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(electrosprayionization,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1~5000μg/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、2000μg/kg及在植株和花生仁样品中,添加水平为5、500、2000μg/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。
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.
作者
李辉
李娜
邵辉
刘磊
宋淑荣
郭永泽
张玉婷
LI Hui;LI Na;SHAO Hui;LIU Lei;SONG Shu-Rong;GUO Yong-Ze;ZHANG Yu-Ting(Research Institution of Agricultural Quality Standards and Testing Technology in Tianjin, Tianjin 300381, China;Ministry of Agriculture and Rural Affairs Lab of Agricultural Product Quality Safety Risk Assessment (Tianjin), Tianjin 300381, China)
出处
《食品安全质量检测学报》
CAS
2019年第10期3012-3016,共5页
Journal of Food Safety and Quality
基金
天津市农业科学院院长基金项目(16002)
天津市蔬菜产业体系创新团队项目(ITTVRS2019021)~~
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
thifluzamide
peanut
residue
ultra performance liquid chromatography-tandem mass spectrometer
risk assessment
