超高效液相色谱-串联质谱法同时测定膨化食品中10种工业染料  

Simultaneous determination of 10 kinds of industrial dyes in puffed food by ultra performance liquid chromatography-Liquid chromatography tandem mass spectrometry

作　　者：邵国健[1] 朱文涛[1] 韩建康[1] 

机构地区：[1]湖州市疾病预防控制中心,浙江湖州313000

出　　处：《中国卫生检验杂志》2017年第6期784-788,共5页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立超高效液相色谱-电喷雾四级杆串联质谱法(UPLC-MS/MS)同时测定膨化食品中10种工业染料(罗丹明B、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、碱性橙2、碱性橙21、碱性橙22、酸性橙Ⅱ、红2G)的分析方法。方法样品分别用丙酮和丙酮∶水(6∶4,V/V)提取,涡旋振荡1 min,超声20 min,10 000 rpm冷冻离心5 min,混合2次提取液,10 000 r/min冷冻离心3 min,0.2μm微孔滤膜过滤,梯度洗脱条件下经ACQUITY UPLC BEH C_(18)柱(2.1 mm×100 mm,1.7μm)分离后,采用超高效液相色谱-串联质谱法多离子反应监测模式(MRM)检测。结果各种工业染料的质量浓度为5 ng/ml^50 ng/ml时,线性关系良好(相关系数r均>0.995 0),检出限为0.01μg/kg^1.0μg/kg,定量限为0.03μg/kg^3μg/kg。3种加标水平下的平均回收率为85.1%~118.3%,相对标准偏差(RSD)为2.4%~12.1%。结论该法具有前处理简单、灵敏度高、准确性强等特点,能够满足膨化食品中10种工业染料同时检测的要求。Objective To develop a method for the simultaneous determination of 10 kinds of industrial dyes（ Rhodamine B,SudanⅠ,SudanⅡ,SudanⅢ,SudanⅣ,Basic Orange 2,Basic Orange 21,Astrazon Orange R,Acid OrangeⅡ,Red 2G） in puffed food by ultra performance liquid chromatography-Liquid chromatography tandem mass spectrometry（ UPLC-MS/MS）method. Methods The samples were conducted for gradient elution twice with acetone and acetone： water（ 6∶4,V/V） by vortex-assisted（ 1 min）,ultrasoud for 20 min,frozen centrifugation at 10 000 min for 5 min,mixing extract for twice,10 000 RPM frozen centrifugation for 3 min and filtering with 0. 2 μm micropore filter. Separations were performed on ACQUITY UPLC BEH C18column（ 2. 1 mm × 100 mm,1. 7 μm） by UPLC-MS/MS in multi-ion reaction monitoring mode（ MRM）.Results The calibration curves of industrial dyes showed a good linearity in the range of 5 ng/ml-50 ng/ml,with correlation coefficients（ r） above 0. 995 0. The detection limits（ LOD） of the method were within 0. 01 μg/kg-1. 0 μg/kg,and the limits of quantification（ LOQ） were within 0. 03 μg/kg-3 μg/kg. The average recoveries of three spiking levels ranged from 85. 1%to 118. 3%,with the relative standard deviation（ RSD） of 2. 4%-12. 1%. Conclusion This method was convenient,selective,sensitive and practical with good recovery. It can be applied to the simultaneous determination of 10 industrial dyes in puffed food.

关 键 词：膨化食品 液相色谱-串联质谱法 工业染料 

分 类 号：O657.72[理学—分析化学]