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

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 C₁₈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R²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0.2²04.2 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。 

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

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 C₁₈ chromatographic column ( 2.1 mm × 100 mm, 1.8 μm) with acetonitrile and aqueous solution of 10 mmol/L ammonium acetate ( adjust to p H4.0 with formic acid) as mobile phase under gradient elution at a flow rate of 0.2 m L/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.