色谱

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高效液相色谱-二极管阵列检测法测定白首乌中的4种苯乙酮类成分

孙印石1,刘政波1,王建华1*,王迎2,周红英1,张文立1,王俊1,乔贵1   

  1. 1.College of Agronomy, Shandong Agricultural University, Taian 271018, China; 2.Taishan Academy of Forestry, Taian 271000, China
  • 收稿日期:2008-05-14 修回日期:2008-08-26 出版日期:2009-01-30 发布日期:1983-03-25
  • 通讯作者: 王建华
  • 基金资助:
    国家科技基础条件平台项目(2005DKA21000)、 泰安市中药现代化科技专项(5012100999)、 泰安市科技发展计划[2007]10和山东农业大学青年科技创新基金项目(23489)

Determination of four acetophenones in Radix Cynanchi bungei by high performance liquid chromatography-photodiode array detection

SUN Yinshi1, LIU Zhengbo1, WANG Jianhua1*, WANG Ying2, ZHOU Hongying1, ZHANG Wenli1, WANG Jun1, QIAO Gui1   

  1. 1.College of Agronomy, Shandong Agricultural University, Taian 271018, China; 2.Taishan Academy of Forestry, Taian 271000, China
  • Received:2008-05-14 Revised:2008-08-26 Online:2009-01-30 Published:1983-03-25
  • Contact: WANG Jianhua

摘要: 建立了白首乌中4种苯乙酮类化合物(Ⅰ:4-羟基苯乙酮,Ⅱ:2,5-二羟基苯乙酮,Ⅲ:白首乌二苯酮,Ⅳ:2,4-二羟基苯乙酮)的高效液相色谱检测方法。采用Symmetry-C18色谱柱(4.6 mm×250 mm,5 μm)分离,流动相为甲醇-水(体积比为26∶74),流速1.0 mL/min;采用二极管阵列检测器检测,化合物Ⅰ、Ⅲ、Ⅳ的检测波长为280 nm,化合物Ⅱ的检测波长为224 nm;测定温度为30 ℃。4种苯乙酮类化合物Ⅰ~Ⅳ的线性范围分别为0.080~0.560 μg,0.080~0.560 μg,0.100~0.700 μg和0.092~0.644 μg (r=0.9996~0.9999);平均加样回收率(n=3)为98.0%~104.0%,相对标准偏差为0.8%~2.6%。该方法简便快速、结果准确、重现性好,可作为白首乌药材质量控制的一个有效方法。

关键词: 白首乌 , 苯乙酮类化合物, 二极管阵列检测, 高效液相色谱

Abstract: A high performance liquid chromatographic (HPLC) method was developed for the determination of four acetophenones, namely 4-hydroxyacetophenone (Ⅰ), 2,5-dihydroxyacetophenone (Ⅱ), baishouwubenzophenone (Ⅲ) and 2,4-dihydroxyacetophenone (Ⅳ), in Radix Cynanchi bungei. The HPLC with photodiode array (PDA) detection was carried out on a Symmetry-C18 (4.6 mm×250 mm, 5 μm) column with CH3OH-H2O (26∶74, v/v) as the mobile phase at the flow rate of 1.0 mL/min and 30 ℃. The compounds Ⅰ, Ⅲ, Ⅳ were monitored at 280 nm, and the compound Ⅱ was at 224 nm. Four acetophenones (Ⅰ-Ⅳ) had good linearities (r=0.9996-0.9999) at the ranges of 0.080-0.560 μg, 0.080-0.560 μg, 0.100-0.700 μg and 0.092-0.644 μg, respectively. The average recoveries were from 98.0% to 104.0% with relative standard deviations (RSD) ranging from 0.8% to 2.6%. The method is of quick, simple and accurate. The method can be used for the quality control of this product

Key words: acetophenones, photodiode array detection, Radix Cynanchi bungei , high performance liquid chromatography (HPLC)