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作 者:张丽先[1,2] 李红伟 宁二娟[1,2] 李自红 范毅[1,2] 魏悦 张桃桃[1,2] ZHANG Li-xian;LI Hong-wei;NING Er-juan;LI Zi-hong;FAN Yi;WEI Yue;ZHANG Tao-tao(Analysis Department of Biological Technology Development Center of Henan Province,Zhengzhou 450002,China;Henan Cogo Testing and International Standardizing Technology Co.,Ltd.,Zhengzhou 450002,China;College of Pharmacy,Henan University of Chinese Traditional Medicine,Zhengzhou 450046,China)
机构地区:[1]河南省生物技术开发中心,郑州450002 [2]河南科高中标检测技术有限公司,郑州450002 [3]河南中医药大学药学院,郑州450046
出 处:《中国新药杂志》2018年第20期2442-2446,共5页Chinese Journal of New Drugs
基 金:河南中医学院博士科研基金资助项目(BSJJ2012-04);河南省科技攻关资助项目(162102310345)
摘 要:目的:建立高效液相法同时测定南葶苈子生品及清炒品中槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷和芥子碱硫氰酸盐含量方法,并对比清炒前后2种成分含量变化。方法:采用NUCLEODUR Pyramid C18色谱柱(250 mm×4. 6 mm,5μm);以乙腈-0. 01 mol·L-1KH2PO4水溶液为流动相,梯度洗脱;流速1. 0m L·min-1;柱温30℃;检测波长254 nm。结果:在选定的色谱条件下,槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷和芥子碱硫氰酸盐分离度良好,槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷线性范围为4. 24~50. 88μg·m L-1,芥子碱硫氰酸盐线性范围为25. 96~311. 04μg·m L-1;平均回收率分别为99. 37%,98. 06%; RSD均小于2. 63%。结论:该方法准确、简便,能够同时测定南葶苈子生品及清炒品中槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷和芥子碱硫氰酸盐含量。Objective: An HPLC method was firstly established for simultaneous determination of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobiosiden and sinapine thiocyanate in Semen Descurainiae,and the content of two components in crude and processed Lepidii Semen were compared. Methods: Analysis was performed on a NUCLEODUR C18 column( 250 mm × 4. 6 mm,5 μm). The mobile phase was acetonitrile and 0. 01 mol·L-1 KH2 PO4 solution,the flow rate was set at 1. 0 m L·min-1,the column temperature was maintained at 30 ℃,and the detected wavelength was 254 nm. Results: Under the selected chromatographic conditions,two substances were separated effectively. Quercetin-3-O-β-D-glucose-7-O-β-D-gentiobiosiden and sinapine thiocyanate had good linearity over the range of 4. 24 ~ 50. 88 and 25. 96 ~ 311. 04 μg·m L-1,respectively. The average recoveries were99. 37% and 98. 06%,and RSDs were all below 2. 63%. Conclusion: The method established is accurate and rapid,which can be used for simultaneous determination of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobiosiden andsinapine thiocyanate in Semen Descurainiae.
关 键 词:南葶苈子 高效液相色谱法 槲皮素-3-O-β-D-葡萄糖-7-O-β-D-龙胆双糖苷 芥子碱硫氰酸盐 含量测定
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