超高效液相色谱-串联质谱法同时测定粮食及肉制品中的24种工业染料

Simultaneous determination of 24 industrial dyes in grain and meat products by ultra performance liquid chromatography-tandem mass spectrometry

建立了测定粮食及肉制品中24种禁用工业染料的超高效液相色谱-串联质谱法。样品经甲醇、乙腈提取后，过WAX固相萃取柱净化。采用ACQUITY UPLC BEH C18分析柱分离，以10mmol／L乙酸铵-0．2％甲酸水溶液和甲醇-乙腈（7：3，v／v）为流动相梯度洗脱，多反应监测（MRM）模式测定。24种染料的相关系数R^2均大于0．99，回收率在61％～116％之间，方法的精密度（RSD，n=6）小于13％，定量限在0．1～4．0μg／kg。该方法灵敏度高，操作简单、高效．适合于粮食及肉制品中24种禁用工业染料的同时定量及确证分析.

An ultra performance liquid chromatography-tandem mass spectrometry （ UPLC-MS/ MS） analytical method was established for the simultaneous determination of 24 forbidden industrial dyes in grain and meat products. The sample was extracted with methanol and acetonitrile, and cleaned-up by a WAX solid phase extraction column. The solution was separated on an ACQUITY UPLC BEH C18 column eluted with a mixture of 10 mmol/L ammonium acetate- 0. 2% formic acid aqueous solution and methanol-acetonitrile （7： 3, v/v） as the mobile phases, and then analyzed in multiple reaction monitoring （MRM） mode. The correlation coefficients were above 0.99, the average recoveries were 61% - 116%, and the relative standard deviations （ RSD, n =6） were lower than 13%. The quantification limits were 0. 1 -4.0 μg/kg. This method is simple, effective, sensitive, and suitable for the determination and confirmation of the 24 forbidden industrial dyes in grain and meat products.