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

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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。
UPLC-MS/MS based technique for the detection of diuron residues in soil
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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