三聚氰胺固定银离子色谱固定相的制备及其在油脂检测中的应用  

Preparation of melamine immobilized silver ion chromatography stationary phase and its application in the detection of oils and fats

作　　者：马自翰 齐创 刘尧刚 胡志雄 韩立娟 张维农 齐玉堂 MA Zihan;QI Chuang;LIU Yaogang;HU Zhixiong;HAN Lijuan;ZHANG Weinong;QI Yutang(College of Food Science and Engineering,Wuhan Polytechnic University,Wuhan 430023,China;Nantong Gold Sun Oil Co,Ltd,Nantong 226403,Jiangsu,China;Engineering Research Center of Lipid-Based Fine Chemicals of Hubei Province,Wuhan 430023,China)

机构地区：[1]武汉轻工大学食品科学与工程学院,武汉430023 [2]江苏南通金太阳粮油股份有限公司,江苏南通226403 [3]湖北省油脂精细化工工程技术研究中心,武汉430023

出　　处：《中国油脂》2018年第8期143-147,151,共6页China Oils and Fats

基　　金：国家自然科学基金项目(31371783);国家粮食局公益性行业科研专项(201513003);国家自然科学基金青年基金项目(31601505);国家"十二五"科技支撑计划项目(2014BAD04B03)

摘　　要：以异氰酸丙基三乙氧基硅烷为偶联剂,三聚氰胺为配体,制备了三聚氰胺键合硅胶色谱固定相,利用三聚氰胺和银离子的络合作用,进一步合成得到三聚氰胺固定银离子色谱固定相。采用红外光谱和元素分析对其进行表征,测得三聚氰胺键合量为0.11 mmol/g,通过分光光度法测得银离子负载量为0.17 g/g。在洗脱体系为乙腈-正己烷(体积比0.3∶99.7)、流速0.5 m L/min条件下,该银离子色谱柱对5种不饱和脂肪酸甲酯混合标样完美分离,应用于4种常见油脂样品中不饱和脂肪酸的测定中亦获得较好效果。A novel melamine -bonded silica gel chromatography stationary phase （MBSP） was prepared using isocyanatopropyltriethoxysilane as the coupling agent and melamine as the ligand, and then the syn- thesized MBSP was further utilized for immobilization of silver ion according to the complexation of mela- mine and silver ion to prepare melamine immobilized silver ion chromatography stationary phase （AgMBSP）. The AgMBSP was characterized by FTIR and elemental analysis, and the results showed that the bonding amount of melamine was 0.11 mmol/g and the loading amount of silver ion was determined as 0.17 g/g by spectrophotometry. Under the HPLC conditions of acetonitrile - n -hexane（0.3：99.7） and flow rate O. 5 mL/min, five kinds of unsaturated fatty acid methyl esters could be completely separa- ted by AgMBSP. Also good results were obtained when the column was applied in the determination ofunsaturated fatty acids in four common oils and fats.

关 键 词：三聚氰胺 银离子色谱固定相 不饱和脂肪酸 

分 类 号：TQ646[化学工程—精细化工] TQ317