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

    Residues and decline dynamics of pyrethroid insecticides in tobacco leaf during curing

    • 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。

       

      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.

       

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