基于UPLC-MS/MS的土壤中敌草隆残留检测技术  

UPLC-MS/MS based technique for the detection ofdiuron residues in soil

作　　者：施超宇 孙晓欣 吴嵘 杨勇 王雪 肖学喜 SHI Chaoyu;SUN Xiaoxin;WU Rong;YANG Yong;WANG Xue;XIAO Xuexi(Zhejiang Zhongyi Testing Research Institute Co.,Ltd,Ningbo 315040,Zhejiang)

机构地区：[1]浙江中一检测研究院股份有限公司,浙江宁波315040

出　　处：《浙江农业科学》2024年第1期157-161,共5页Journal of Zhejiang Agricultural Sciences

摘　　要：为了提高土壤中敌草隆的萃取效率,更为精确地检测其残留量,采用加压溶剂萃取作为土壤中敌草隆的萃取方式,使用超高效液相色谱-三重四极杆串联质谱法对土壤中残留的敌草隆进行了检测,建立了一种土壤中敌草隆萃取和检测的新方法。试样经冷冻干燥处理后,将其研磨样装入加压溶剂萃取仪,使用2∶1的甲醇-二氯甲烷混合溶液作为萃取剂,萃取液经Carb/PSA石墨化炭黑/乙二胺-N-丙基固相萃取柱净化后,通过C18色谱柱进行分离,并以体积比为1∶9的甲醇-二氯甲烷混合溶剂进行梯度洗脱,质谱中选择电子轰击离子源和多反应监测模式。结果显示,敌草隆在20~500μg·L^(-1)范围内具有良好的线性关系,相关系数为0.999 5,且目标峰分离效果较好;不同浓度下敌草隆的加标回收率为71.2%~90.3%,相对标准偏差为1.7%~9.4%,检出限为0.000 287μg·g^(-1)。该方法有利于对土壤中敌草隆残留量大批量检测的操作,提高了目标物的萃取效率和检测效率,提高样品检测准确性。In order to improve the extraction efficiency of diuron in soil and to detect its residues more accurately,pressurized solvent extraction was used as the extraction method for diuron in soil,and a new method for the extraction and detection of diuron in soil was established by using ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry.The sample was freeze-dried and loaded into a pressurized solvent extractor,and a methanol-dichloromethane mixture was used as the extractant.The extract was cleaned up by a Carb/PSA graphitized carbon black/ethylenediamine-N-propyl solid phase extraction column,and then separated by a C18 column with a gradient elution of methanol-dichloromethane mixture at a volume ratio of 1∶9.The electron bombardment ion source and multiple reaction were selected in the mass spectrometry monitoring mode.The results showed that there was a good linear relationship within the range of 20-500μg·L^(-1) diuron,with a correlation coefficient of 0.9995,and the target peak separation effect is good.The spiked recoveries of diuron were 71.2%-90.3%,the relative standard deviations were 1.7%-9.4%,and the detection limits were 0.0002870μg·g^(-1).This method is conducive to the operation of large-scale detection of diuron residues in soil,improving the extraction and detection efficiency of target substances,and improving the accuracy of sample detection.

关 键 词：敌草隆 加压溶剂萃取 液质联用 农药残留 

分 类 号：S482.4[农业科学—农药学]