高效液相色谱-串联质谱法同时测定减肥类保健食品中27种违法添加化学药品

Simultaneous determination of 27 chemical drugs illegally added in slimming health food by high performance liquid chromatography-tandem mass spectrometry

目的:建立一种高效液相色谱-串联质谱(HPLC-MS/MS)同时测定减肥类保健食品中27种违法添加化学药品的方法。方法:采用Agilent Eclipse Plus C_(18)色谱柱(2.1 mm×100 mm,1.8μm),以10 mmol/L乙酸铵(用甲酸调节pH至4.0)溶液为流动相A,乙腈为流动相B,梯度洗脱,流速为0.2 m L/min。通过HPLC-MS/MS系统中多反应监测模式(MRM)对减肥类保健食品中27种违法添加化学药品进行定性和定量分析。结果:该方法线性R^2均大于0.99,精密度相对标准偏差小于8.0%,不同质量浓度样品平均回收率为74.5%~106.7%,检出限为0.2~204.2 ng/g。结论:此方法测定快速、准确、灵敏度高、分离度高,可用于减肥类保健食品中27种违法添加化学药品的检测。

Objective：To develop detection method for the simultaneous screening and confirmation of 27 illegally added in slimming health food using high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） .Methods：The chemical drugs were separated on an Agilent Eclipse Plus C-8 chromatographic column （2.1 mm x 100 mm, 1.8 p,m）with acetonitrile and aqueous solution of 10 mmol/L ammonium acetate （adjust to pH4.0 with formic acid）as mobile phase under gradient elution at a flow rate of 0.2 mL/min.The 27 illegally added in slimming health food were conducted qualitatively and quantitatively analysis by tandem mass spectrometry under multiple reaction monitoring（MRM） mode.Results：The method was linear with correlation coefficients （R2） which were not less than 0.99, and the precision expressed as relative standard deviations（RSDs） were not more than 8.0% .The recoveries of 27 drugs illegally added in slimming health food at different spiked concentrations ranged from 74.5% to 106.7% .The limits of detection （LODs）were in the range of 0.2-204.2 ng/g. Conclusion：This method is rapid,accurate and sensitive with a high degree of separation,and can be used for the detection of the 27 illegally added chemicals in slimming health foods.