摘要
以莠去津为模板分子,甲基丙烯酸(methacrylic acid,MAA)为功能单体,乙腈为致孔剂,采用沉淀聚合法制备莠去津分子印迹聚合物微球(molecularly imprinted polymer microspheres,MIPMs).对MIPMs制备工艺进行优化,当莠去津与MAA物质的量比1:4、乙腈用量50 mL、聚合温度60℃时,MIPMs的吸附效果最好.通过吸附实验考察MIPMs对目标物的吸附性能,并结合Scatchard分析可知MIPMs对莠去津存在两类吸附位点,且最大表观结合量为282.69μmol/g.以MIPMs作为固相萃取材料,制备分子印迹固相萃取(molecularly imprinted solid phase extraction,MISPE)柱,用于样品前处理,并建立莠去津-MISPE-高效液相色谱法测定食品中4种三嗪类农药(西玛津、莠灭净、莠去津、扑草净)残留的方法.结果表明,MISPE柱对4种三嗪类农药具有特异选择性,4种农药的线性相关系数为0.9991~0.9997,检出限为0.5~5 ng/mL,平均回收率在86.2%~95.7%之间,相对标准偏差为1.98%~4.51%(n=5).该方法能够简单、准确、高选择性地检测食品中三嗪类农药残留.
Molecularly imprinted polymer microspheres (MIPMs) were prepared by precipitation polymerization with atrazine as the template molecule, methacrylic acid (MAA) as the functional monomer, and acetonitrile as the porogen. The preparation process was optimized, and the best adsorption performance was observed for MIPMs prepared under the following conditions: atrazine-to-MAA molar ratio 1:4, addition of 50 mL of acetonitrile, and polymerization temperature 60 ℃. The adsorption properties of the MIPMs toward target compounds were investigated through adsorption experiments and Scatchard analysis. It was found that there were two types of adsorption sites for atrazine in the MIPMs, and the maximum apparent binding capacity was 282.69 μmol/g. A molecularly imprinted solid phase extraction (MISPE) column was prepared with the MIPMs as a sorbent for sample pretreatment, and an atrazine-MISPE-high performance liquid chromatography (HPLC) method was established for determining residues of four triazine pesticides, simazine, ametryn, atrazine and prometryn, in foods. The results showed that the MISPE column had specific selectivity to the four triazine pesticides with linear correlation coefficients of 0.999 1–0.999 7. The detection limits of the method were 0.5–5 ng/mL. The average recoveries were between 86.2% and 95.7%, and the relative standard deviations (RSDs) were 1.98%–4.51%(n = 5). This method can easily, accurately and selectively detect triazine herbicide residues in foods.
作者
张凯杰
秦思楠
赵春娟
高文惠
ZHANG Kaijie;QIN Sinan;ZHAO Chunjuan;GAO Wenhui(College of Bioscience and Bioengineering,Center for Fermentation Engineering of Hebei Province,Hebei University of Science and Technology,Shijiazhuang 050000,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2019年第20期338-345,共8页
Food Science
基金
河北省重点研发计划项目（19275505D）
石家庄市科学技术研究与发展计划项目(181490372A)
关键词
莠去津
三嗪类农药残留
分子印迹聚合物微球
吸附性能
沉淀聚合
固相萃取
高效液相色谱法
食品检测
atrazine
triazine herbicide residues
molecularly imprinted polymer microspheres
adsorption properties
precipitation polymerization
solid phase extraction
high performance liquid chromatography
food detection
