| 马自翰，齐创，刘尧刚，等.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[J].中国油脂,2018,43(8):.[MA Zihan, QI Chuang, LIU Yaogang，etc.Preparation of melamine immobilized silver ion chromatography stationary phase and its application in the detection of oils and fats[J].China Oils and Fats,2018,43(8):.] |
| 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 |
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| DOI： |
| 中文关键词: 三聚氰胺 银离子色谱固定相 不饱和脂肪酸 |
| 英文关键词:melamine silver ion chromatography stationary phase unsaturated fatty acid |
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| 中文摘要: |
| 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 mL/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。 |
| 英文摘要: |
| 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 synthesized MBSP was further utilized for immobilization of silver ion according to the complexation of melamine 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 0.5 mL/min, five kinds of unsaturated fatty acid methyl esters could be completely separated by AgMBSP. Also good results were obtained when the column was applied in the determination of unsaturated fatty acids in four common oils and fats. |
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