高效液相色谱-串联质谱法同时测定面粉中7种非法添加剂

Simultaneous Determination of 7 Illegal Additives in Flour by High Performance Liquid Chromatography-Tandem Mass Spectrometry

目的:建立一种分析面粉中7种非法添加剂的高效液相色谱-串联质谱检测方法。方法:试样经乙腈∶水(1∶1,V∶V)提取、超声、离心、氮吹浓缩后,经Agilent Eclipse Plus C_(18) RRHD色谱柱分离、0.1%甲酸-5 mmol·L^(-1)甲酸铵水和甲醇为流动相进行等度洗脱,采用多反应监测模式分析。结果:7种目标化合物在0.10~8.00 ng·mL^(-1)呈良好的线性关系(R^(2)>0.990),检出限为0.03~0.15 mg·kg^(-1),定量限为0.10~0.45 mg·kg^(-1);回收率在88.6%~104.3%,相对标准偏差在2.1%~5.8%(n=6)。结论:该方法简便、灵敏、准确,可满足小麦粉中7种非法添加物的同时检测要求。

Objective:To establish a high performance liquid chromatography-tandem mass spectrometry method for the determination of 7 illegal additives in flour.Method:The samples were extracted by acetonitrile∶water(1∶1,V∶V),concentrated by ultrasound,centrifugation and nitrogen blowing,separated by Agilent Eclipse Plus C_(18) RRHD column,and then eluted with 0.1%formic acid-5 mmol·L^(-1) ammonium formate water and methanol as mobile phase,and analyzed by multi-reaction monitoring mode.Result:There was a good linear relationship(R^(2)>0.990)between 0.10~8.00 ng·mL^(-1) for the 7 target compounds.The limit of detection was 0.03~0.15 mg·kg^(-1),and the limit of quantification was 0.10~0.45 mg·kg^(-1).The recoveries were 88.6%~104.3%,and the relative standard deviations were 2.1%~5.8%(n=6).Conclusion:The method is simple,sensitive and accurate,and can satisfy the simultaneous detection of 7 illegal additives in wheat flour.