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

    Residues of metamifop and its metabolites in paddy rice

    • 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。

       

      Abstract: In this work, a method for the determination of the residues of metamifop and its three metabolites in samples of brown rice, paddy hull and rice straw was validated based on ultra performance liquid chromatography-tandem mass spectrometry. The three metabolites were N-(2-fluorophenyl)-2-hydroxy-N-methylpropionamide (HFMPA), N-(2-fluorophenyl)-2-(4-hydroxyphenoxy)-N-methylpropionamide (HPFMPA) and 6-chloro-3H-benzooxazol-2-one (6-CBO). The detection of 6-CBO was performed by tandem mass spectrometry with electrospray ionization in negative mode (ESI-), and the other three analytes were determined in positive mode (ESI+). The samples of paddy rice were extracted with acetonitrile by an oscillator, and cleaned up by C18 SPE cartridges. The method was validated and the matrix effects were evaluated. The method was applied to detect real final residue samples in the field trials. and the matrix effects were estimated. The average recoveries of metamifop and its metabolites in brown rice, paddy hull and rice straw at three spiked levels (0.01, 0.1 and 2.0 mg/kg) were in the range of 79%-108% with good precision (RSD<10.8%). Satisfactory linear relationships of metamifop, HFMPA, HPFMPA and 6-CBO were obtained in the range of 0.0005-0.02 mg/L with the correlation coefficient (r) over 0.9941. Limits of quantifications (LOQs) of metamifop, HFMPA, HPFMPA and 6-CBO in brown rice, paddy hull and rice straw were 0.01 mg/kg. To investigate the final residues of metamifop and its metabolites in paddy rice, the field trials were conducted in paddy rice in ten Provinces in China. The final residues of metamifop, HFMPA, HPFMPA and 6-CBO in brown rice and paddy hull were all below 0.01 mg/kg , which were lower than the maximum residue limit (MRL) of metamifop in brown rice (0.05 mg/kg) established in China. The residues of HFMPA were found in rice straw in the range of < 0.01 mg/kg-0.098 mg/kg, while the final residues of metamifop, HPFMPA and 6-CBO in rice straw were all below LOQ. It is recommended that 20% metamifop + bentazone micro-emulsion (ME, 3.3% metamifop) could be applied at the highest application dosage of 720 g a.i./hm2 (metamifop 118.8 g a.i./hm2 ) in rice and be applied only once.

       

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