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噁唑酰草胺及其代谢物在水稻上的残留检测方法和储藏稳定性研究

Study on the Residue Determination and Storage Stability of Metamifop and Its Metabolites in Rice

  • 摘要: 建立了水稻糙米、稻壳和稻杆中噁唑酰草胺及代谢物HPMFPA、HFMPA、6-CBO的残留分析方法。采用乙腈为提取剂,PSA和C18为分散剂的QuEChERS前处理方法,用超高效液相色谱-三重四级杆质谱在选择离子监测(SIM)模式下进行检测,外标法定量。结果表明,噁唑酰草胺及代谢物在0.01~0.5 mg·kg-1添加水平范围内,平均回收率为70.1%~108.8%,相对标准偏差为1.8%~11.9%。在储藏温度-18℃、储藏时间为32周的试验期间,噁唑酰草胺及其代谢物降解率均小于30%。该方法简单快捷,准确且灵敏度高,是一种较为实用的检测分析方法。储藏稳定性试验结果表明,噁唑酰草胺及其代谢物在水稻样品中均比较稳定。

     

    Abstract: A residual analysis method was established for the simultaneous determination of metamifop and its metabolites HPMFPA, HFMPA, 6-CBO in brown rice, rice hull, rice stalk. The samples were extracted with acetonitrile, and then purified by QuEChERS with primary secondary amine(PSA) and C18 sorbent, and then determined by ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry in select ion monitoring mode with external standard method for quantification. The results showed that the recoveries of metamifop and its metabolites at the addition levels(0.01~0.5 mg·kg-1) were within 70.1%~108.8%, with the relative standard deviation(RSD, n=5) between 1.8% and 11.9%. The degradation rate of both metamifop and its metabolites was less than 30% during 32 weeks of storage at-18 ℃. The method is simple, fast, accurate and sensitive, which can be used as a practical detection and analysis technique. The storage stability results showed that metamifop and its metabolites were stable in rice samples.

     

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