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联苯菊酯、噻虫嗪及其代谢物噻虫胺在小麦上的残留及膳食风险评估

吕莹 齐艳丽 任鹏程 连少博 王霞 秦曙

吕莹, 齐艳丽, 任鹏程, 连少博, 王霞, 秦曙. 联苯菊酯、噻虫嗪及其代谢物噻虫胺在小麦上的残留及膳食风险评估[J]. 农药学学报, 2021, 23(2): 366-372. doi: 10.16801/j.issn.1008-7303.2021.0052
引用本文: 吕莹, 齐艳丽, 任鹏程, 连少博, 王霞, 秦曙. 联苯菊酯、噻虫嗪及其代谢物噻虫胺在小麦上的残留及膳食风险评估[J]. 农药学学报, 2021, 23(2): 366-372. doi: 10.16801/j.issn.1008-7303.2021.0052
Ying LYU, Yanli QI, Pengcheng REN, Shaobo LIAN, Xia WANG, Shu QIN. Residue behavior and dietary risk assessment of bifenthrin, thiamethoxam and clothianidin in wheat[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 366-372. doi: 10.16801/j.issn.1008-7303.2021.0052
Citation: Ying LYU, Yanli QI, Pengcheng REN, Shaobo LIAN, Xia WANG, Shu QIN. Residue behavior and dietary risk assessment of bifenthrin, thiamethoxam and clothianidin in wheat[J]. Chinese Journal of Pesticide Science, 2021, 23(2): 366-372. doi: 10.16801/j.issn.1008-7303.2021.0052

联苯菊酯、噻虫嗪及其代谢物噻虫胺在小麦上的残留及膳食风险评估

doi: 10.16801/j.issn.1008-7303.2021.0052
基金项目: 山西省财政厅政府购买科技公共服务项目 (晋财教[2017]357号);农业行业标准制定和修订项目
详细信息
    作者简介:

    吕莹,女,本科,研究方向为农药残留和农产品质量安全,E­mail:609963949@qq.com

    通讯作者:

    秦曙,通信作者 (Author for correspondence),女,研究员,研究方向为农药残留和农产品质量安全,E­mail:qinshu55@126.com

  • 中图分类号: S482.3;TQ450.26;O657.63

Residue behavior and dietary risk assessment of bifenthrin, thiamethoxam and clothianidin in wheat

  • 摘要: 建立了小麦及其秸秆中联苯菊酯、噻虫嗪和代谢物噻虫胺残留量的分析方法。样品经乙酸-乙腈提取,无水硫酸镁、N-丙基乙二胺 (PSA) 及GCB净化,超高效液相色谱-三重四极杆串联质谱仪 (UPLC-MS/MS) 检测。结果表明:在0.0025~0.1 mg/L范围内,联苯菊酯、噻虫嗪和噻虫胺的峰面积与其质量浓度间呈良好线性关系,R2均大于0.99。麦粒样品在0.01、0.1和0.5 mg/kg,秸秆样品在0.05、0.5和3 mg/kg添加水平下,联苯菊酯、噻虫嗪和噻虫胺在小麦及其秸秆中的添加回收率分别在93%~98%、87%~98%和87%~98%之间,相对标准偏差 (RSD) 分别在0.8%~4.8%、0.6%~4.1%和1.0%~3.3%之间。按照《农作物中农药残留试验准则》在全国12个小麦主产区开展规范残留试验,采用35%联苯菊酯 • 噻虫嗪悬浮剂,以制剂用量150 g/hm2 (有效成分52.5 g/hm2) 的剂量,于小麦蚜虫始盛时期施药1次,施药后间隔14 d和21 d采集的麦粒中联苯菊酯、噻虫嗪和噻虫胺的残留量结果验证了相关残留限量 (MRL) 值的适用性,且多点试验的结果具有更高的可靠性。长期及短期膳食暴露风险评估结果表明,小麦中联苯菊酯、噻虫嗪和噻虫胺残留量对1~6岁儿童和普通人群产生的膳食暴露风险在可接受范围内。
  • 1  联苯菊酯、噻虫嗪及噻虫胺结构式

    1.  The structural formula of bifenthrin, thiamethoxam and clothianidin

    表  1  联苯菊酯、噻虫嗪和噻虫胺主要质谱参数

    Table  1.   The major MS parameters of bifenthrin, thiamethoxam and clothianidin

    化合物
    Compound
    保留时间
    Retention time/min
    母离子
    Parent ion
    子离子
    Daughter ion
    锥孔电压
    Cone voltage/V
    碰撞能量
    Collision energy/eV
    联苯菊酯 bifenthrin  6.20 439.8 180.9a 12 26
    165.7b 12 58
    噻虫嗪 thiamethoxam 2.45 291.9 210.9a 30 10
    132.0b 30 22
    噻虫胺 clothianidin  2.71 249.9 168.9a 16 12
    132.0b 16 12
    注:a 定量离子,b 定性离子。Note: a quantitative ion, b qualitative ion.
    下载: 导出CSV

