基于石墨烯修饰的分子印迹膜丝网印刷电极快速测定烟草中苯霜灵农药残留
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摘要
建立了一种基于石墨烯修饰的分子印迹膜丝网印刷电极快速检测烟草样品中苯霜灵的电化学分析法。利用石墨烯的信号放大作用,结合分子印迹技术,以丙烯酰胺为功能单体,苯霜灵(Ben)为模板分子,在石墨烯修饰的丝网印刷电极表面,通过紫外引发聚合形成能识别苯霜灵分子的印迹敏感膜,采用循环伏安法、差分脉冲伏安法研究了印迹膜的结构、性能和分子印迹效应。该传感器对Ben的检测浓度范围为7.0×10~(–9)～6.8×10~(–4) mol/L,Ben的检出限为2.1×10~(–9) mol/L,测定结果的相对标准偏差不大于3.21%(n=5),加标回收率为101.7%～110.4%。该方法可用于烟草中苯霜灵的测定。
A screen printing electrode was fabricated for rapid determination of benalaxyl(Ben)in tobacco based on graphene modified molecular inprinting membrane screen printing electrode.The sensor was prepared by ultraviolet polymerization on the surface of graphene modified screen printing electrode with Ben as template.The structure,properties and molecular imprinting effect of the imprinted membrane were studied by CV and DPV.The sensor was used to determine benalaxyl whose linear range was 7.0×10~(–9)–6.8×10~(–4) mol/L with the detection limit of 2.1×10~(–9) mol/L.The relative standard deviations of the detection data were not more than 3.21%(n=5),and the recoveries of benalaxyl were 101.7%–110.4%.The method can be applied to the determination of benalaxyl in different tobacco samples.
A screen printing electrode was fabricated for rapid determination of benalaxyl(Ben)in tobacco based on graphene modified molecular inprinting membrane screen printing electrode.The sensor was prepared by ultraviolet polymerization on the surface of graphene modified screen printing electrode with Ben as template.The structure,properties and molecular imprinting effect of the imprinted membrane were studied by CV and DPV.The sensor was used to determine benalaxyl whose linear range was 7.0×10~(–9)–6.8×10~(–4) mol/L with the detection limit of 2.1×10~(–9) mol/L.The relative standard deviations of the detection data were not more than 3.21%(n=5),and the recoveries of benalaxyl were 101.7%–110.4%.The method can be applied to the determination of benalaxyl in different tobacco samples.
引文
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[3]RAMIREZ RESTREPO A,GALLO ORTIZA F,HOYOS OSSAD E,et al.QuEChERS GC-MS validation and monitoring of pesticide residues in different foods in the tomato classification group[J].Food Chem,2014,158:153-161.
[4]PANO-FARIAS N S,CEBALLOS-MAGANA S G,MUNIZ-VALENCIA R,et al.Direct immersion single drop microextraction method for multi-class pesticides analysis in mango using GC-MS[J].Food Chem,2017,237:30-38.
[5]王鹏,刘东晖,王玉红,等.高效液相色谱法拆分苯霜灵对映体分析化学[J].2006,34(11):1 524-1 528.
[6]FU L,LU X,TAN J,et al.Multi-residue determination and potential risks of emerging pesticides in aquatic products from Northeast China by LC-MS/MS[J].J Environ Sci(China),2018,63:116-125.
[7]倪永付,朱涛,朱莉萍,等.搅拌棒萃取LC-MS/MS法检测大蒜中苯霜灵、扑灭津、哒螨灵及吡螨胺残留[J].食品与发酵科技,2016,52(3):103-105,110.
[8]朱莉萍,高坤,朱涛,等.液相色谱一电喷雾串联质谱测定蔬菜及其制品中苯霜灵等5种农药残留量[J].分析测试学报,2012,31:12-14.
[9]GARCIA M D,DUQUE S U,FERNANDEZ A B,et al.Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS[J].Talanta,2017,163:54-64.
[10]PALENIKOVA A,MARTINEZ-DOMINGUEZ G,ARREBOLAF J,et al.Multiresidue method for trace pesticide analysis in honeybee wax comb by GC-QqQ-MS[J].Food Chem,2015,173:796-807.
[11]Nieto-García,Antonio José,Romero-González,et al.Multifamily determination of pesticide residues in soya-based nutraceutical products by GC/MS-MS[J].Food Control,2015,47:369-380.
[12]YANG L,YANG J,XU B J,et al.Multi-pesticide residue analysis in nutraceuticals from grape seed extracts by gas chromatography coupled to triple quadrupole mass spectrometry[J].Talanta,2016,161:413-418.
[13]陈晓,谭学才,严军,等.3D石墨烯修饰的猛杀威分子印迹电化学传感器的制备[J].分析化学,2016,44(12):1 834-1 839.
[14]LI J B,WANG X J,DUAN H M,et al.Based on magnetic graphene oxide highly sensitive and selective imprinted sensor for determination of sunset yellow[J].Talanta,2016,147:169-176.
[15]KONG L,JIANG X Y,ZENG Y B,et al.Molecularly imprinted sensor based on electropolmerizedpoly(o-phenylenediamine)membranes at reduced graphene oxide modified electrode for imidacloprid determination[J].Sens Actuators B,2013,185:424-431.