HPLC-CAD分离测定山楂不同炮制品中熊果酸和齐墩果酸

Determination of isomeric ursolic acid and oleanolic acid in different processed products of Shanzha by HPLC-CAD

目的:建立HPLC-CAD法同时测定山楂不同炮制品,同分异构体熊果酸、齐墩果酸含量差异的方法。方法:色谱柱采用Thermo Scientific Accucore^(TM)C_(18)柱(100mm×3mm,2.6μm),以0.5%醋酸铵水(A)-乙腈(B)-甲醇(C)(21:61:18)为流动相,流速0.3mL·min^(-1),柱温25℃;电喷雾式检测器(CAD)参数:采集频10Hz,雾化温度35℃,滤波为10s。结果:熊果酸、齐墩果酸分别在0.0019~0.1196mg·mL^(-1)(r=0.9982)、0.0029~0.0920mg·mL^(-1)(r=0.9982)范围内线性关系良好,平均加样回收率分别为100.75%、98.95%,RSD值分别为2.91%、2.31%;且炒山楂中熊果酸、齐墩果酸的平均含量均较焦山楂、山楂炭的含量高。结论:建立的HPLC-CAD法可同时分离测定山楂不同炮制品中熊果酸、齐墩果酸含量,该方法稳定可靠,重现性好,为其检测分析和质量控制提供了新的方向。

Objective:To establish a method for simultaneously detecting the differences in the contents of isomeric ursolic acid and oleanolic acid in diferent processed products of Shanzha using HPLC-CAD.Method:A Thermo Scientifc AccucorerM Cis column(100 mmx3 mm,2.6μm)was used with 0.5%ammonium acetate water(A)-acetonitrile(B)-methanol(C)(21:61:18)as mobile phase,flow rate 0.3 mL·min^(-1),column temperature 25°C.The charged aerosol detector(CAD)parameters were as follows:10 Hz for sampling rate,35°C for the nebulizer temperature,and 5 s for filter.Result:Ursolic acid and oleanolic acid showed good linearity in the ranges of 0.0019~0.1196 mg·mL^(-1)(r-0.9982)and 0.0029~0.0920 mg·mL^(-1)(r-0.9982),respectively,with the average spiked recoveries of 100.75%and 98.95%.The RSD values were 2.91%and 2.31%,respectively.And the average contents of ursolic acid and oleanolic acid in fried Shanzha were higher than those in charred Shanzha and Shanzha charcoal.Conclusion:The established HPLC-CAD method can simultaneously separate and detect the contents of ursolic acid and oleanolic acid in different processed products of Shanzha.This method is stable,reliable,and exhibits good reproducibility,providing a new direction for the detection,analysis,and quality control of Shanzha.