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应用介孔分子印迹聚合物萃取粮食中的乙酰甲胺磷
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作者单位
谭钰清,孙梦谣,刘宇婷,张伽宜,李智昊,陈立钢 东北林业大学理学院 
基金项目:黑龙江省自然科学基金(JJ2018ZR0081);东北林业大学国家级大学生创新训练项目(201810225100)
中文摘要:以乙酰甲胺磷为模板分子,3 氨基丙基三乙氧基硅烷(APTES)为功能单体,表面活性剂正十二烷胺(DDA)为介孔模板剂,正硅酸乙酯为交联剂,采用溶胶凝胶技术制备乙酰甲胺磷介孔分子印迹聚合物(MIP),并对其进行了表征。Scatchard分析表明,该聚合物对乙酰甲胺磷有两种结合方式,最大表观结合量Qmax1=4703 mg/g,Qmax2=9031 mg/g;平衡解离常数kd1=5714 mg/L,kd2=18868 mg/L。吸附动力学测定结果显示,其对乙酰甲胺磷的吸附符合准二级动力学模型;吸附热力学测定结果显示其吸附为放热过程。将该聚合物用于基质固相分散萃取(MSPD)粮食中乙酰甲胺磷,最佳条件为:聚合物与样品的质量比为1∶1,研磨时间为8 min,淋洗剂为乙醇-水(2∶1,体积比),洗脱剂为乙腈-乙酸溶液(19∶1,体积比)。所得洗脱液采用高效液相色谱法检测,测得乙酰甲胺磷的线性范围为003~03 μg/g,检出限为0015 μg/g,回收率为925%~971%,相对标准偏差为29%~37%。该方法兼具介孔分子印迹技术的高选择性如和MSPD技术的快速分离性,为乙酰甲胺磷残留分析提供了新思路。
中文关键词:乙酰甲胺磷  介孔分子印迹聚合物  粮食  基质固相分散萃取  高效液相色谱
 
Extraction of Acephate in Grains Using Mesoporous Molecularly Imprinted Polymer
Abstract:An acephate mesoporous molecularly imprinted polymer(MIP) was prepared by sol-gel technique using acephate as template molecule,3 aminopropyl propyl triethoxysilane(APTES) as functional monomer,surfactant dodecylamine(DDA) as mesoporous template and tetraethoxysilane as coupling agent.And it was characterized.Results of Scatchard analysis showed that there existed two kinds of binding sites.The values of apparent maximum absorption capacity were calculated as follows:Qmax1=4703 mg/g and Qmax2=9031 mg/g,and the dissociation constants:kd1=5714 mg/L and kd2=18868 mg/L.The adsorptive dynamics results showed that the adsorption of the polymer toward acephate accorded with quasi secondary dynamics model.The results of adsorption thermodynamics showed that the adsorption process was exothermic.The prepared polymer was used for matrix solid phase dispersion(MSPD) extraction of acephate in grains.The optimum experimental conditions were as follows:the ratio of polymer to sample:1∶1,grinding time:8 minutes,the washing solvent:ethanol-water(2∶1,by volume),the eluent:acetonitrile-acetic acid(19∶1,by volume).The final eluent was detected by high performance liquid chromatography,and the calibration curve of acephate was linear in the range of 003-03 μg/g with a detection limit of 0015 μg/g.Recoveries for acephate were between 925%and 971%with relative standard deviations(RSD) of 29%-37%.With the advantages of high selectivity of mesoporous molecularly imprinting technique and the rapid separation of matrix solid phase dispersion extraction,this method provides a new idea for the residue analysis of acephate.
Key Words:acephate  mesoporous molecularly imprinted polymer  grains  matrix solid phase dispersion extraction  high performance liquid chromatography
引用本文:谭钰清,孙梦谣,刘宇婷,张伽宜,李智昊,陈立钢.应用介孔分子印迹聚合物萃取粮食中的乙酰甲胺磷[J].分析测试学报,2019,(7):811-816.
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