目的:建立微波辅助提取、高效液相色谱同时测定山茱萸中马钱苷、獐芽菜苷及山茱萸新苷3种环烯醚萜苷的方法。方法:采用响应曲面法优化微波功率、提取溶剂以及料液比等提取条件;应用Agilent TC-C18柱分离,以水和乙腈为流动相梯度洗脱,流速1.0 mL/min,检测波长240 nm。结果:最佳微波提取工艺为:以体积分数72%的乙醇作溶剂,液料比15 mL/g,在微波功率400 W下提取10 min,连续提取两次;3个成分的高效液相色谱峰面积与浓度呈良好的线性关系(r〉0.9994),加样回收率分别为98.68%、98.24%和98.29%。结论:所建立的微波辅助提取高效液相色谱同时测定方法简便、准确、重现性好,可用于山茱萸药材中3种环烯醚萜苷的同时测定。
Objective:To establish a method of microwave-assisted extraction and high performance liquid chromatographic(HPLC) for simultaneous determination of three iridoid glycosides including loganin,sweroside and cornuside in Cornus officinalis.Methods:The extraction conditions of microwave power,ethanol concentration,liquid to sample ratio were optimized with a response surface methodology(RSM);Three constituents were separated on an Agilent TC-C18 column by gradient elution using acetonitrile and water as the mobile phase.The flow rate was 1.0 mL/min.The detection wave length was 240 nm.Results:The optimal conditions of microwave extraction were as follows:microwave power 400 W,ethanol concentration 72%,liquid to sample ratio 15 mL/g,the extraction time 10 min,the extraction times 2;The HPLC peak areas of all the constituents showed good linearity(r〉0.9994) in the range of the tested concentration,the average recoveries of the method were 98.68%,98.24% and 98.29%,respectively.Conclusions:The established method of microwave-assisted extraction and HPLC simultaneously determination has the advantages of convenient,precision and reliability.It can be used in simultaneous determination of three iridoid glycosides in Cornus officinalis.