液相色谱串联质谱法测定食品中淫羊藿苷等20种功能成分

采用超高效液相色谱—串联质谱仪建立了配制酒、饮料及代用茶中淫羊藿苷、金丝桃苷、补骨脂素等20种功能成分定量的检测方法。样品经甲醇—水溶液提取后,稀释净化,提取液离心,过滤,上机测定,Thermo Acclain RSLC C18(2.6μm,2.1mm×100mm)色谱柱进行分离,乙腈和水为流动相梯度洗脱,电喷雾正、负离子多反应监测扫描(MRM)模式下进行测定,外标法定量。20种化合物的线性检测范围最高浓度为500ng/mL,相关系数R2>0.99,定量限为0.5~5.0mg/kg,于1倍定量限、2倍定量限、10倍定量限3个添加水平下进行加标回收试验,20种化合物平均回收率为72.80%~107.75%,相对偏差>10%。该方法操作方便、简单、快捷、清洁、灵敏度高、重复性好。

Determination of icariin and other 20 functional components in food by liquid chromatography tandem mass spectrometry

A method for the quantitative determination of icariin,hypericin and Psoralen in mix liquor,beverage sample and tea substitutes were established by ultra-high-performance liquid chromatography tandem mass spectrometry.Samples were extracted by methanol water solution,diluted,purified,extracted,centrifuged,filtered,and determined by Thermo Acclain RSLC C18(2.6μm,2.1 mm×100 mm)chromatographic column.The determination was carried out under the mode of electrospray positive and negative ion multi-reaction monitoring scanning(MRM)with acetonitrile and water.The maximum linear detection concentration of 20 compounds was 500 ng/mL,the correlation coefficient(R2)was greater than 0.99,and the quantitative limit was 0.5~5.0 mg/kg.The recovery test of standard addition was carried out at three levels of 1,2 and 10 times limit of quantitation.The average recovery rate of 20 compounds was between 72.80% ~107.75%,and the relative deviation was less than10%.Conclusion:The method is easy to operate,simple,fast,clean,high sensitivity and good repeatability.