    表  2  联苯菊酯、噻虫嗪和噻虫胺在小麦中的添加回收率及相对标准偏差

    Table  2.   The recoveries and RSD of bifenthrin, thiamethoxam and clothianidin in wheat

    基质
    Matrix
    添加水平
    Spiked level/ (mg/kg)
    联苯菊酯 bifenthrin噻虫嗪 thiamethoxam噻虫胺 clothianidin
    平均回收率
    Average recoveries/%
    相对标准偏差
    RSD/%
    平均回收率
    Average recoveries/%
    相对标准偏差
    RSD/%
    平均回收率
    Average recoveries/%
    相对标准偏差
    RSD/%
    麦粒 Wheat grain 0.01 95 4.8 97 0.6 95 1.0
    0.1 93 2.5 97 1.7 98 1.1
    0.5 94 0.8 98 1.3 98 1.1
    秸秆 Wheat-straw 0.05 98 3.3 87 4.1 87 3.3
    0.5 95 2.6 90 3.7 88 2.9
    3 97 2.8 90 1.1 91 1.0
    下载: 导出CSV

    表  3  联苯菊酯、噻虫嗪和噻虫胺在小麦中的残留量

    Table  3.   Residues of bifenthrin, thiamethoxam and clothianidin in wheat

    试验点 Test site联苯菊酯残留量
    Residues of bifenthrin
    噻虫嗪残留量
    Residues of thiamethoxam
    噻虫胺残留量
    Residues of clothianidin
    14 d 21 d 14 d 21 d 14 d 21 d
    北京市 Beijing 0.010 < LOQ < LOQ < LOQ < LOQ < LOQ
    < LOQ < LOQ < LOQ < LOQ < LOQ < LOQ
    上海市 Shanghai 0.019 0.019 < LOQ < LOQ < LOQ < LOQ
    0.023 0.016 < LOQ < LOQ < LOQ < LOQ
    山东省 Shandong Province 0.010 0.010 < LOQ < LOQ < LOQ < LOQ
    0.011 0.011 < LOQ < LOQ < LOQ < LOQ
    山西省 Shanxi Province 0.025 0.011 < LOQ < LOQ < LOQ < LOQ
    0.016 0.017 < LOQ < LOQ < LOQ < LOQ
    吉林省 Jilin Province 0.010 < LOQ < LOQ < LOQ < LOQ < LOQ
    0.010 < LOQ < LOQ < LOQ < LOQ < LOQ
    安徽省 Anhui Province 0.018 < LOQ < LOQ < LOQ 0.012 < LOQ
    0.019 < LOQ < LOQ < LOQ 0.014 < LOQ
    河南省 Henan Province 0.028 0.027 < LOQ < LOQ 0.013 < LOQ
    0.028 0.030 < LOQ < LOQ 0.013 < LOQ
    天津市 Tianjin < LOQ < LOQ < LOQ < LOQ < LOQ < LOQ
    < LOQ < LOQ < LOQ < LOQ < LOQ < LOQ
    云南省 Yunnan Province 0.030 0.024 0.016 < LOQ 0.010 < LOQ
    0.033 0.026 0.014 < LOQ < LOQ < LOQ
    四川省 Sichuan Province 0.012 0.010 < LOQ < LOQ 0.018 < LOQ
    0.012 0.010 < LOQ < LOQ 0.018 < LOQ
    江苏省 Jiangsu Province 0.026 0.040 < LOQ < LOQ < LOQ < LOQ
    0.025 0.041 < LOQ < LOQ < LOQ < LOQ
    湖北省 Hubei Province < LOQ < LOQ < LOQ < LOQ < LOQ < LOQ
    < LOQ < LOQ < LOQ < LOQ < LOQ < LOQ
    最大值 Max 0.033 0.041 0.016 0.010 0.018 0.010
    最小值 Min 0.010 0.010 0.010 0.010 0.010 0.010
    残留中值 STMR 0.014 0.010 0.010 0.010 0.010 0.010
    平均值 Average 0.017 0.016 0.010 0.010 0.011 0.010
    标准差 STDEVP 0.0078 0.0096 0.0014 0 0.0024 0
    95% 置信区间计算公式
    95% confidence interval calculation formula
    $ \left[\mu {-1}{.96}\times \dfrac{\delta }{\sqrt{{n}}},\;\mu +{1}{.96}\times \dfrac{\delta }{\sqrt{{n}}}\right]$
    µ 为均值,δ 为标准差,n 为样本数量 µ is the mean, δ is the standard deviation, and n is the sample size
    95% 置信区间上限值
    The upper limit of the 95% confidence interval
    0.020 0.020 0.010 0.010 0.012 0.010
    下载: 导出CSV
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  • 收稿日期:  2020-04-29
  • 录用日期:  2020-12-17
  • 刊出日期:  2021-04-10

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