液质联用法同时测定保健食品中维生素E、维生素E乙酸酯和辅酶Q10

Detection of vitamin E,vitamin E acetate and coenzyme Q10 in health food by HPLC-MS/MS

目的采用高效液相色谱-串联质谱法(HPLC-MS/MS),建立保健食品中维生素E、维生素E乙酸酯和辅酶Q10的检测方法。方法样品经过乙腈超声提取(50℃),采用HPLC-MS/MS法进行检测。色谱条件:采用Agilent Eclipse-plus C18(2.1 mm×50 mm,1.8μm)色谱柱,流动相为乙醇-甲醇(含0.1%甲酸)溶液,梯度洗脱,流速为0.2 ml/min,柱温为35℃。质谱条件:电喷雾离子源(ESI+),干燥气温度为250℃,鞘气流速为11 L/min,源电压为4 kV,检测方式为多重反应监测(MRM)模式。结果维生素E、维生素E乙酸酯和辅酶Q10在相应的浓度范围内与峰面积都呈良好线性关系(r>0.99),加样回收率为78.1%~96.3%,精密度RSD<6%,方法检出限在0.008μg/g^0.15μg/g。结论此方法测定快速准确、灵敏度高,专属性强,可用于保健食品中维生素E、维生素E乙酸酯和辅酶Q10的检测。

Objective A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method was used to establish a method for the detection of vitamin E,vitamin E acetate and coenzyme Q10 in health foods.Methods The samples were ultrasonically extracted with acetonitrile(50 ℃) . HPLC analysis was performed on an Agilent Eclipse Plus C18 column(2.1 mm × 50 mm,1.8 μm).A gradient program was used with mobile phase consisting of ethanol and methanol(0.1% acetic acid) for gradient elution,the flow rate was 0.2 ml/min and the column temperature was set at 35 ℃ . MS/MS analysis was performed on electrospray ionization(ESI+) source.The capillary voltage was 4 k V,the gas flow rate was11 L/min and the gas temperature was set at 250 ℃ . Multiple reaction monitoring(MRM) mode was used for qualitative and quantitative detection.Results Good linearity of vitamin E,vitamin E acetate and coenzyme Q10 was obtained in their own concentration ranges(r>0.99).The recoveries were within 78.1%-96.3%,and the precision of RSD were<6%.Limits of detection were within 0.008 μg/g-0.15 μg/g.Conclusion The method is proved to be specific,sensitive and accurate.Therefore,it can be used to detect vitamin E,vitamin E acetate and coenzyme Q10 in health food.