超高效液相色谱-电喷雾串联质谱法同时测定调味品与熟肉制品中6种工业染料

摘要

A method has been established for the determination of 6 industrial dyes,Basic OrangeⅡ, Basic Orange 21,Basic Orange 22,Acid Orange Ⅱ,Azophloxine I and Rhodamine Bextra in condi-ments and cooked meat products by ultra performance liquid chromatography combined with electros-pray tandem mass spectrometry (UPLC-MS/MS).Samples are extracted with solution of acetonitrile and water (7∶3).The supernatant is separated on BEH C18 column (1.7μm,2.1 ×50 mm)by gra-dient elution with methanol and 10 mmol/L ammonium acetate with 0.1% (volume ratio)formic acid. Under the optimal experimental conditions,LODs of Basic OrangeⅡ,Basic Orange 21 ,Basic Orange 22,Acid Orange Ⅱ and Rhodamine Bextra are all 0.5μg/kg,LOQs are all 1μg/kg;LOD of Azo-phloxineI is 50μg/kg,and LOQ is 100μg/kg .The method shows a good linearity of Basic OrangeⅡ, Basic Orange 21,Basic Orange 22,Acid Orange Ⅱand Rhodamine Bextra in the range of 1~50μg/kg with correlation coefficients more than 0 .9 9;The range of linearity and correlation coefficient of Azo-phloxine I are respectively 50~100μg/kg and more than 0.99.Recoveries for samples spiked at three levels range from 7 5 .6%to 9 9 .7%with RSDs from 0 .9%to 1 0 .7%.This method is suitable for the determination of industrial dyes in condiments and cooked meat products.%建立了超高效液相色谱-电喷雾串联质谱法（UPLC-MS/MS）测定调味品与熟肉制品中碱性橙Ⅱ、碱性橙21、碱性橙22、酸性橙Ⅱ、酸性红1号和碱性玫瑰精6种工业染料分析方法。样品用V（乙腈）∶V（水）7∶3的溶液提取，取上清液过滤，以 BEH C18柱（1．7μm，2．1×50 mm）为分离柱，甲醇和10 mmol/L乙酸铵（含0．1％甲酸）梯度洗脱，在优化的实验条件下，碱性橙Ⅱ、碱性橙21、碱性橙22、酸性橙Ⅱ和碱性玫瑰精的检出限均为0．5μg/kg ，定量限为1μg/kg；酸性红1号检出限为50μg/kg ，定量限为100μg/kg；碱性橙Ⅱ、碱性橙21、碱性橙22、酸性橙Ⅱ和碱性玫瑰精的线性范围为1～50μg/kg，相关系数均大于0．99。酸性红1号的线性范围为50～1000μg/kg，相关系数大于0．99。样品在三个添加水平下平均回收率在75．6％～99．7％之间，相对标准偏差在0．9％～10．7％。可用于调味品与熟肉制品中6种工业染料的检测。