液相色谱-串联质谱法快速检测速冻调制食品中7种甜味剂与防腐剂含量

Rapid determination of 7 kinds of sweeteners and preservatives content in quick-frozen prepared food by liquid chromatogram-tandem mass spectrometry

目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectroscopy,LC-MS/MS)快速检测速冻调制食品中7种甜味剂与防腐剂的分析方法。方法采用Phenomenex Kinetex F5色谱柱(50 mm×2.1 mm,2.6μm),以0.05%甲酸-10 mmol/L乙酸铵和乙腈进行梯度洗脱,电喷雾离子源(electrospray ionization,ESI)负离子模式、多反应监测(multiple reaction monitoring,MRM)模式进行测定。结果在0.01~0.20 mg/kg质量浓度范围内,目标物的线性关系良好,相关系数均大于0.99,方法检出限(S/N=3)为0.01~0.10 mg/kg;在不同添加浓度(1.0、2.0、10.0 mg/kg)下,其回收率为81.2%~105.3%、相对标准偏差均不大于10%。结论该方法具有操作简便、快速、准确、灵敏等优点,可满足速冻调制食品中7种甜味剂与防腐剂的定性定量分析,为速冻调制食品中防腐剂与甜味剂的快速筛查和风险分析奠定基础。

Objective To establish an analytical method for rapid detection of 7 kinds of sweeteners and preservatives in quick-frozen prepared foods by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods Used Phenomenex Kinetex F5 column(50 mm×2.1 mm,2.6μm),and performed the gradient elution with 0.05%formic acid-10 mmol/L ammonium acetate and acetonitrile.Used the electrospray ionization(ESI)negative ion mode and multiple reaction monitoring(MRM)mode for detection.Results The target substance exhibits a good linear relationship within the concentration range of 0.01–0.20 mg/kg,as indicated by correlation coefficients greater than 0.99.The limits of detection(S/N=3)of the method were 10–50μg/kg.At different concentrations(1.0,2.0,10.0 mg/kg),the recovery rate ranged from 81.2%–105.3%,and the relative standard deviation was not greater than 10%.Conclusion This method is straightforward to use,fast,highly accurate,and sensitive,and is capable of performing qualitative and quantitative analysis of 7 kinds of sweeteners and preservatives in quick-frozen prepared foods.It provides a basis for rapid screening and risk assessment of preservatives and sweeteners in these foods.