超高效液相色谱串联质谱法检测婴儿配方奶粉中的双氰胺  

Determination of Dicyandiamide residue in Infant Formula Milk Powder by Ultra Performance Liquid Chromatography Combined with Mass Spectrometry

作　　者：那文志 胡冬梅[1] 李则均 

机构地区：[1]黑龙江省完达山乳业股份有限公司质检中心,黑龙江哈尔滨150078

出　　处：《生命科学仪器》2013年第4期33-36,共4页Life Science Instruments

摘　　要：目的:建立一种要儿配方奶粉中双氰胺残留量的超高效液相色谱质谱检测方法。方法:采用三氯乙酸溶液沉淀蛋白,处理液用Waters Sep-Pak AC2固相萃取柱净化,用超高效液相色谱-串联质谱仪测定,外标法定量。结果:在0.10μg/mL^50.0μg/mL范围内,线性良好,线性方程为y=2310.43×x+1.01815,相关系数为0.999826(n=6)。加标回收率在90%~110%,相对标准偏差在10%以内。最低检出限为0.05mg/kg。结论:本方法操作简便,检出限低,重复性好,适合婴儿配方奶粉中双氰胺残留的测定。[Objective] A new method to detect the dicyandiamide residue in infant formula milk powder by using ultra high performance liquid chromatography combined with mass spectrometry is established. [ Methods ] After protein precipitation with trichloroacetic acid solution, the treatment fluid was purified by using a Waters Sep-Pak AC2 solid phase extraction column, and then determinated by ultra-high performance liquid chromatography combined with mass spectrometry, and external standard method was used for quantification. [ Results ] In the range of 0.10 μg/mL - 50.0 μg/mL range, the results showen good linearity, the linear equation is y=2310.43x＋l.01815, and the correlation coefficient is 0.999826 （ n=6 ） . The recovery is 90% - 110%, the relative standard deviation is less than 10%, and the detection limit is 0.05 mg/kg. [Conclusions] This method is simple, with low detection limit and good repeatability to detect the dicyandiamide residue in infant formula milk powder.

关 键 词：双氰胺 超高效液相色谱 婴儿配方奶粉 

分 类 号：TS252.51[轻工技术与工程—农产品加工及贮藏工程]