克百威分子印迹聚合物合成方法的优化
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摘要
目的制备粒径均一的荧光标记克百威分子印迹聚合物。方法通过单因素实验对分散聚合法合成聚苯乙烯种球进行优选,通过均匀设计对多步溶胀法制备克百威分子印迹微球进行优化。结果聚苯乙烯种球粒径在1.85μm左右,单分散指数(monodispersity index,MDI)为1.56%;克百威分子印迹微球粒径为6～8μm,MDI为2.5%～3.0%。最优合成条件为甲基丙烯酸用量:5.0 mmoL,温度:64℃,转速:300 r·min~(-1),微球吸附平衡时间:2 h,最大吸附量:76.717μmol·g~(-1)和106.411μmol·g~(-1)。结论通过均匀设计优化后制备的克百威分子印迹微球粒径均一,荧光性能稳定,适用于固相萃取前处理过程对吸附效率的要求。
Objective To prepare fluorescent labeled carbofuran molecularly imprinted polymer with uniform particle size.Methods Single factor experiment and uniform design were used to optimize the preparation of polystyrene microspheres(Ps) by dispersive polymerization and carbofuran molecularly imprinted microsphere(QDs@MIPs) by multi-step swelling method respectively.Results The average diameter of Ps was 1.85μm and the monodisperse index(MDI) was 1.56%.The particle size of QDs@MIPs was between 6-8 μm and MDI was 2.5%-3.0%.And,the optimum synthesis condition was 5.0 mmoL of methacrylic acid and temperature was 64 centigrade,speed was 300 rpm,adsorption equilibrium time was 2 h.Finally,the maximum adsorption capacity was 76.717 μmol·g~(-1) and 106.411 μmol·g~(-1).Conclusion The optimized carbofuran QDs@MIPs by uniform design have the uniform particle size and moderate fluorescence intensity,which indicates the prepared carbofuran QDs@MIPs are suitable for the requirement of adsorption efficiency before solid phase extraction.
Objective To prepare fluorescent labeled carbofuran molecularly imprinted polymer with uniform particle size.Methods Single factor experiment and uniform design were used to optimize the preparation of polystyrene microspheres(Ps) by dispersive polymerization and carbofuran molecularly imprinted microsphere(QDs@MIPs) by multi-step swelling method respectively.Results The average diameter of Ps was 1.85μm and the monodisperse index(MDI) was 1.56%.The particle size of QDs@MIPs was between 6-8 μm and MDI was 2.5%-3.0%.And,the optimum synthesis condition was 5.0 mmoL of methacrylic acid and temperature was 64 centigrade,speed was 300 rpm,adsorption equilibrium time was 2 h.Finally,the maximum adsorption capacity was 76.717 μmol·g~(-1) and 106.411 μmol·g~(-1).Conclusion The optimized carbofuran QDs@MIPs by uniform design have the uniform particle size and moderate fluorescence intensity,which indicates the prepared carbofuran QDs@MIPs are suitable for the requirement of adsorption efficiency before solid phase extraction.
引文
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[3] 方开泰.均匀设计与均匀设计表[M].北京:科学出版社,1994:18-21.
[4] 邓勃.试验设计与优化方法[J].分析科学学报,1996(2):72-77.
[5] LIU S S,XIAO Q F,ZHANG J,et al.Uniform design ray in the assessment of combined toxicities of multi-component mixtures[J].Science Bulletin,2016,61(1):52-58.
[6] 张丹,孙英华,刘艳,等.均匀设计法制备苦参碱渗透泵型控释片[J].沈阳药科大学学报,2007(1):16-19.
[7] XIE X D,ZHOU K F,CHEN B Y,et al.Degradation of oxytetracycline using microporous and mesoporous photocatalyst composites:Uniform design to explore factors[J].Journal of Environmental Chemical Engineering,2016,4(4):4453-4465.
[8] HUANG Q H,LIU C,CHEN S J,et al.Effects of formulation on set-to-touch time of waterborne alkyd resin by uniform design [J].Progress in Organic Coatings,2015,87:189-196.
[9] MARIA B T,JOSé C R,EUTIMIO G,et al.Optimization of artificial neural network by genetic algorithm for describing viral production from uniform design data [J].Process Biochemistry,2016,51:422-430.
[10] BO Y,PANG Z L.Generating test data based on improved uniform design strategy[J].Physics Procedia,2015,25:1245-1252.
[11] LIU H L,ZHOU K W,WU D,et al.A novel quantum dots-labeled on the surface of molecularly imprinted polymer for turn-off optosensing of dicyandiamide in dairy products[J].Biosensors and Bioelectronics,2016,77:512-517.
[12] 王慧,王颜红,张红,等.量子点编码乙酰甲胺磷分子印迹荧光微球的制备及性能[J].沈阳药科大学学报,2015,32(4):265-270.
[13] 洪美花.分子印迹聚合物微球的制备及特性评价[D].西宁:青海师范大学,2010.
[14] 陈军.三嗪类除草剂分子印迹聚合物的制备及其在痕量分析检测中的应用研究[D].长沙:湖南农业大学,2013.
[15] 方开泰.均匀设计及其应用(Ⅳ)[J].数理统计与管理,1994(4):54-56.
[16] 赵奕殊.均匀设计表及其使用表的构造[J].战术导弹技术,1988(4):53-58.
[17] 方开泰.均匀设计及其应用(Ⅲ)[J].数理统计与管理,1994(3):52-55.
[18] NADIN A,GEORGES I,ELENA P,et al.Biosensor-assisted selection of optimal parameters for designing molecularly imprinted polymers selective to phosmet insecticide[J].Talanta,2017,174:414-419.
[19] 王雅琼,许文林,吴昊.苯乙烯分散聚合工艺条件对转化率及微球尺寸的影响[J].化学反应工程与工艺,2002(2):138-143.