| QuEChERS-超高效液相色谱-串联质谱法测定双氟磺草胺和氯氟吡氧乙酸在小麦和土壤中的残留及消解动态 |
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| 引用本文： | 金涛,段劲生,高同春.QuEChERS-超高效液相色谱-串联质谱法测定双氟磺草胺和氯氟吡氧乙酸在小麦和土壤中的残留及消解动态[J].农药学学报,2018,20(4):468-476. |
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| 作者姓名： | 金涛 段劲生 高同春 |
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| 作者单位： | 安徽省农业科学院 植物保护与农产品质量安全研究所，农业部农产品质量安全风险评估实验室 (合肥) ，安徽科立特农药环境评价科技有限公司，合肥 230031 |
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| 基金项目： | 国家重点研发计划（2016YFD0200207，2016YFD0200803，2016YFD0201205）；安徽省农业科学院科技创新团队项目（14C1105）；安徽省农业生态环保与质量安全产业技术体系（AHCYJSTX-15） |
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| 摘 要： | 建立了同时测定小麦及其土壤中双氟磺草胺和氯氟吡氧乙酸残留的QuEChERS-超高效液相色谱-串联质谱方法，并采用该方法研究了低温冷藏条件下双氟磺草胺和氯氟吡氧乙酸在小麦上的储藏稳定性以及15%双氟磺草胺?氯氟吡氧乙酸悬乳剂在小麦和土壤中的最终残留及消解动态。结果表明:在添加水平为0.005~1 mg/kg范围内，双氟磺草胺和氯氟吡氧乙酸在小麦及土壤中的平均回收率在82%~108%之间，相对标准偏差在0.41%~11%之间 (n=5) ，均能满足农药残留分析的要求。在 –20℃下储藏365 d后，麦粒中双氟磺草胺和氯氟吡氧乙酸的残留量变化小于30%，符合植源性农产品中农药残留储藏稳定性试验准则要求，储藏稳定。双氟磺草胺在小麦植株和土壤中的消解半衰期分别为4.4~8.1 d和2.4~9.3 d；氯氟吡氧乙酸在小麦植株和土壤中的消解半衰期分别为7.9~10.6 d和11.8~24.8 d，即在相同的试验条件下双氟磺草胺在植株和土壤中消解速率快于氯氟吡氧乙酸的。采用推荐剂量有效成分180 g/hm2和推荐高剂量有效成分270 g/hm2的15%双氟磺草胺?氯氟吡氧乙酸悬乳剂于小麦田施药1次，在小麦收获期的麦粒中均未检出双氟磺草胺和氯氟吡氧乙酸残留。
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| 关 键 词： | QuEChERS 超高效液相色谱-串联质谱 双氟磺草胺 氯氟吡氧乙酸 小麦 土壤 残留 消解 |
| 收稿时间： | 2018/4/25 0:00:00 |
Residue and dissipation of florasulam and fluroxypyr in wheat and soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry |
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| JIN Tao,DUAN Jinsheng and GAO Tongchun.Residue and dissipation of florasulam and fluroxypyr in wheat and soil by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Pesticide Science,2018,20(4):468-476. |
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| Authors: | JIN Tao DUAN Jinsheng and GAO Tongchun |
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| Institution: | Institute of Plant Protection and Agricultural Product Quality and Safety, Anhui Academy of Agricultural Sciences/Key Laboratory of Agro-Product Safety Risk Evaluation (Hefei), Ministry of Agriculture/Kelite Pesticide Environment Evaluation Technology Co., Ltd, Hefei 230031, China |
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| Abstract: | A simultaneous method was developed for the determination of florasulam and fluroxypyr in wheat and soil using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) . The storage stability of florasulam and fluroxypyr in wheat under cold storage condition was studied. The final residue and dissipation of the two herbicides in wheat and soil were also determined by this new method. At the spiked level from 0.005 mg/kg to 1 mg/kg, the average recoveries of florasulam and fluroxypyr in wheat and soil were 82%-108%, and the relative standard deviations were 0.41%-11%(n=5) . The results showed that the method is reliable and practical for pesticide residue analysis. After storage at –20℃ for 365 d, the decrease of residues of florasulam and fluroxypyr in wheat is less than 30%, which is in the line with the requirements of the storage stability test criteria for pesticide residues in plant-derived agricultural products. The dissipation half-lives of florasulam in wheat and soil was 4.4-8.1 d and 2.4-9.3 d, respectively.The dissipation half-lives of fluroxypyr in wheat and soil was 7.9-10.6 d and 11.8-24.8 d, respectively. Under the same experimental conditions, the degradation rates of florasulam in plants and soil were faster than those of fluroxypyr. When the formulated pesticide of florasulam and fluroxypyr 15% suspensions (SE) was sprayed once at the recommended dose (active ingredients: 180 g/hm2) and high dose (active ingredients: 270 g/hm2) in wheat fields, the florasulam and fluroxypyr residues were not detected in wheat during the harvest period. |
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| Keywords: | QuEChERS UPLC-MS/MS florasulam fluroxypyr wheat soil residue dissipation |
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