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高效液相色谱法测定甲基二磺隆在谷子和土壤中的残留及消解动态 被引量:1

Residue and Degradation of Mesosulfuron-methyl in Foxtail Millet and Soil by High Performance Liquid Chromatography
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摘要 为研究甲基二磺隆在谷子及土壤中的残留消解特征,采用高效液相色谱法建立了谷子及土壤中甲基二磺隆残留检测技术。样品经乙腈-三乙胺(0.02 mol/L)提取,石墨化炭黑(GCB)净化,以乙腈∶磷酸(0.01 mol/L)=50∶50为流动相,高效液相色谱外标法定量检测。结果表明,该方法的最低检出量为0.2 ng,在植株和籽粒中的最低检测质量浓度为0.02 mg/kg,土壤中为0.008 mg/kg;在0.008~0.500 mg/kg添加范围内,平均回收率为91.99%~98.17%,相对标准偏差为2.28%~12.43%。利用该方法于2014年检测了晋谷21号及土壤中甲基二磺隆的残留消解动态和最终残留量,甲基二磺隆在植株中的半衰期为6.4 d,土壤中的半衰期为16.6~18.7 d;在收获期植株、籽粒及土壤中均未检出甲基二磺隆。由此可知,甲基二磺隆是一种易降解除草剂;在该试验检测条件下,其在小米、秸秆中残留量均低于我国和美国制定的相关MRL标准。 To study the residue and degradation of mesosulfuron-methyl in foxtail millet of crop field trials,a high performance liquid chromatography(HPLC)method was developed.Samples were extracted with acetonitrile-triethylamine(0.02 mol/L),cleaned up by graphitized carbon black(GCB),acetonitrile∶phosphoric acid(0.01 mol/L)=50∶50 as the mobile phase,detected by HPLC with quantification by external standard method.The result showed that the minimum detectable amount of this method was 0.2 ng,and the lowest detection concentration was 0.02 mg/kg in plants and grains,and the soil was 0.008 mg/kg.In the range of 0.008-0.500 mg/kg,the average recoveries of mesosulfuron-methyl were 91.99%-98.17%,and coefficient of variations were 2.28%-12.43%.The degradation and final residues of mesosulfuron-methyl in Jingu 21 and soil were determined in Shanxi,China during 2014.The degradation results showed the half-lives of mesosulfuron-methyl in foxtail millet plant was 6.4 d,and the half-lives in soil was 16.6-18.7 d;mesosulfuron-methyl was not detected in the straw,grain and soil at harvest stage.It indicates that mesosulfuron-methyl is a readily degradable herbicide,under the test conditions,the residues in millet and straw are lower than the relevant MRL standards formulated by China and the United States.
出处 《山西农业科学》 2018年第3期429-432,共4页 Journal of Shanxi Agricultural Sciences
基金 国家自然科学基金项目(31301269) 山西省农业科技攻关项目(20150311016-2) 山西省重点研发项目(2015-TN-09) 山西省重点研发计划(一般项目)(201603D221003-2) 山西农业大学青年拔尖创新人才支持计划(TYIT201406) 山西农业大学青年科技研究基金项目(201601D202075)
关键词 甲基二磺隆 谷子 高效液相色谱 残留 消解动态 mesosulfuron-methyl foxtail millet HPLC residue degradation
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