双氟磺草胺与唑草酮悬乳剂在田间小麦和土壤中的残留动态及安全性评价
The degradation dynamics and safety evaluation of florasulam and carfentrazone-ethyl in wheat and soil
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摘要: 本文建立了双氟磺草胺和唑草酮在小麦和土壤中残留检测的超高效液相色谱-串联质谱方法.该方法双氟磺草胺的最小检出量为5.0×10-4 ng,唑草酮的最小检出量为2.9×10-4 ng;在添加水平为双氟磺草胺0.010-0.50 mg·kg-1和唑草酮0.020-1.0 mg·kg-1在小麦及土壤中的平均回收率在75%-108%和76%-107%之间,相对标准偏差在4.2%-12.5%和3.5%-11%之间(n=5).采用该方法研究了3%双氟磺草胺-唑草酮(2%:1%)悬乳剂两年三地(2016-2017年,北京、黑龙江和陕西)的田间消解动态和最终残留.结果表明,双氟磺草胺在小麦植株和土壤中的消解半衰期分别为5.4-7.3 d和5.5-12.2 d;唑草酮在小麦植株和土壤中的消解半衰期分别为5.1-7.7 d和6.1-12.5 d.根据最终残留田间试验,在收获期,双氟磺草胺在植株中的最终残留<0.010 mg·kg-1;土壤中的最终残留为<0.007 mg·kg-1;麦粒中的最终残留均<0.005 mg·kg-1;收获期,唑草酮在植株中的最终残留<0.015 mg·kg-1;土壤中的最终残留为<0.027 mg·kg-1;麦粒中的最终残留均<0.020 mg·kg-1.参考我国对于双氟磺草胺和唑草酮在小麦种的MRL值,推荐安全间隔期为收获期.Abstract: A method was developed for the determination of florasulam and carfentrazone-ethyl simultaneously in wheat and soil by using ultra performance liquid chromatography-tandem mass spectrometry (UPLCMS/MS). The detection limits were 5.0×10-4 ng for florasulam and 2.9×10-4 ng for carfentrazone-ethyl. The recoveries in wheat and soil were 75%-108% for florasulam (RSD=4.2%-12.5%, n=5) at the spiked level from 0.010 mg·kg-1 to 0.50 mg·kg-1, and 76%-107% for carfentrazone-ethyl (RSD=3.5%-11%, n=5) at the spiked level from 0.020 to 1.0 mg·kg-1. The method was adopted to investigate the residues dynamics and final residues of florasulam and carfentrazone-ethyl in wheat and soil with the formulated pesticide of 3% florasulam and carfentrazone-ethyl (2%:1%) suspensions (SE) in Beijing, Heilongjiang and Shaanxi in 2016 and 2017. The results showed that the dissipation half-life of florasulam was 5.4-7.3 d and 5.5--12.2 d in wheat and soil, of fluroxypyr was 5.1-7.7 d and 6.1-12.5 d in wheat and soil, respectively. On the basis of the results, the florasulam residues was less than 0.010 mg·kg-1 in wheat stalk, 0.007 mg·kg-1 in soil and 0.005 mg·kg-1 in wheat seed; and carfentrazone-ethyl residues were less than 0.015 mg·kg-1 in wheat stalk, 0.027 mg·kg-1 in soil and 0.020 mg·kg-1 in wheat seed in the harvest. In consequence, the harvest time of wheat was recommended as the pre-harvest interval (PHI) of the formulated pesticide of 3% florasulam and carfentrazone-ethyl suspension.
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Key words:
- florasulam /
- carfentrazone-ethyl /
- wheat /
- pesticide residue /
- dissipation
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