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噁唑酰草胺及其代谢物在水稻上的残留

何红梅 徐玲英 张昌朋 王祥云 李艳杰 赵学平

何红梅, 徐玲英, 张昌朋, 王祥云, 李艳杰, 赵学平. 噁唑酰草胺及其代谢物在水稻上的残留[J]. 农药学学报, 2022, 24(2): 385-394. doi: 10.16801/j.issn.1008-7303.2021.0185
引用本文: 何红梅, 徐玲英, 张昌朋, 王祥云, 李艳杰, 赵学平. 噁唑酰草胺及其代谢物在水稻上的残留[J]. 农药学学报, 2022, 24(2): 385-394. doi: 10.16801/j.issn.1008-7303.2021.0185
HE Hongmei, XU Lingying, ZHANG Changpeng, WANG Xiangyun, LI Yanjie, ZHAO Xueping. Residues of metamifop and its metabolites in paddy rice[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 385-394. doi: 10.16801/j.issn.1008-7303.2021.0185
Citation: HE Hongmei, XU Lingying, ZHANG Changpeng, WANG Xiangyun, LI Yanjie, ZHAO Xueping. Residues of metamifop and its metabolites in paddy rice[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 385-394. doi: 10.16801/j.issn.1008-7303.2021.0185

噁唑酰草胺及其代谢物在水稻上的残留

doi: 10.16801/j.issn.1008-7303.2021.0185
基金项目: 浙江省分析测试基金项目 (2018C37013).
详细信息
    通讯作者:

    何红梅,hehongmei53@163.com.

  • 中图分类号: TQ450.2;O657.63

Residues of metamifop and its metabolites in paddy rice

Funds: The Analysis and Testing Technology Projects of Zhejiang (2018C37013).
  • 摘要: 为探明噁唑酰草胺及其3个代谢物 (N-(2-氟苯基)-2-(4-羟基苯氧基)-N-甲基丙酰胺(HPFMPA)、N-(2-氟苯基)-2-羟基-N-甲基丙酰胺(HFMPA)和6-氯-苯并噁唑酮(6-CBO)) 在水稻上的最终残留量,在我国10个主要水稻产区开展了噁唑酰草胺的田间残留试验。建立了糙米、稻壳和稻秆中噁唑酰草胺及其代谢物残留量的检测方法,评估了方法的基质效应。样品经乙腈提取、盐析、C18固相萃取小柱净化后采用超高效液相色谱-串联质谱法 (UPLC-MS/MS) 测定,6-CBO采用电喷雾负离子模式,其他采用电喷雾正离子模式。糙米、稻壳和稻秆中3档添加水平 (0.01、0.1和2.0 mg/kg) 下的平均回收率为79%~108%,相对标准偏差为0.9%~10.8%。噁唑酰草胺及其代谢物在糙米、稻壳和稻秆中的定量限(LOQ)均为0.01 mg/kg,在0.0005~0.02 mg/L质量浓度范围内,溶剂标准曲线和基质匹配标准曲线的线性关系均良好 (r>0.9941),无明显基质效应。残留试验结果表明:噁唑酰草胺及其代谢物在糙米和稻壳中的残留量均<0.01 mg/kg,糙米中的残留量低于我国最大残留限量 (MRL) 值 (0.05 mg/kg);HFMPA在稻秆中的残留量为<0.01~0.098 mg/kg,其余3个化合物在稻秆中的残留量均低于LOQ。建议20% 噁唑•灭草松微乳剂 (ME,其中噁唑酰草胺质量分数为3.3%) 在水稻上施用时,可按最高施药剂量 (有效成分720 g/hm2,噁唑酰草胺为118.8 g/hm2 ) 施药1次。
  • 1  噁唑酰草胺及其3个代谢物的结构式

    1.  The structural formula of metamifop and its metabolites HPFMPA, HFMPA and 6-CBO

    图  1  噁唑酰草胺色谱图

    A-1~A-7分别为标样 (0.00167 mg/L) 、糙米空白及添加 (0.01 mg/kg) 、稻壳空白及添加 (0.01 mg/kg) 和稻秆空白及添加 (0.01 mg/kg) 色谱图。

    Figure  1.  Chromatograms of metamifop

    Chromatograms of metamifop (A-1~A-7, standard of 0.00167 mg/L, brown rice blank and spiked (0.01 mg/kg), paddy hull blank and spiked (0.01 mg/kg),rice straw blank and spiked (0.01mg/kg).

