大学 中医药学院 中医络病研究北京市重点实验室,北京100069 [2]中国食品药品检定研究院,北京100050
出 处:《中国中药杂志》2018年第8期1662-1666,共5页China Journal of Chinese Materia Medica
基 金:国家自然科学基金项目(81403183);北京市教育委员会科技发展计划一般项目(KM201810025017)
摘 要:建立山绿茶中海南冬青皂苷D、冬青皂苷A1、3β,19α-dihydroxyolean-12-ene-24,28-dioic acid(命名为ilexhainanin E)、冬青素A、齐墩果酸、熊果酸等3对齐墩果烷型、乌苏烷型三萜同分异构体HPLC-ELSD含量测定方法,用于指导山绿茶药材的质量控制。以6种三萜成分为对照品,采用Waters XBridge C(18)色谱柱(4.6 mm×250 mm,5μm),甲醇(A)-0.5%甲酸水溶液(B)为流动相,梯度洗脱(0~18 min,70%~85%A;18~20 min,85%~95%A;20~35 min,95%A),流速1.0 m L·min^-1;柱温30℃;ELSD漂移管70℃,载气为N2,流速2.8 L·min^-1。进样量10μL。6批山绿茶药材中海南冬青皂苷D、冬青皂苷A1、ilexhainanin E、冬青素A、齐墩果酸、熊果酸质量分数分别为3.7~8.5,10.3~22.1,2.8~5.9,7.8~14.1,2.6~3.8,8.8~11.9 mg·g^-1。该研究可用于山绿茶药材中三萜成分的含量测定,为该药材质量标准的完善提供参考。The present study is to develop an HPLC-ELSD method for simultaneous determination of three pairs of triterpenoid isomers,Ilexsaponin A)1,Ilexhainanoside D,Ilexgenin A,3β,19α-dihydroxyolean-12-ene-24,28-dioic acid( ilexhainanin E) ursolic acid and oleanic acid in the leaf of Ilex hainanensis,which could provide evidence to the quality control of this herb. The six constituents were measured on a Waters XBridge C(18) column( 4. 6 mm × 250 mm,5 μm),with a mobile phase consisting of methanol( A)-0. 5% formic acid in water( B) at a flow rate of 1. 0 m L·min^-1( 0-18 min,70%-85% A,18-20 min,85%-95% A; 20-35 min,95%A). The carrier gas was N2,and the pressure was 2. 8 L·min^-1. The drift tube in this experiment were set at 70 ℃. The injection volume was 10 Μl. The contents of the six triterpenoids in 6 samples were 3. 7-8. 5,10. 3-22. 1,2. 8-5. 9,7. 8-14. 1,2. 6-3. 8 and 8. 8-11. 9 mg·g^-1,respectively. The established method is proved to be accurate and sensitive for the determination of triterpenoids in Ilicis Hainanensis Folium,and may be used for the quality improvement of this herb.
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