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目的通过HPLC-SPD-ELSD串联系统比较、样品前处理及色谱条件的优化,测定保健食品中黄芪甲苷的量。方法采用以甲醇为提取溶剂对样品进行超声提取;选用色谱柱Thermo Accucore XL C8(150mm×4.6mm,4μm);流动相乙腈-水(32∶68);柱温35℃;体积流量1ml/min;紫外检测波长192nm;进样量20μl;漂移管温度40℃;氮气压力308kPa。结果黄芪甲苷在0.05~0.25mg/ml范围呈良好的线性关系,在ELSD和SPD结果分别为:r=0.999 8和r=0.999 2;方法检出限为0.02、0.04 mg/g;3批样品黄芪甲苷平均含量分别为1.06、1.03、1.05 mg/g和1.11、1.06、1.09mg/g;平均加样回收率96.80%和98.70%,RSD2.58%和2.91%(n=3)。结论该法便捷经济、准确可靠,可根据实际情况选择ELSD或SPD检测器,为保健食品中黄芪甲苷的质量控制与评价及相关研究提供了更全面的方法。
OBJECTIVE To determine the amount of Astragaloside in health food by HPLC-SPD-ELSD in-line system comparison, sample pretreatment and optimization of chromatographic conditions. Methods The samples were extracted with methanol as extraction solvent. The column was Thermo Accucore XL C8 (150mm × 4.6mm, 4μm). The mobile phase was acetonitrile-water (32:68). The column temperature was 35 ℃. The volume flow rate was 1ml / min ; UV detection wavelength 192nm; injection volume 20μl; drift tube temperature 40 ℃; nitrogen pressure 308kPa. Results Astragaloside had a good linear relationship in the range of 0.05-0.25 mg / ml. The results of ELSD and SPD were r = 0.999 8 and r = 0.999 2, respectively. The detection limits were 0.02,0.04 mg / g. The average content of astragaloside in samples was 1.06, 1.03, 1.05 mg / g and 1.11, 1.06, 1.09 mg / g, respectively. The average recoveries were 96.80% and 98.70%, RSD 2.58% and 2.91% (n = 3), respectively. Conclusion The method is convenient and economical, accurate and reliable. The ELSD or SPD detector can be selected according to the actual situation. It provides a more comprehensive method for the quality control and evaluation of astragaloside in health foods.