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以γ-氯丙基三氯硅烷为媒介,将乙二胺偶联接枝到硅胶微粒表面,制备乙二胺硅胶功能填料(EDA/SiO2),研究了其对Ag+的吸附性能。利用Ag+改性的乙二胺偶联接枝硅胶为固定相,制备4.6 mm×250 mm分析柱应用于EPA和DHA分离。结果表明:在乙二胺偶联接枝硅胶与硝酸银质量比为15:1、pH=6、反应时间25 h的条件下制备的Ag+改性硅胶,在洗脱体系为正己烷:异丙醇=1500:1,流速为1 mL/min,样品浓度为1 mg/mL EPA和DHA混合液,进样5μL的条件下,EPA和DHA达到基线分离,分离度为1.50;该填料可以有效地分离EPA和DHA。
To ethylenediamine silica gel functional filler (EDA / SiO2) was prepared by γ-chloropropyltrichlorosilane coupling grafting ethylenediamine onto the surface of silica gel particles, and its adsorption performance on Ag + was studied. Ag + modified ethylenediamine coupled grafted silica gel as the stationary phase, the preparation of 4.6 mm × 250 mm analytical column should be used for EPA and DHA separation. The results showed that the Ag + modified silica gel prepared under the conditions of ethylenediamine coupling grafted silica gel and silver nitrate mass ratio of 15: 1, pH = 6 and reaction time of 25 h was n-hexane: isopropyl Ethanol = 1500: 1, the flow rate was 1 mL / min, the concentration of the sample was 1 mg / mL and the mixture of EPA and DHA. Under the condition of 5 μL injection, EPA and DHA reached baseline separation with a resolution of 1.50. Isolate EPA and DHA.