氧化石墨烯色谱固定相的制备及其在食品中三聚氰胺分析中的应用  

Fabrication of Graphene Oxide@SiO_2 as Stationary Phase and Its Application in Determination of Melamine in Food Samples

作　　者：张瑶琴 艾连峰[2] 王曼曼 王学生 刘珊 侯宁 

机构地区：[1]华北理工大学公共卫生学院,河北唐山063000 [2]河北出入境检验检疫局,河北石家庄050000

出　　处：《分析测试学报》2016年第8期981-986,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(21305028);河北省自然科学基金项目(B2013209238;H2016209018);河北省教育厅自然科学项目(Q2012155);国家质检总局项目(2013IK154;2014IK092)

摘　　要：以N,N-二环己基碳二亚胺为偶联剂,利用氧化石墨烯表面的羧基与氨基化硅球表面的氨基反应合成了一种氧化石墨烯键合硅球色谱固定相,通过扫描电镜和拉曼光谱对其进行表征,并考察了极性小分子在柱上的色谱行为。与氨基化硅球固定相相比,在相同的色谱条件下,三聚氰胺、双氰胺等氨基化合物的保留因子明显提高,且该固定相在亲水模式下对氨基化合物具有良好的保留性能,将其作为分析柱用于鸡蛋和牛奶中三聚氰胺的分析。该方法在0.2～50μg/m L范围内线性良好,相关系数（r）为0.999 9,定量下限为0.87mg/kg。在1,2,10 mg/kg加标水平下的回收率为84.7%～93.9%,相对标准偏差为4.1%～6.3%。Graphene oxide （GO） has received great interest for its unique properties and potential ap- plications in separation. Here, （GO） @ SiC2 composites-based stationary phase for high performance liquid chromatograpily （HPLC） were fabricated by covalently bonding GO onto aminosilica micro- spheres using N, N-dicyclohexylcarbodiimide as coupling agent. The reaction was achieved via cou- pling the amino groups of aminosilica and the carboxyl groups of GO. The prepared GO@ SiO2 was characterized by scanning electron microscopy and Raman spectroscopy. GO@ SiO2 composites were developed as stationary phase, and the chromatographic properties of bare SiO2 and GO@ SiO2 were investigated by a series of polar compounds including melamine, cyanuric acid, clenbuterol, 4-ami- noantipyrine and 4-methylaminoantipyrine. Under the same conditions, GO@ SiO2 column obtained a better separation for polar analytes in hydrophilic mode and the column was used as an analytical col- umn for the determination of melamine in egg arid milk samples. The proposed method was linear over the range of 0. 2 -50. 0 μg/mL with a correlation coefficient（r） of 0. 999 9. The limit of quantitation for melamine was 0. 87 mg/kg. The recoveries of melamine at three spiked levels of 1, 2, 10 mg/kg ranged from 84.7% to 93.9% with relative standard deviations （RSDs） of 4. 1% -6. 3%.

关 键 词：氧化石墨烯 固定相 三聚氰胺 牛奶 鸡蛋 高效液相色谱(HPLC) 

分 类 号：O657.72[理学—分析化学] O623.732[理学—化学]