首页|基于UPLC-MS/MS的土壤中敌草隆残留检测技术

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 of diuron residues in soil

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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 20~500 μg·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0.000 287 μg·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 20-500 μg·L-1 diuron,with a correlation coefficient of 0.999 5,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 0.000 287 0 μg·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.

diuronpressurized solvent extractionliquid mass spectrometrypesticide residues

施超宇、孙晓欣、吴嵘、杨勇、王雪、肖学喜

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浙江中一检测研究院股份有限公司, 浙江 宁波 315040

敌草隆 加压溶剂萃取 液质联用 农药残留

2024

浙江农业科学
浙江省农业科学院,浙江大学

浙江农业科学

影响因子:0.523
ISSN:0528-9017
年,卷(期):2024.65(1)
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