花生中噻呋酰胺残留量的检测及膳食风险评估

Determination of thifluzamide residue in peanut and dietary risk assessment

中文关键词:  噻呋酰胺  花生  残留  超高效液相色谱-串联质谱仪  风险评估

英文关键词:thifluzamide  peanut  residue  ultra performance liquid chromatography-tandem mass spectrometer  risk assessment

中文摘要:

      目的 建立超高效液相色谱-串联质谱联用法检测噻呋酰胺残留的分析方法, 探明噻呋酰胺在花生中的残留特性和使用安全性。方法 样品经乙腈提取, QuEChERS方法净化, 在电喷雾正离子(electrospray ionization, ESI+)模式下, 用超高效液相色谱-串联质谱联用仪(ultra performance liquid chromatography-tandem mass spectrometer, UPLC-MS/MS)采用多反应监测(multiple reaction monitoring, MRM)模式检测。结果 噻呋酰胺在1~5000 μg/L浓度范围内线性良好, 相关系数在0.9998和1之间。在花生壳和土壤样品中, 添加水平为1、500、2000 μg/kg及在植株和花生仁样品中, 添加水平为5、500、2000 μg/kg时, 加标回收率在75.5%~107.9%之间, 相对标准偏差不大于10%; 240 g/L噻呋酰胺悬浮剂, 150~225g a.i/ha用药1次, 采收间隔期14、21、28 d, 噻呋酰胺在花生中的最大风险商为0.0013。结论 该方法简便、快速、灵敏高, 能有效克服杂质干扰, 膳食风险结果表明, 240 g/L噻呋酰胺悬浮剂按上述方法使用安全。

英文摘要:

      Objective To establish a method for the determination of thiafuramide residue by ultra performance liquid chromatography-tandem mass spectrometry, and investigate the residual properties and safety of thiafuramide in peanut. Methods The samples were extracted with acetonitril, and cleaned-up by QuEChERS. Then, the residues of thifluzamide were analyzed by ultra performance liquid chromatography-tandem mass spectrometer (UPLC/MS/MS), under electrospray positive ion using multiple reaction monitoring (MRM) mode. Results The thifluzamide had high correlation coefficients at the range of 1?5000 μg/L, with the correlation coefficients between 0.9998 and 1. When the spiked levels of 1, 500, 2000 μg/kg in peanut hull and soil, and the spiked levels of 5, 500, 2000 μg/kg in peanut plant and peanut kernel, the spiked recoveries of thifluzamide in all samples were between 75.5% and 107.9%, with the relative standard deviation (RSD) less than 10%. Spraying 1 times during growing period of peanut with 150-225 g a.i./ha of 240 g/L thifluzamide suspension concentrate, the maximum value at risk quotient of thifluzamide after the last application for 14, 21, 28 d was 0.0013. Conclusion This method is simple, rapid, sensitive, which can effectively overcome the interference of impurities. The dietary risk assessment results show that 240 g/L thifluzamide suspension concentrate is safety with the above application.