快速溶剂萃取-电雾式检测器同时测定山楂及其炮制品中5种三萜酸类成分的含量

Simultaneous determination of five triterpenic acids in Crataegi Fructus by accelerated solvent extraction-charged aerosol detector

建立一种快速溶剂萃取-电雾式检测器(ASE-CAD)同时测定山楂及其炮制品中5种三萜酸类成分含量的方法.试验确定ASE萃取山楂的最优条件:以甲醇作溶剂,提取温度100℃,静态提取时间5 min,循环次数2次,提取池冲洗体积60%.HPLC方法:采用Thermo Acclaim C30(4.6 mm×250 mm,5μm)色谱柱,乙腈-1%乙酸铵为流动相,梯度洗脱,体积流量1.0 mL·min^(-1),柱温25℃,CAD雾化温度70℃,采集频率5 Hz,分别测定齐墩果酸、熊果酸、白桦脂酸、科罗索酸、山楂酸的含量.结果表明,齐墩果酸、白桦脂酸、科罗索酸、山楂酸的线性范围为5—75μg·mL^(-1),熊果酸的线性范围为5—250μg·mL^(-1);相关系数均不小于0.9970;平均回收率在88%—101%之间,RSD均小于5%.该方法准确、简便、重复性好,适用于山楂及其炮制品中齐墩果酸、熊果酸、白桦脂酸、科罗索酸、山楂酸的含量测定.

The objective of this paper is to establish a method for the simultaneous determination of five triterpenic acids in Crataegi Frucuts and its processed products by accelerate solvent extraction(ASE)-charged aerosol detector(CAD).The optimal extraction conditions were determined by the ASE test:methanol was used as solvent,ASE extraction temperature was 100℃,extraction time was 5 min and cycle time was 2.For the HPLC analysis,Thermo Acclaim C30(4.6 mm×250 mm,5μm)was employed,the mobile phase for the analysis pump was composed of acetonitrile-1%ammonium acetate in program of gradient elution,and the flow rate was 1.0 mL·min with oven temperature 25℃.The parameters applied for CAD are nebulizer temperature at 70℃and data rate at 5 Hz.The results showed that the calibration curves were linear over a concentration range of 5—75μg·mL^(-1) for oleanolic acid,betulinic acid,corosolic acid and maslinic acid,and 5—250μg·mL^(-1) for ursolic acid.The correlation coefficients were greater than 0.9970.The average recoveries were between 88%and 101%,with RSDs less than 5%.This method is accurate,simple and reproducible.It can be used for the determination of oleanolic acid,betulinic acid,corosolic acid,maslinic acid and ursolic acid in Crataegi Frucuts.