应用所建立的分散固相萃取?液相色谱?串联质谱法测定土壤和番茄中霜霉威为0.02、0.20、2.00 mg·kg-1等3个添加浓度时,日内平均回收率为83.9%—104.6%,日内相对标准偏差为1.0%—5.5%,日间平均回收率为84.3%—108.9%,日间相对标准偏差为1.4%—4.9%.霜霉威在1.0—200?0μg·L-1浓度范围内相关系数R2>0.9992,在土壤中和番茄基质中定量限均为0.02 mg·kg-1.该方法能够满足现有限量标准的要求.霜霉威消解动态试验采用推荐高剂量(90 g·ha-1)为施药剂量,在植株第2穗果膨大期开始喷药1次,分别测定喷药后2h、1d、2d、4d、7d、14d的霜霉威残留量的变化.浙江杭州、山东潍坊和河南商丘的3个试验点消解动态试验中,降解动态符合一级动力学指数模型.2011—2012年霜霉威在番茄中降解半衰期为2.4—4.7 d,在土壤中降解半衰期1.1—1.5 d.施药5 d后的残留量均小于检测限,远远低于2.0 mg·kg-1最大残留限量,实际样品中霜霉威的残留量均低于检测限.72?2%霜霉威水剂按照推荐剂量1.5倍喷施番茄1次,其喷施2 h后的残留量仅为1.5 mg·kg-1,符合残留要求可以安全使用.
The dissipation of propamocarb in tomato and soil was studied to formulate a scientific basis for the acceptable dose and the pre?harvest interval. Dissipation experiments were conducted by applying propamocarb once on tomato and soil with hole application at 90 g·ha-1 after fruit enlargement. The samples were collected randomly from each plot at different time intervals i.e, 2 h, 1, 2, 4, 7, 14 days after the application. Dispersive solid phase extraction combined to ultra?high performance liquid chromatography-tandemmass spectrometry ( UPLC?MS/MS) method was used to determine the propamocarb residue in tomato and soil. Recovery test was processed in three spiked levels of 0.02, 0.20 and 2.00 mg·kg-1 . The results showed that the within?day average recovery rate of propamocarb in tomato and soil were 83.9%—104.6%, the within?day RSDs were 1.0%—5.5%;the between?day average recovery rate were 84?3%—108.9%, the between?day RSDs were 1.4%—4.9%. The correlation coefficient of propamocarb in the range of 1. 0—200. 0 μg·L-1 was R2>0?9992, LOQ were 0.02 mg·kg-1 . The actual samples and field experimental samples were detected by using this method, the results showed that the degradation half?life of propamocarb in tomato and soil were 2.4—4.7 d and 1.1—1.5 d, respectively. The residues were less than max residue limits ( MRLs ) . The propamocarb agent ( 72?2%) applied with hole application can be considered safe after more than 2 h in the application to the pre?harvest intervals.
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