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作 者:符必述 魏谭军[1] 王丽[1] 罗健华[1] 杨芝芳 陈飞 肖成[1] FU Bishu;WEI Tanjun;WANG Li;LUO Jianhua;YANG Zhifang;CHEN Fei;XIAO Cheng(Dazhou Hospital of Integrated TCM&WM,Dazhou 635000,China)
机构地区:[1]达州市中西医结合医院药学部,四川达州635000
出 处:《药学与临床研究》2021年第5期351-354,共4页Pharmaceutical and Clinical Research
基 金:四川省重大科技专项项目(2020YFS0533);达州市重点研发计划项目(20ZDYF0007)。
摘 要:目的:建立高效液相色谱一测多评法测定神术合剂中白术内酯Ⅱ、苍术素、柚皮芸香苷、橙皮苷、川陈皮素、橘红素、广藿香酮的含量。方法:采用Agilent Eclipse C18色谱柱(250 mm×4.6 mm,5μm),柱温25℃;乙腈-0.1%磷酸水溶液为流动相,流速0.8 mL·min^(-1);检测波长分别为270 nm(白术内酯Ⅱ和苍术素)和310 nm(柚皮芸香苷、橙皮苷、川陈皮素、橘红素和广藿香酮);以橙皮苷为内参物,建立与其它6种成分的相对校正因子,计算各成分含量。结果:白术内酯Ⅱ、苍术素、柚皮芸香苷、橙皮苷、川陈皮素、橘红素、广藿香酮分别在2.37~59.25、5.28~132.00、4.69~117.25、5.86~146.50、1.47~36.75、0.74~18.50、0.56~14.00μg·mL-1(r≥0.9991)范围内线性关系良好;平均加样回收率(RSD)分别为98.45%(1.29%)、100.05%(0.68%)、98.58%(1.80%)、99.05%(1.54%)、97.60%(1.51%)、96.98%(0.88%)、97.31%(1.03%);神术合剂中7个成分一测多评法计算结果与外标法实测值间无明显差异。结论:本方法操作便捷、专属性强,稳定性和重复性好,能够同时测定神术合剂中广藿香酮等7个成分含量,可用于神术合剂的质量控制。Objective:To establish an HPLC-QAMS method for the determination of atracylenolideⅡ,atractylodin,narirutin,hesperidin,nobiletin,tangeretin and pogostone in Shenzhu Mixtures.Methods:The method was performed on a column of Agilent Eclipse C_(18)(250 mm×4.6 mm,5μm),with a mobile phase consisting of acetonitrile-0.1%phosphoric acid solution flowing at 0.8 mL·min^(-1).The column temperature was 25℃.The detection wavelengths were set at 270 nm for atracylenolideⅡand atractylodin,310 nm for narirutin,hesperidin,nobiletin,tangeretin and pogostone.Using hesperidin as an internal standard,the relative correction factors of the other six constituents were calculated for content determination.Results:AtracylenolideⅡ,atractylodin,narirutin,hesperidin,nobiletin,tangeretin and pogostone showed good linear relationships within the ranges of 2.37-59.25,5.28-132.00,4.69-117.25,5.86-146.50,1.47-36.75,0.74-18.50 and 0.56-14.00μg·mL-1(r≥0.9991),whose average recoveries(RSDs)were 98.45%(1.29%),100.05%(0.68%),98.58%(1.80%),99.05%(1.54%),97.60%(1.51%),96.98%(0.88%)and 97.31%(1.03%),respectively.The contents of the seven components in Shenzhu Mixtures showed no significant difference between the data measured by the external standard method and the data calculated by the QAMS method.Conclusion:The established HPLC-QAMS method is simple,highly specific,stable and repeatable,which can simultaneously determine the contents of atracylenolideⅡ,atractylodin,narirutin,hesperidin,nobiletin,tangeretin and pogostone,and can be used for quality control of Shenzhu Mixtures.
关 键 词:高效液相色谱一测多评法 神术合剂 相对校正因子 白术内酯Ⅱ 苍术素 柚皮芸香苷 橙皮苷 川陈皮素 橘红素 广藿香酮
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