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拟除虫菊酯类杀虫剂在烟叶烘烤过程中的消解动态与最终残留
引用本文:杨立强,徐光军,闫晓阳,徐金丽,郑晓,宋超,周杨全,孙惠青,王秀国,李义强.拟除虫菊酯类杀虫剂在烟叶烘烤过程中的消解动态与最终残留[J].农药学学报,2013,15(5):534-540.
作者姓名:杨立强  徐光军  闫晓阳  徐金丽  郑晓  宋超  周杨全  孙惠青  王秀国  李义强
作者单位:1.中国农业科学院 烟草研究所/烟草行业烟草病虫害监控与综合治理重点实验室, 山东 青岛 266101
基金项目:国家烟草专卖局重点项目(TS-06-20110039;110200902073).
摘    要:采用气相色谱-质谱联用技术,测定了良好农业规范(GAP)条件下3种常用拟除虫菊酯类杀虫剂高效氯氟氰菊酯、高效氯氰菊酯及溴氰菊酯在山东、四川、云南、辽宁和江西5地烟叶中的消解动态及最终残留。样品经乙腈提取,SPE-PSA柱净化,气-质联用、选择离子监测模式(GC-MS/SIM)下测定,外标法定量。结果表明:在0.01 ~1 mg/kg添加水平下,3种农药在鲜烟叶和干烟叶中的平均回收率分别在82.9% ~ 110.9%和85.2%~108.3%之间,相对标准偏差(RSD)分别为1.7% ~4.4%和2.3% ~5.7%;3种农药在鲜烟叶和干烟叶中的定量限(LOQ)均为0.01mg/kg;方法的准确度和精密度均符合农药残留检测要求。烘烤过程中残留农药消解明显,高效氯氟氰菊酯、高效氯氰菊酯和溴氰菊酯的消解率分别高达78%、89%和91%。高效氯氟氰菊酯、高效氯氰菊酯和溴氰菊酯乳油分别按有效成分450~675 g/hm2、600~900 g/hm2及450~675 g/hm2于烟叶采 烤初期喷雾施药2次,距末次施药后14d,干烟叶中3种农药的残留量分别为0.022~ 0.50、0.14~0.82和0.046~0.21 mg/kg,均低于国际烟草合作研究中心(CORESTA)提出的指导性农药残留限量标准(GRL)值(0.5、1和1mg/kg),因此建议其安全间隔期可定为14d。

关 键 词:拟除虫菊酯    杀虫剂    烟叶    烘烤    残留    消解动态
收稿时间:2013/5/22 0:00:00
修稿时间:9/3/2013 12:00:00 AM

Residues and decline dynamics of pyrethroid insecticides in tobacco leaf during curing
YANG Liqiang,XU Guangjun,YAN Xiaoyang,XU Jinli,ZHENG Xiao,SONG Chao,ZHOU Yangquan,SUN Huiqing,WANG Xiuguo and LI Yiqiang.Residues and decline dynamics of pyrethroid insecticides in tobacco leaf during curing[J].Chinese Journal of Pesticide Science,2013,15(5):534-540.
Authors:YANG Liqiang  XU Guangjun  YAN Xiaoyang  XU Jinli  ZHENG Xiao  SONG Chao  ZHOU Yangquan  SUN Huiqing  WANG Xiuguo and LI Yiqiang
Institution:1.Tobacco Research Institute of CAAS/Key Laboratory of Tobacco Pest Monitoring Controlling & Integrated Management, Qingdao 266101, Shandong Province, China
Abstract:A GC-MS method was developed for the simultaneous determination of pyrethroid insecticides in tobacco leaf in Shandong,Sichuan,Yunnan,Liaoning and Jiangxi,under the good agricultural practices conditions.Tobacco leaf samples were extracted with acetonitrile and cleaned-up by SPE-PSA,then detected by GC-MS/SIM with external standard method.The average recoveries ranged from 82.9% to 110.9% with relative standard deviations (RSD) from 1.7% to 4.4% in fresh tobacco leaves and from 85.2% to 108.3% with RSD from 2.3% to 5.7% in cured tobacco leaves at 0.01,0.1 and 1 mg/kg,respectively.The limits of quantification (LOQ) of three pyrethroid insecticides were 0.01 mg/kg.The sensitivity and accuracy of the current method was suitable for analysis of target pesticide residues.Dissipation of three pyrethroid insecticides was significant after flue-curing,and the decline rates of lambda-cyhalothrin,beta-cypermethrin and deltamethrin were 78%,89%,91%.The residues of lambda-cyhalothrin,beta-cypermethrin and deltamethrin in cured tobacco leaves were determined after two applications at levels of 450-675 g/hm2,600-900 g/hm2 and 450-675 g/hm2,with residues ranged from 0.022-0.50 mg/kg,0.14-0.82 mg/kg and 0.046-0.21 mg/kg in tobacco 14 days after the last application,lower than GRLs(0.5,1 and 1 mg/kg).According to these findings,a prehavest interval of 14 days was recommended.
Keywords:pyrethroid  insecticide  tobacco leaf  flue-curing  residue  decline dynamics
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