全自动固相萃取/超高效液相色谱串联质谱法检测食品中的9种合成色素

摘要

建立了超高效液相色谱串联质谱法检测食品中柠檬黄、苋菜红、胭脂红、日落黄、亮蓝、新红、靛蓝、诱惑红、赤鲜红9种合成色素的快速检测方法。采用反相-弱阴离子交换固相萃取小柱，在Labtech的Speline全自动固相萃取平台上实现对样品的连续、自动化处理过程，极大地提高了工作效率。净化液经Agilent XDB C18色谱柱，以甲醇和10mmol/L乙酸铵溶液为流动相梯度洗脱，6min内实现基线分离。采用电喷雾正离子模式（ESI+）电离，多反应监测（MRM）模式定量检测。9种合成色素的质量浓度在10～500μg/L的范围内与其响应值呈线性关系，其检出限（3S/N）在0.009～0.044mg/kg之间。将该方法应用于食品中合成色素的测定，其回收率范围为88.8%～108.2%，相对标准偏差（n=6）均小于5%。该方法高效、快速、准确，可满足批量化检测的需求。%A new method was developed for the rapid detection of 9 synthetic colorants in food by ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The solid phase extraction(SPE)column with double func-tions of reversed phase and weak anion exchange was applied on the Labtech Speline auto-SPE platform for sequential and automatic process,which promoting working efficiency greatly. Subsequently,the purified liquid was separated well by Ag-ilent Eclipes Plus C18 column within 6 minutes when methanol and 10 mmol/L ammonium acetate solution were adopted as mobile phase for a gradient elution. And the qualitative and quantitative analysis was performed by mass spectrometry with electrospray in positive ionization mode and multiple reaction monitoring(MRM)mode,ultimately. Results showed that the response of synthetic colorants had a good linearity with its mass concentration in 10~500μg/L and the limit of detec-tion(3S/N)between 0.009 and 0.044mg/kg. The proposed method was used for the determination of synthetic colorants in food,giving values of recovery in the range of 88.8%~108.2%with relative standard deviations(RSDs,n=6)less than 5%. This method was efficient,rapid and accurate,which could meet the requirement of mass detection.