[目的]开发同时检测生乳中吡虫啉(Imidacloprid)、吡唑醚菌酯(Pyrazole ether ester)、氟虫腈(Fluorine worm nitrile)3 种农药残留的胶体金免疫层析的方法。[方法]采用柠檬酸三钠还原法制备胶体金溶液,冻干法制备胶体金标抗体冻干粉,置于微孔杯内,复溶后,吸取全部反应液于胶体金试纸条样品垫上,经层析,在免疫层析试纸条上显示结果。[结果]吡虫啉、吡唑醚菌酯、氟虫腈3 种农药检测检测下限分别为0.1 mg/kg,0.03mg/kg,0.02 mg/kg,保质期为1 年,符合《GB27632021食品安全国家标准 食品中农药最大残留限量》对生乳中农药残留做出明确限量规定吡虫啉、吡唑醚菌酯、氟虫腈最大残留量0.1 mg/kg,0.03 mg/kg,0.02 mg/kg要求。[结论]该方法操作简单,快速灵敏,稳定准确,可以作为前期农残检测的快速筛查手段。
[Objective] To develop a colloidal gold immunochromatography method for simultaneous detection of Imidacloprid,Pyrazole ether ester and Fluorine worm nitrile residues in raw milk. [Method] The colloidal gold solution was prepared by trisodium citrate reduction method, and the colloidal gold standard antibody lyophilized powder was prepared by lyophilization method. The powder was placed in a microporous cup,and the reaction solution was absorbed on the sample pad of colloidal gold test strip after resolution. [Result] The sensitivity of three pesticides,imidacloprid,pyrazoline and fipronil,were 0.1 mg/kg, 0.03mg/kg and 0.02 mg/kg,respectively. The shelf life was 1 year. In accordance with GB2763-2021 National Food Safety Standard Maximum Residue Limits for Pesticides in Food,the maximum residue limits of imidacloprid,pyrazolylosteril and fipronil in raw milk are specified to be 0.1mg/kg,0.03mg/kg and 0.02mg/kg respectively. [Conclusion] This method is simple, rapid,sensitive,stable and accurate,and can be used as a rapid screening method for early detection of agricultural residues.
[1] 王刚,毛华明,刘树民,等.牛奶中农药残留研究进展及其HACCP控制体系的确立[J].中国乳业,2005(12):28-31.
[2] 宋瑶,刘畅,朱敏,等.气相色谱法测定酸奶中4种拟除虫菊酯农药的残留[J]. 中国乳品工业,2016,44(7):44-46.
[3] Martha Z,Laura Y G,Milton R M,et al.Multi-residue analysis of pesticides in blood plasma using hollow fiber solvent bar microextraction and gas chromatography with a flame ionization detector[J]. Environmental Toxicology and Pharmacology,2021,82:1-8.
[4] Li B,Zeng F G,Dong Q C,et al.Rapid determination method for 12 pyrethroid pesticide residues in tea by stir bar sorptive extraction-thermal desorption-gas dhromatography[J]. Physics Procedia,2012,25:776-1780.
[5] Rajput S,Kumari A,Arora S,et al.Multi-residue pesticides analysis in water samples using reverse phase high performance liquid chromatography(RP-HPLC)[J]. MethodsX,2018,5:744-751.
[6] Harshit D,Charmy K,Nrupesh P.Organophosphorus pesticides determination by novel HPLC and spectrophotometric method[J].Food chemistry,2017,230:448-453.
[7] 陈锦杭,冯城婷,林秋凤,等. QuEChERS-固相萃取-气相色谱/四极杆飞行时间质谱法快速测定牛奶中的11种有机磷[J].中国乳品工业, 2021,49(1):51-54.
[8] Rakesh K G,Sujan M,Arijita B,et al.Introducing a low-cost jute activated carbon as a novel cleanup agent in multiclass pesticide residue analysis using gas chromatography tandem mass spectrometry[J]. Journal of Cleaner Production, 2021,319(15):1-12
[9] 蔡光辉, 李萌, 吴绪金,等.吡唑醚菌酯在杨桃中残留检测及膳食风险评估[J]. 食品安全质量检测学报, 2021,12(14):5532-5538.
[10] Silva R D O,Menezes M G G D,Castro R C D,et al. Efficiency of ESI and APCI ionization sources in LC-MS/MS systems for analysis of 22 pesticide residues in food matrix[J],Food Chemistry,2019,297,1-6.
[11] Cong C Y,Dong Y H,Qiao C,et al.A one adsorbent QuEChERS method coupled with LC-MS/MS for simultaneous determination of 10 organophosphorus pesticide residues in tea[J], Food Chemistry,2020, 321, 126657.
[12] Guoliang Q,Limin W,Yunru W,et al.A monoclonal antibody-based sensitive enzyme-linked immunosorbent assay (ELISA) for the analysis of the organophosphorous pesticides chlorpyrifos-methyl in real samples[J],Food Chemistry,2009,117(2):364-370.
[13] 朱亮亮,王琳琛,王兆芹,等.检测4种有机磷农药胶体金免疫层析试纸条的研制[J]. 山东畜牧兽医,2019,40(8):10-12.
[14] 施诚愿张俊聪. 金标检测卡对蔬菜上多菌灵和啶虫脒农药残留快速检测的效果[J]. 上海蔬菜,2020(2):76-77.
[15] 冯月君,张瑜,万宇平,等. 一种异丙威胶体金免疫快速检测试纸条的研制[J]. 中国酿造,2020,39(1):194-197.
[16] 高思远,李丽娅,孟利 .农药残留免疫分析技术研究进展[J].食品工业科技,2019,40(22):346-353.
[17] Frens G.Particle size and sol stability in metal colloids[J]. Colloid-Z.u.Z.Polymere,1972,250(7):736-741.
[18] Frens G.Controlled nucleation for the rrgulation of the particle size in monodisperse gold suspensions[J]. Nature Physical Science,1973,241(1):20-22.
[19] 周佳,何丹,王炳志,等. 胶体金免疫层析法同时检测果蔬中克百威、水胺硫磷、百菌清及虫酰肼的应用研究[J]. 食品安全质量检测学报, 2021,12(19):7607-7610.
[20] 陈美莲,章慧,丰东升,等. 胶体金法快速检测蔬菜中多菌灵·吡虫啉和啶虫脒的应用研究[J]. 安徽农业科学, 2020,48(22):193-197.
[21] 国家标准化管理委员会,国家质量监督检验检疫总局. GB/T 23379-2009 中国标准书号[S].
[22] 农业部,国家食品药品监督管理总局,国家卫生和计划生育委员会. GB 23200.34-2016 中国标准书号[S].
[23] 国家质量监督检验检疫总局. SN/T1982-2007 中国标准书号[S].