建立了基于改进的 QuEChERS方法结合液相色谱-串联质谱测定腐竹和豆干中二甲基黄和二乙基黄的方法。在2.0 g腐竹和豆干样品中加入5 mL水浸泡，然后加入10 mL乙腈提取，加入1.0 g NaCl、2.0 g无水硫酸镁进行液液分离；取1 mL提取液经50 mg N-丙基二乙胺分散固相萃取净化，经液相色谱分离、质谱测定，外标法定量。二甲基黄在添加水平为0.3、1和10μg／kg时，方法的回收率为73.5％~84.5％；二乙基黄在添加水平为0.1、1和10μg／kg时，方法的回收率为70.5％~81.2％；方法的相对标准偏差小于11％。二甲基黄的检出限和定量限分别为0.1μg／kg和0.3μg／kg，二乙基黄的检出限和定量限分别为0.05μg／kg和0.1μg／kg。该方法可以用于腐竹、豆干中二甲基黄和二乙基黄的快速筛查和定量分析。
A modified QuEChERS( quick,easy,cheap,effective,rugged and safe)method followed by liquid chromatography-tandem mass spectrometric analysis was developed for the determination of dimethyl yellow and diethyl yellow in yuba and dried beancurd. Yuba and dried beancurd samples were soaked by deionized water,then acetonitrile was added to extract the analytes. Sodium chloride and anhydrous magnesium sulfate were added for liquid-liquid separa-tion. The extracts were cleaned-up by dispersive solid-phase using N-propyl diethylamine. The analytes were separated by liquid chromatography and determined by mass spectrometry. Exter-nal standard method was used for quantification. The recoveries of dimethyl yellow were in the range of 73. 5%-84. 5% at spiked levels of 0. 3,1 and 10 μg/kg and the recoveries of diethyl yellow were in range of 70. 5%-81. 2% at spiked levels of 0. 1,1 and 10 μg/kg;relative stand-ard deviations of the method were lower than 11%. The limit of detection and the limit of quan-tification of dimethyl yellow were 0. 1 μg/kg and 0. 3 μg/kg,respectively;the limit of detection and the limit of quantification of diethyl yellow were 0. 05 μg/kg and 0. 1 μg/kg,respectively. This method can be used in rapid screening and quantitative analysis of dimethyl yellow and diethyl yellow in yuba and dried beancurd.
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