摘要
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 establish a method of content analysis of Astragaloside Ⅳ in health food by comparing the HPLC-PDA-ELSD series system and by optimizing the sample pretreatment conditions or HPLC conditions. MethodsThe sample was subjected to ultrasonic extraction with methanol as solvent.Thermo Accucore XL C8(150mm×4.6mm,4μm)column was used at 30 ℃.The mobile phase was acetonitrile-water(32:68)at at a flow rate of 1.0ml/min with the detection wavelength at 192 nm,the injection volume of 20μl.The temperature of drift tube was 40 ℃ with nitrogen as carrier gas with the flow rate of 308 kPa. Results There was a good linear relationship over a range of 0.05-0.25mg/ml for AstragalosideⅣ.The results in ELSD and SPD were:r=0.999 8and r=0.999 2;LOD 0.02mg/g and 0.04mg/g;the average content of Astragaloside Ⅳin three batches of samples were 1.06,1.03,1.05 mg/g and 1.11,1.06,1.09mg/g;the average recovery was 96.80% and 98.7%,RSD2.58% and 2.91%(n= 3),respectively. Conclusion The method is simple,convenient and economical,The results are accurate and reliable,and can choose ELSD or PDA detector according to the actual situation,so as to offer a more holistic approach to achieve the better quality control and evaluation of the products,or carry out related research.
出处
《预防医学论坛》
2016年第4期303-305,共3页
Preventive Medicine Tribune