SPE-UPLC-MS/MS同时测定食品中二甲基黄、二乙基黄  

Determination of Dimethyl Yellow, Diethyl Yellow in Food Using SPE-UPLC-MS/MS Method

作　　者：王雪娇 郦明浩[2] 李锦清[2] 

机构地区：[1]佛山市质量计量检测中心,广东佛山528225 [2]广东省产品质量监督检验中心,广东佛山528300

出　　处：《广东化工》2016年第24期147-148,共2页Guangdong Chemical Industry

摘　　要：建立固相萃取-超高效液相色谱-串联质谱/质谱法（SPE-HPLC-MS/MS）测定食品中二甲基黄、二乙基黄的分析方法。试样经乙腈提取,C18固相萃取柱净化后,以乙腈和0.1%甲酸水溶液（v/v）为流动相,C18色谱柱分离,采用电喷雾离子源,正离子扫描多反应监测（MRM）模式进行检测。二甲基黄和二乙基黄在0.1～50μg/L浓度范围内均呈良好线性关系,相关系数（r^2）均大于0.999。加标回收率为79.8%～86.8%,相对标准偏差为7.4%～10.8%。二甲基黄、二乙基黄的方法检出限均为0.5μg/kg;定量限均为2μg/kg。方法简单快速、准确、灵敏,适用于食品中二甲基黄、二乙基黄的测定。A method was established for the determination of dimethyl yellow, diethyl yellow in food using solid phase extraction（SPE） and ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. The sample was extracted by acetonitrile, and purified by C18 SPE column. The target compound was separated on a reversed phase column by acetonitrile and 0.1 % formic acid water solution（v/v）, and then detected by positive electrospray ionization under multiple reaction monitoring（MRM） mode. Under the optimized conditions, the calibration curves for dimethyl yellow and diethyl yellow were linear in the range of 0.1～50 μg·L-1 with correlation coefficients（r^2） greater than 0.999. The average recoveries of blank matrix sample was 81.6 %～90.1 %, and the relative standard deviation（RSD） was 7.4 %～10.8 %. The limits of detection（LOD） and quantitation（LOQ） of dimethyl yellow and diethyl yellow were 0.5 μg·kg^-1 and 2 μg·kg^-1 in food, respectively. The developed method is simple, rapid, accurate and sensitive for the detection of dimethyl yellow, diethyl yellow in food.

关 键 词：二甲基黄 二乙基黄 超高效液相色谱-串联质谱/质谱法 固相萃取 

分 类 号：O65[理学—分析化学]