基于磁固相萃取-便携式离子阱质谱的蔬菜中3种农药残留的快速检测  

Rapid detection of three pesticide residues in vegetables based on magnetic solid phase extraction and portable ion trap mass spectrometer

作　　者：陈庭男 齐沛沛[2] 华修德[1] 王鸣华[1] 何吉 闻路红 章文天 王新全 CHEN Tingnan;QI Peipei;HUA Xiude;WANG Minghua;HE Ji;WEN Luhong;ZHANG Wentian;WANG Xinquan(School of Plant Protection,Nanjing Agricultural University,Nanjing 210095,China;Institute of Quality Safety and Nutrition of Agro-products,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China;China Innovation Instrument Co.,Ltd.,Ningbo 315100,Zhejiang Province,China)

机构地区：[1]南京农业大学植物保护学院,南京210095 [2]浙江省农业科学院农产品质量安全与营养研究所,杭州310021 [3]宁波华仪宁创智能科技有限公司,浙江宁波315100

出　　处：《农药学学报》2023年第5期1165-1172,共8页Chinese Journal of Pesticide Science

基　　金：浙江省重点研发计划项目(2020C02023).

摘　　要：针对当前我国典型的高风险蔬菜芹菜、韭菜和豇豆中易超标农药啶虫脒、吡虫啉及禁限用农药克百威的残留问题,基于磁固相萃取和便携式离子阱质谱构建了多农药残留现场、快速检测技术。系统优化了磁固相萃取方法的关键影响因素,最佳优化条件为:2 g蔬菜样品经20 mL水萃取后,采用30 mg磁固相吸附剂,超声辅助吸附水溶液中目标农药15 min,再用4 mL体积分数为0.1%的甲酸乙腈超声解吸附3 min后进行便携式质谱分析。方法验证结果表明:啶虫脒、吡虫啉及克百威3种农药在芹菜、韭菜和豇豆样品基质溶液中的线性范围为0.01~0.25 mg/L(除吡虫啉在韭菜中的线性范围为0.05~0.5 mg/L外);检出限均为0.001~0.035 mg/L,定量限均为0.02~0.05 mg/kg;在0.02、0.05和0.2 mg/kg 3个添加水平下时,3种农药的回收率在50%~71%之间,相对标准偏差在4.2%~22%之间。该方法具有较好正确度、精密度和操作便捷等优势,在蔬菜中多种农药残留的快速定性/半定量筛查方面具有广阔的应用前景。A rapid method was established for the detection of acetamiprid,imidacloprid and carbofuran in three typically high residue vegetables,including celery,leek and cowpea,using magnetic solid-phase extraction and portable ion trap mass spectrometer.The main extraction conditions were optimized and the suitable procedures were as follows:The vegetable samples were extracted by 20 mL water,and the target pesticides in the extracted solution was then adsorbed by 30 mg magnetic solid-phase absorbents using the ultrasonic extraction for 15 min.After the magnetic separation,the adsorbed pesticides were desorbed with 4 mL of acetonitrile with 0.1%(V/V)formic acid by ultrasonic extraction for 3 min.Method validation indicated that all the three pesticides showed good linearity in the range of 0.01-0.25 mg/L,except that it was 0.05-0.5 mg/L for imidacloprid in leek sample.The limits of detection were 0.001-0.035 mg/L,and the limits of quantitation were 0.02-0.05 mg/kg.The spiked recoveries ranged from 50%to 71%with the RSDs of 4.2%to 22%at the spiked levels of 0.02,0.05 and 0.2 mg/kg.The presented method displayed good qualitative/semi quantitative ability,and could be used for simultaneous and rapid on-site detection of multiple pesticide residues in vegetables.

关 键 词：磁固相萃取 便携式离子阱质谱 蔬菜 农药多残留 快速检测 

分 类 号：TQ450.2[化学工程—农药化工]