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基于LC-MS/MS技术土壤中14种除草剂残留的检测方法

Detection method for 14 herbicide residues in soil based on LC-MS/MS technology

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【作者】 常雪淼; 王宇欣; 张明; 王召; 孙楠; 陈建华; 胡彬; 马金海; 马栋豪; 李劲松;

【Author】 CHANG Xuemiao;WANG Yuxin;ZHANG Ming;WANG Zhao;SUN Nan;CHEN Jianhua;HU Bin;MA Jinhai;MA Donghao;LI Jinsong;College of Water Resources & Civil Engineering, China Agricultural University;Pingfeng Seed Industry Company;Pingdingshan Academy of Agricultural Sciences;Beijing Plant Protection Station;Pingdingshan Jiudu Agricultural Technology Company;Hangzhou Spectrum Technology Development Company;

【通讯作者】 王宇欣;

【机构】 中国农业大学水利与土木工程学院; 平顶山市平丰种业有限责任公司; 平顶山市农业科学院; 北京市植物保护站; 平顶山市韭都农业科技有限公司; 杭州谱育科技发展有限公司;

【摘要】 以河南省平顶山市现代农业研发基地为研究对象,建立土壤中苯达松、2甲4氯及氟磺胺草醚和11种磺酰脲类除草剂的快速检测方法,采用液相色谱-串联质谱(LC-MS/MS),通过分步提取结合C18固相萃取净化,使用ACQUITY UPLC?HSS T3柱,以体积分数为1%甲酸水溶液-乙腈为流动相梯度,结合电喷雾正/负离子切换多反应监测模式进行定量分析,采用LC-MS/MS进行定量。试验结果表明:1)14种除草剂的质量分数为0.05~10μg/kg时,进样量与对应的峰面积间呈良好的线性关系,相关系数r≥0.99,加标回收率为88.79%~119.48%;2)非健康生长地块中健康和非健康韭菜根际土中乙草胺的残留量均高于健康生长地块的健康韭菜根际土,表明乙草胺的残留可能与韭菜非健康生长存在潜在关联。本研究为国产LC-MS/MS仪器的应用提供了技术支撑,也为农田除草剂溯源及农产品安全评估提供了技术参考。

【Abstract】 The Modern Agricultural Research and Development Base in Pingdingshan City,Henan Province,was selected as the research object.A rapid method for the determination of bendazone,2-methyl-4-chlorophenoxyacetic acid,flusulfenoxuron and a total of 11 sulfonylurea herbicides in soil was established.Liquid Chromatography-tandem Mass Spectrometry (LC-MS/MS) technology was adopted.Samples were cleaned-up by stepwise extraction coupled with C18 solid-phase extraction,and quantified by an ACQUITY UPLC?HSS T3 column using a 1% formic acid aqueous solution-acetonitrile as mobile phase gradient.Combined with electrospray positive/negative ion switching multiple reaction monitoring mode,samples were quantitatively analyzed by using LC-MS/MS.The results showed that:1) A good linear relationship was observed between the injection mass fraction and the corresponding peak areas for the 14 herbicides at mass fractions ranging from 0.05 to 10μg/kg,with the correlation coefficient of r≥0.99.The spiked recoveries ranged from 88.79% to 119.48%;2) The residues of acetamiprid in the inter-root soils of healthy and unhealthy leeks in non-healthy growing soil were higher than that in healthy leek inter-root soil,suggesting that ethofumesate residues might be potentially associated with unhealthy leek growth.In conclusion,this study provides technical support for the application of domestic LC-MS/MS instruments,and technical reference for the traceability of herbicides in farmland and the safety assessment of agricultural products.

【关键词】 LC-MS/MS; 除草剂残留; 土壤; 检测技术;
【Key words】 LC-MS/MS; herbicide residues; soil; detection technology;
【基金】 平顶山市重大科技专项(2020ZD19);现代农业产业技术研究体系专项(CARS-23-C02)
  • 【文献出处】 中国农业大学学报 ,Journal of China Agricultural University , 编辑部邮箱 ,2025年07期
  • 【分类号】O657.63;S481.8
  • 【下载频次】98
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