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

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

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（4．6mm×250mm，5μm）分离，流动相为甲醇-水（体积比为26：74），流速1．0mL／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280nm，化合物Ⅱ的检测波长为224nm；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0．080～0．560μg，0．080～0．560μg，0．100～0．700μg和0．092～0．644μg（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。

A high performance liquid chromatographic （HPLC） method was developed for the determination of four acetophenones, namely 4-hydroxyacetophenone （ Ⅰ ）, 2,5-dihydroxyace- tophenone （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-H20 （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 Ⅱwas at 224 nm. Four acetophenones （ Ⅰ- Ⅳ） had good linearities （ r = 0. 999 6 - 0. 999 9） at the ranges of 0. 080 - 0. 560 μg, 0. 080 - 0. 560 μg, 0. 100 - 0. 700μg 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.