目的建立一种巯基键合银离子色谱固定相的制备方法。方法以活化硅胶为原料,巯丙基三甲氧基硅烷为偶联剂,在邻二甲苯溶液中合成巯丙基键合硅胶,利用巯基与银离子之间的键合作用合成银离子色谱固定相。采用红外光谱、元素分析与银离子负载量对其进行表征,以0.5%乙腈-正己烷(V:V)溶液为流动相,对5种不同不饱和脂肪酸标样及4种常见食用油中的不饱和脂肪酸甲酯进行分离分析与评价。结果经表征与分析可知,巯丙基硅胶键合银离子效果很好,其银离子负载量为0.182 g/g,该分析条件下,对于常见不饱和脂肪酸甲酯的具有很好分离效果,且具有很好的稳定性与重现性。结论该巯基键合银离子色谱固定相对不饱和脂肪酸甲酯具有较好的分离能力,在多不饱和脂肪酸的分析、分离纯化方面具有较好的应用潜力。
Objective To establish a method for the preparation of silver ion stationary phase bonded by mercaptopropyl silica gel(SISP-MSG). Methods Mercaptopropyl silica gel(MSG) was prepared with activated silica gel as raw material,(3-mercaptopropyl)trimethoxysilane as coupling agent and o-xylene as solvent. The obtained MSG was further reacted with silver nitrate for the preparation of proposed silver ion stationary phase, and characterized by infrared spectrum, element analysis and the loading amount of silver ion. The mixture solution of 5 kinds of different standards of unsaturated fatty acids and 4 kinds of common edible oil samples were separated and analyzed with acetonitrile-n-hexane(0.5%) as mobile phase. Results According to the results of characterization and analysis, the MSG showed perfect bonding effect for silver ions, and the loading amount of silver ion was 0.182 g/g. Under the prescribed analysis condition, 5 different kinds of common unsaturated fatty acid methyl esters had been well separated with a good stability and reproducibility. Conclusion SISP-MSG can provide a good separation of unsaturated fatty acid methyl esters, and it will have a good potential for the application of polyunsaturated fatty acids' analysis and purification.