    图  4  6-CBO色谱图

    D-1~D-7分别为标样 (0.00167 mg/L) 、糙米空白及添加 (0.01mg/kg) 、稻壳空白及添加 (0.01mg/kg) 和稻秆空白及添加 (0.01mg/kg) 色谱图。

    Figure  4.  Chromatograms of 6-CBO

    Chromatograms of 6-CBO (D-1~D-7, standard of 0.00167 mg/L, brown rice blank and spiked (0.01mg/kg), paddy hull blank and spiked (0.01mg/kg),rice straw blank and spiked (0.01mg/kg).

    图  2  HPFMPA色谱图

    B-1~B-7分别为标样 (0.00167 mg/L) 、糙米空白及添加 (0.01 mg/kg) 、稻壳空白及添加 (0.01 mg/kg) 和稻秆空白及添加 (0.01 mg/kg) 色谱图。

    Figure  2.  Chromatograms of HPFMPA

    Chromatograms of HPFMPA (B-1~B-7, standard of 0.00167 mg/L, brown rice blank and spiked (0.01 mg/kg), paddy hull blank and spiked (0.01 mg/kg),rice straw blank and spiked (0.01 mg/kg).

    图  3  HFMPA色谱图

    C-1~C-7分别为标样 (0.00167 mg/L) 、糙米空白及添加 (0.01 mg/kg) 、稻壳空白及添加 (0.01 mg/kg) 和稻秆空白及添加 (0.01 mg/kg) 色谱图。

    Figure  3.  Chromatograms of HFMPA

    Chromatograms of HFMPA (C-1~C-7, standard of 0.00167 mg/L, brown rice blank and spiked (0.01 mg/kg), paddy hull blank and spiked (0.01 mg/kg),rice straw blank and spiked (0.01 mg/kg).

    表  1  噁唑酰草胺及其代谢产物质谱参数

    Table  1.   Mass spectrometric ( MS) parameters for detection of metamifop and its metabolites

    化合物
    Compound
    保留时间
    Retention
    time/min
    离子化模式
    Ionization
    mode
    离子对
    Ion pair,
    m/z
    碰撞电压
    Collision
    energy/
    eV
    噁唑酰草胺
    metamifop
    3.50 ESI+ 441.1/180.1 27
    441.1/288.1* 23
    HFMPA 1.64 ESI+ 198/125.9* 10
    198/180 10
    HPFMPA 2.03 ESI+ 290.1/180 10
    290.1/180 10
    6-CBO 2.26 ESI 168/75.8 22
    168/131.8* 18
    注:* 定量离子。Note: * Quantitative ion.
    下载: 导出CSV

    表  2  方法的正确度和精密度 (n=5)

    Table  2.   The trueness and precision of the method (n=5)

    化合物
    Compound
    添加水平
    Spiked level/
    (mg/kg)
    平均回收率
    Average recovery/%
    相对标准偏差
    RSD/%
    糙米
    Brown rice
    稻壳
    Paddy hull
    稻秆
    Rice straw
    糙米
    Brown rice
    稻壳
    Paddy hull
    稻秆
    Rice straw
    噁唑酰草胺

    metamifop
    0.01 91 80 96 9.0 2.6 10.8
    0.1 98 92 91 9.2 5.2 9.7
    2.0 98 79 103 0.9 1.7 3.3
    HFMPA 0.01 94 88 100 4.9 2.1 8.3
    0.1 89 99 90 1.5 2.3 6.1
    2.0 92 84 103 4.5 2.6 6.6
    HPFMPA 0.01 101 92 95 5.6 6.6 8.2
    0.1 100 108 97 2.8 9.8 6.6
    2.0 103 95 97 2.6 9.0 5.4
    6-CBO 0.01 91 92 101 2.5 1.2 3.7
    0.1 85 98 94 3.0 2.1 5.1
    2.0 94 84 87 2.4 7.6 3.8
    下载: 导出CSV
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  • 收稿日期:  2021-07-02
  • 录用日期:  2021-10-24
  • 网络出版日期:  2022-01-11
  • 刊出日期:  2022-04-01

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