HPLC-ELSD法同时测定无梗五加果中3种3,4-裂环羽扇豆烷型三萜化合物的含量  

Simultaneous Determination of Three 3,4-seco-Lupane-type Triterpenoids in Acanthopanax Sessiliflorus Fruits by HPLC-ELSD

作　　者：吴高松[1] 王知斌[1] 杨春娟[1] 刘华[1] 王秋红[1] 杨炳友[1] 匡海学[1] 

机构地区：[1]黑龙江中医药大学,教育部北药基础与应用研究重点实验室/黑龙江省中药天然药物药效物质基础重点实验室,黑龙江哈尔滨150040

出　　处：《中医药信息》2017年第1期36-39,共4页Information on Traditional Chinese Medicine

基　　金：国家重点基础研究发展计划-973计划(No.2013CB531801);黑龙江中医药大学“优秀创新人才”支持项目(No.2012RCD05);黑龙江中医药大学“杰出人才培养”基金项目(No.2012cj02)

摘　　要：目的:建立HPLC-ELSD法同时测定无梗五加果中22-α-hydroxychiisanogenin(1)、chiisanogenin(2)和(1R,11α)1,4-epoxy-11-hydroxy-3,4-secolupane-20(30)-ene-3,28-dioic acid(3)的含量方法测定。方法:采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.2%(V/V)乙酸水溶液梯度洗脱,流速1.0 m L/min,柱温为25℃,使用蒸发光散射检测气(载气流速1.60 L/min,蒸发温度60℃,漂移管温度45℃)。结果:在70 min内,无梗五加果中上述3个成分完全分离,峰面积的对数与进样量的对数呈现良好的线性关系(r=0.999 5~0.999 7);平均加样回收率(n=6)分别为102.9%(RSD=1.9%)、95.4%(RSD=3.0%)、98.7%(RSD=2.3%)。样品中化合物1~3的含量分别为9.37~9.61、2.03~2.18、0.39~0.45 mg/g。结论:该方法简单、快速、结果可靠,可用于同时测定无梗五加果中化合物1~3的含量。Objective： To establish a high performance liquid chromatography -evaporative light scattering detection （ HPLC - EISD） method for the simultaneous determination of 22 - α- hydroxychiisanogenin （ 1 ）, chiisanogenin （ 2 ）, （ 1 R, 11 or） 1,4 - epoxy - 11 - hydroxy - 3, 4 -seeolupane - 20 （ 30 ） -ene - 3, 28 - dioic acid （3） in the Acanthopanax sessiliflorus fruits. Methods： The Diarnonsil C18 column （250 mm ×4.6 mm, 5 μm） was used,using gradient elution with a mobile phase of methanol as solvent A and 0. 2% （V/V） acetic acid in water as solvent B ; the flow rate was 1.0 mL/min ; the column temperature was maintained at 25℃. The ELSD conditions were as follows： the evaporative temperature was set at 60℃ ; the drift tube temperature was set at 45 ℃ ; the gas flow rate was 1.60 L/min. Results ： The three compounds were eompletely separated within 70 min. The regression equation showed a good liner relationship between logarithm of the peak area and logarithm of the content of each compound （ r = 0. 999 5 - 0. 999 7 ）. The average recoveries （n =6） were 102. 9% （ RSD = 1.9% ）, 95.4% （ RSD = 3.0% ） and 98.7% （ RSD = 2.3% ）, respectively. The contents of compounds 1 -3 in samples were 9.37 -9.61,2.03 -2. 18,0. 39 -0. 45 mg/g, respectively. Conclusion： The method is simple, fast and reliable, which can be used to determine the contents of compounds 1 -3 in A. sessiliflorus fruit.

关 键 词：无梗五加果 高效液相色谱—蒸发光散射检测 含量测定 

分 类 号：R284.1[医药卫生—中药学] O657.72[医药卫生—中医学]