摘要
采用溶胶-凝胶法,以γ-Fe_(2)O_(3)为原材料,原硅酸四乙酯(TEOS)为硅源,通过TEOS的水解和缩合包裹修饰得到γ-Fe_(2)O_(3)@SiO_(2)的纳米复合材料,之后通过3-氨丙基三甲氧基硅烷(APTMS)、戊二酸酐(GTA)的共价修饰来得到磁性微球(γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH),然后用所得的羧基化微球、对苯二甲酸(H_(2)BDC)、ZrCl_(4)制备核壳式磁性微球(γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66);由羧基化微球、2-氨基对苯二甲酸(H_(2)N-BDC)、ZrCl4制备得到γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-NH_(2)磁性微球;由二乙烯三胺(2,3-NH_(2))修饰核壳式磁性微球(γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66)得到γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-2,3-NH_(2)磁性微球,由三乙烯四胺(3,4-NH_(2))修饰核壳式磁性微球(γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66)得到γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-3,4-NH_(2)磁性微球.利用红外光谱(IR)和X-射线粉末衍射(XRD)分析得出核壳式磁性微球γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66的结构信息,结果表明其产物修饰成功.荧光分光光度计测定对水杨酸(SA)进行磁固相萃取(MSPE)的实验,设置不同梯度pH和不同洗脱液,观察pH和洗脱液对被修饰的磁性微球的洗脱效果及影响,结果表明被修饰的磁性微球在碱性(pH=8)条件下吸附效果好,γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-2,3-NH_(2)颗粒在0.1 mol/L NaOH洗脱液中的洗脱效果最好,γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-3,4-NH_(2)磁性微球在MeOH洗脱液中的洗脱效果最好,γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-NH_(2)磁性微球在1%SDS洗脱液中的洗脱效果最好.但经MeOH洗脱液洗脱后的γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-3,4-NH_(2)磁性微球骨架结构坍塌.
With γ-Fe_(2)O_(3) as raw material and tetraethyl orthosilicate(TEOS)as silicon source,γ-Fe_(2)O_(3)@SiO_(2) nanocomposites were prepared by sol-gel method,and then magnetic microspheres(γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH)were prepared by covalent modification of 3-aminopropyltrimethoxysilane(APT-MS)and glutaric anhydride(GTA).The magnetic microspheres(γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH),terephthalic acid(H_(2)BDC)and ZrCl_4 were used for the preparation of core-shell magnetic microspheres(γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66).Furthermore,γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-NH_(2) core-shell magnetic microspheres were prepared by 2-amino terephthalic acid(H_(2)N-BDC)and ZrCl_(4),and γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-2,3-NH_(2)core-shell magnetic microspheres were modified by diethylenetriamine(2,3-NH_(2)).And diethylenetriamine(2,3-NH_(2))could be replaced by triethylenetetramine(3,4-NH_(2)),and γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-3,4-NH_(2)core-shell magnetic microspheres could be obtained.The structure information of core-shell magnetic microspheres was obtained by Infrared spectrum(IR)and X-ray diffraction(XRD),and the results showed that the product was successfully modified.The samples of magnetic solid phase extraction(MSPE)of salicylic acid(SA)were measured by fluorescence spectrophotometer.The different gradient pH and different eluents were set to observe the elution effect and influence of pH and eluant on modified magnetic microspheres.The results showed that the modified magnetic microspheres had good adsorption effect in alkaline(pH=8)environment.The elution effect of γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-2,3-NH_(2)particles in 0.1 mol/L NaOH eluent is the best,the elution effect ofγ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-3,4-NH_(2) magnetic microspheres in MeOH eluent is the best,the elution effect of γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/UiO-66-NH_(2) magnetic microspheres in 1% SDS eluent is the best.However,the skeleton structure of γ-Fe_(2)O_(3)@SiO_(2)-NH_(2)-COOH/
作者
杨琳燕
韦冬微
王思蒙
李爽
陈峥嵘
朱欣怡
李存
Yang Linyan;Wei Dongwei;Wang Simeng;Li Shuang;Chen Zhengrong;Zhu Xinyi;Li Cun(Tianjin Key Laboratory of Agricultural Animal Breeding and Healthy Husbandry,College of Animal Science and Veterinary Medicine,Tianjin Agricultural University,Tianjin 300392,China)
出处
《南开大学学报（自然科学版）》
CAS
CSCD
北大核心
2024年第3期113-120,共8页
Acta Scientiarum Naturalium Universitatis Nankaiensis
基金
国家自然科学基金(32202760)
农业农村部智慧养殖重点实验室(省部共建)开放课题(2023-TJAULSBF-2103)
天津市高等院校“兽医生物技术创新团队”资助项目(TD13-5091)
国家级大学生创新创业训练计划(202110061011)。
