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Method validation, storage stability and field trial for residues of florasulam and pyroxsulam in cereal by liquid chromatography with tandem mass spectrometry

机译:液相色谱-串联质谱法对谷物中植物素和嘧菌酯残留的方法验证,储存稳定性和现场试验

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摘要

A QuEChERS method with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was modified and validated for the determination of florasulam and pyroxsulam residues in wheat grain and straw. The validated method was applied to cereals including oat, millet, corn and rice. Average recoveries were 76-113% with RSDs 2-15%. The limits of quantitation (LOQ) were 0.005 mg/kg for wheat grain and 0.01 mg/kg for wheat straw and four cereals. Ion suppression for florasulam (-28% to -76%) was observed in all the matrices except corn, whereas ion enhancement were shown for pyroxsulam (44% to 83%). Degradation rates of florasulam and pyroxsulam were 6% and 23%, respectively, in wheat grain and straw after eight-week storage at -20°C. The ultimate residues in field trials in ten regions were all ≤0.05 mg/kg, and long term dietary risk assessment indicated that hazard quotients were 0.02% and 0.001% for florasulam and pyroxsulam, respectively, which shows that it is safe to spray the two herbicides on wheat.
机译:改进了液相色谱-串联质谱法(LC-MS / MS)的QuEChERS方法,并验证了该方法可用于测定小麦籽粒和稻草中的植物素和嘧菌酯残留。经验证的方法适用于谷物,包括燕麦,小米,玉米和大米。平均回收率为76-113%,RSD为2-15%。小麦籽粒的定量限(LOQ)为0.005 mg / kg,小麦秸秆和四种谷物的定量限为0.01 mg / kg。除玉米外,在所有基质中均观察到了对植物脂素的离子抑制(-28%至-76%),而对于吡氧舒兰则显示出离子增强(44%至83%)。在-20°C储存八周后,小麦籽粒和秸秆中植物素苏丹草和吡氧磺草胺的降解率分别为6%和23%。在十个地区的田间试验中,最终残留物均≤0.05mg / kg,长期饮食风险评估表明,菌群素和吡氧舒兰的风险商分别为0.02%和0.001%,这表明将两者喷雾是安全的小麦上的除草剂。

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