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Determination of sulfoxaflor residues in vegetables, fruits and soil using ultra-performance liquid chromatography/tandem mass spectrometry

机译:超高效液相色谱/串联质谱法测定蔬菜,水果和土壤中的硫草酸残留

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Sulfoxaflor is a novel sulfoximine insecticide which is effective against a wide range of sap-feeding insect pests, including aphids, whiteflies, hoppers, and lygus. In this study, a rapid, highly sensitive and selective method was developed for determining sulfoxaflor residues in vegetables, fruits and soil by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compound was extracted with acetonitrile and cleaned with dispersive solid phase extraction using primary and secondary amine (PSA). Two pairs of precursor product ion transitions for sulfoxaflor were measured and evaluated. Satisfactory linearities in the range of 10a€“1000 ??g La?’1 of sulfoxaflor were obtained, where the correlation coefficients (R2) were higher than 0.9977 in all cases. Average recoveries in cucumber, tomato, cabbage, apple, grape and soil at three levels (10 ??g kga?’1, 100 ??g kga?’1 and 1000 ??g kga?’1) ranged from 78.4% to 98.7%, with relative standard deviations (RSDr) from 1.2% to 14.5%. The reproducibility (RSDR) ranged from 2.9 to 15.6%. The LODs ranged from 0.2 to 0.6 ??g kga?’1, and LOQs from 0.7 to 2.0 ??g kga?’1. This method was used to determine sulfoxaflor residues in cucumber and soil samples for studies of their dissipation under field conditions. The trial results showed that the half-lives of sulfoxaflor obtained after treatment ranged from 1.6 to 2.9 days in cucumber and from 1.5 to 7.2 days in soil in Shandong, Henan and Zhejiang. The developed analytical method provides a basis to establish maximum residue limits and monitor sulfoxaflor residues in vegetables and fruits.
机译:磺胺嘧啶是一种新型的磺胺嘧啶杀虫剂,对多种以树液为食的害虫(包括蚜虫,粉虱,漏斗和盲肠)有效。在这项研究中,开发了一种快速,高度灵敏和选择性的方法,用于通过超高效液相色谱-串联质谱法(UPLC-MS / MS)测定蔬菜,水果和土壤中的磺胺类农药残留。用乙腈萃取目标化合物,并使用伯胺和仲胺(PSA)通过分散固相萃取进行清洁。测量和评估了两对磺胺草醚的前体产物离子跃迁。在磺胺草醚的10a?1000?g La?1?范围内获得了令人满意的线性,在所有情况下,相关系数(R2)均高于0.9977。黄瓜,番茄,卷心菜,苹果,葡萄和土壤在三个水平(10 ?? g kga?'1、100 ?? g kga?'1和1000 ?? g kga?'1)的平均回收率在78.4%至98.7%,相对标准偏差(RSDr)从1.2%增至14.5%。重现性(RSDR)为2.9至15.6%。 LOD的范围为0.2到0.6 ?? g kga?'1,LOQ的范围为0.7到2.0?g kga?'1。该方法用于测定黄瓜和土壤样品中的硫代草酸残留物,以研究其在田间条件下的消散。试验结果表明,处理后得到的亚砜草的半衰期在黄瓜中为1.6至2.9天,在山东,河南和浙江为1.5至7.2天。发达的分析方法为建立最大残留限量和监测蔬菜和水果中的硫代沙弗残留提供了基础。

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