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作 者:陈伟[1] 刘红彦[1] 范芳婷[1] 倪云霞[1] 赵辉[1] 刘新涛[1]
机构地区:[1]河南省农业科学院植物保护研究所,农业部华北南部农作物有害生物综合治理重点实验室,河南省农作物病虫害防治重点实验室,郑州450002
出 处:《农药》2011年第12期909-911,914,共4页Agrochemicals
基 金:国家芝麻产业技术体系(nycytx-20-1-05);农业部948项目“芝麻抗灾轻简化生产技术引进与利用”(2010-C3)
摘 要:[目的]为了准确评价甲基硫菌灵在芝麻上使用后其对芝麻的安全性,通过高效液相色谱法对其及代谢物多菌灵残留量进行测定,并建立快速分析方法。[方法]采用1%甲酸的乙腈溶液浸泡萃取,然后利用N-丙基乙二胺(PSA)和C18粉末净化,反相高效液相色谱法测定,外标法定量。[结果]在0.1~1.0 mg/kg添加水平范围内,多菌灵的添加回收率为76.37%~102.34%,RSD为3.36%~8.86%;甲基硫菌灵的添加回收率为87.29%~108.42%,RSD为3.81%~5.71%。多菌灵、甲基硫菌灵最小检出质量分数分别为0.015、0.002 mg/kg。2009、2010年芝麻中多菌灵平均残留量分别为0.0577、0.2437 mg/kg,甲基硫菌灵残留量分别为0.2663、0.3002 mg/kg。[结论]2010年芝麻中多菌灵的残留量高于无公害芝麻多菌灵残留限量指标(0.2 mg/kg);2009、2010年芝麻中甲基硫菌灵的残留量均高于欧盟残留限量标准(0.1 mg/kg)。In order to accurately evaluate the sesame's safety of thiophanate-methyl,the rapid simultaneous method for determination of residual thiophanate-methyl and its metabolite carbendazim was developed in the study,then the residues of them in sesame seeds were detected by the method.[Methods] The thiophanate-methyl and carbendazim residues were extracted by 1% formic acid in acetonitrile,then purified by PSA and C18,and detected by HPLC.[Results] The average recoveries of carbendazim and thiophanate-methyl stood with ranges of 76.37-102.34% and 87.29-108.42% at three spiking levels from 0.1 to 1.0 mg/kg with their relative standard deviations of 3.36-8.86% and 3.81-5.71% in sesame seeds respectively.The lowest concentrations detected for carbendazim and thiophanate-methyl were 0.015 and 0.002 mg/kg in sesame seeds respectively.The trial experiments in Zhengzhou and Nanyang showed that the average residues of carbendazim and thiophanate-methyl in sesame seeds were 0.0577(2009),0.2437(2010) mg/kg and 0.2663(2009),0.3002(2010) mg/kg.[Conclusions] The residue of carbendazim was higher than the MRLs of pollution-free sesame(0.2 mg/kg) in 2010.The residue of thiophanate-methyl was higher than the MRLs of European Union(0.1 mg/kg) in 2009 and 2010.
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