高效液相色谱-质谱联用法同时测定减肥类保健品中12种非法添加物质

Simultaneous Determination of 12 Kinds of Chemicals Illegally Added Into the Weight Controlling Health Food by High Performance Liquid Chromatography-mass Spectrometry

建立高效液相色谱-质谱联用法同时测定减肥类保健品中非法添加的12种化合物的方法。样品采用乙腈超声提取,经Welch Xtimate C_(18)色谱柱(4.6mm×150mm,5μm)分离,以0.1%甲酸-5mmol/L乙酸铵水溶液(A)-乙腈(B)为流动相进行梯度洗脱,流速0.5mL/min,柱温30℃。质谱采用电喷雾离子源正/负离子模式将样品离子化,并用多反应监测模式对12种化合物进行测定。12种化合物在各自考察范围内线性良好,相关系数均大于0.9960;精密度和重复性的相对标准偏差分别为2.1%~6.5%、2.1%~6.3%;高、中、低3种添加浓度的平均回收率范围为77.3%~120.9%;检出限为0.012~1.121 ng/mL,定量限为0.060~2.687 ng/mL。该方法灵敏度高、操作简便、结果准确,可用于减肥类保健品中12种非法添加物的同时测定。

To establish a method to determinate 12 chemicals illegally added into the weight controlling health food simultaneously by high performance liquid chromatography-mass spectrometry(HPLC-MS).The samples were extracted with acetonitrile by ultrasonic processing and separated on a Welch Xtimate C_(18)(4.6mm×150 mm,5μm)column with 0.1%formic acid water solution(added 5 mmol/L ammonium acetate)(A)and acetonitrile(B)as the mobile phase by gradient elution at the flow rate of 0.5 mL/min,with the column temperature of 30℃.The samples were ionized by using positive/negative ion mode of electrospray ion source for mass spectrometry,and 12 compounds were determined by multi-reaction monitoring mode.The 12 compounds showed good linearity within their respective ranges,and the correlation coefficients were all greater than 0.9960.The relative standard deviations of precision and reproducibility were 2.1%~6.5%and 2.1%~6.3%,respectively.The average recoveries of the three additive concentrations of high,medium and low concentrations ranged from 77.3%to 120.9%.The limits of detection were 0.012~1.121 ng/mL and the limits of quantitation were 0.060~2.687 ng/mL.With the advantages of high sensitivity,simple operation and accurate results,the method can be used in simultaneous determination of 12 chemicals illegally added into the weight controlling health food.