戊唑醇及吡唑醚菌酯在玉米上的残留行为及风险评估  

Residue behavior and dietary risk assessment of tebuconazole and pyraclostrobin in corn

作　　者：齐艳丽 李晋栋 高婧 李春勇 任鹏程 宋晋雄 王霞[1] 乔雄梧[1] 秦曙[1] QI Yanli;LI Jindong;GAO Jing;LI Chunyong;REN Pengcheng;SONG Jinxiong;WANG Xia;QIAO Xiongwu;QIN Shu(Institute of Quality,Safety of Agro-Products and Testing Technology,Shanxi Academy of Agricultural Sciences,Laboratory of Quality and Safety Risk Assessment for Agro-Products(Taiyuan),Ministry of Agriculture and Rural Affairs,Taiyuan 030031,China)

机构地区：[1]山西省农业科学院农产品质量安全与检测研究所,农业农村部农产品质量安全风险评估实验室(太原),太原030031

出　　处：《农药学学报》2020年第1期115-121,共7页Chinese Journal of Pesticide Science

基　　金：山西省农业科学院博士研究基金(YBSJJ1801);2017年政府购买科技公共服务项目“农产品质量安全风险监测及评估”。

摘　　要：建立了玉米及其秸秆中戊唑醇和吡唑醚菌酯残留的分析方法。样品经乙腈提取,N-丙基乙二胺(PSA)和C18净化,利用超高效液相色谱-串联三重四极杆质谱仪(UPLC-MS/MS)检测。结果表明:在0.0025~0.1 mg/L范围内,戊唑醇及吡唑醚菌酯的峰面积与其质量浓度间呈良好的线性关系,R^2均大于0.99。鲜食玉米及成熟玉米籽粒在0.01、0.1和1 mg/kg,青玉米秸秆在0.01、0.1和2 mg/kg,成熟玉米秸秆在0.02、0.2和6 mg/kg添加水平下,戊唑醇在玉米及其秸秆中的添加回收率在75%~101%之间,相对标准偏差(RSD)在1.3%~6.0%之间;吡唑醚菌酯在玉米及其秸秆中的添加回收率在76%~101%之间,RSD在2.1%~8.4%之间。30%戊唑醇·吡唑醚菌酯悬浮剂以有效成分180 g/hm^2剂量施药3次,分别于末次施药后21和28 d采集的鲜食玉米及成熟玉米籽粒中,戊唑醇和吡唑醚菌酯残留量均低于定量限(0.01 mg/kg),也低于CAC、EU和EPA的最大残留限量值(MRL)。膳食风险评估结果表明:一般人群戊唑醇的国家估算每日摄入量为0.1545 mg,占日允许摄入量的8.2%;一般人群吡唑醚菌酯的国家估算每日摄入量为0.45 mg,占日允许摄入量的24.0%。因此,建议在玉米上使用30%戊唑醇·吡唑醚菌酯悬浮剂时,最高施药剂量为有效成分180 g/hm^2,最多施药3次,施药间隔为7 d,安全间隔期为21 d。A high efficient and simple methods for residue analysis of tebuconazole and pyraclostrobin in corn and stover(forage)were developed.The samples were extracted with acetonitrile,purified with primary secondary amine(PSA)and C18,and detected by ultra performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS).The results showed that all the correlation coefficient of calibration curves were over 0.99 in ranged of 0.0025 to 0.1 mg/L.At three spiked concentration levels,the average recoveries of the tebuconazole varied from 75% to 101% with the relative standard deviations(RSDs)ranging from 1.3%to 6.0%;the average recoveries of the pyraclostrobin varied from76%to 101% with the RSDs ranging from 2.1% to 8.4%.The 30% suspension concentrate(SC)of tebuconazole·pyraclostrobin was sprayed at 180 g a.i./ha for 3 times on corn.The residue of tebuconazole and pyraclostrobin in corn were less than 0.01 mg/kg at day 21 and 28 after the last application,which were below the maximum residue limits(MRLs)for tebuconazole and pyraclostrobin in the Codex Alimentarius Commission(CAC),European Union(EU)and Environmental Protection Agency(EPA).For general population,the national estimated daily intake of tebuconazole was 0.1545 mg,accounting for 8.2%of the acceptable daily intake.The national estimated daily intake of pyraclostrobin was 0.45 mg,accounting for 24.0% of the acceptable daily intake.Thus,the dosage of 180 g a.i./ha for tebuconazole·pyraclostrobin 30%SC was recommended on corn with the preharvest interval at 21 days,and maximum application of three times with a 7-day interval between the sprays.

关 键 词：戊唑醇 吡唑醚菌酯 玉米 残留 风险评估 超高效液相色谱-串联三重四极杆质谱 

分 类 号：TQ450.26[化学工程—农药化工]