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加速溶剂萃取-气相色谱/质谱法测定灯盏花及其土壤中阿特拉津和二甲戊乐灵残留

Determination of Atriazine and Pendimethalin in Erigeron breviscapus(Vant.)Hand-Mazz and Soil by Accelerated Solvent Extraction and Gas Chromatography-Mass Spectrometry

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【作者】 程启明黄青廖祯妮杨建文吴道聪苏丽

【Author】 CHENG Qi-ming;HUANG Qing;LIAO Zhen-ni;YANG Jian-wen;WU Dao-cong;SU Li;Agricultural College of Guangxi University;Key Laboratory of Urban Environment & Health,Institute of Urban Environment,Chinese Academy of Sciences;Honghe Qianshan Biotechnology Co.LTD;

【机构】 广西大学农学院中国科学院城市环境研究所,城市环境与健康重点实验室红河千山生物工程有限公司

【摘要】 建立了加速溶剂萃取(ASE)-气相色谱/质谱法(GC/MS)同时测定灯盏花及其土壤中阿特拉津和二甲戊乐灵2种除草剂的农药残留。样品采用丙酮-二氯甲烷(1∶1,V/V)加速溶剂萃取,弗罗里硅土柱层析净化,用GC/MS选择离子监测(SIM)法测定。结果表明,2种除草剂在0.05~2.00mg/L范围内线性良好,相关系数分别为0.9987~1.0000(灯盏花),0.9880~0.9980(土壤);在0.1、0.5和1.0mg/L添加水平下,2种除草剂在灯盏花及其土壤中的平均回收率分别为67.38%~104.02%和71.69%~105.58%,相对标准偏差(RSD)分别为3.21%~13.48%和2.65%~18.26%,方法的检出限(LOD)在灯盏花中为3.00~4.10ng/g,在土壤中为1.50~2.50ng/g。应用该法成功测定了云南省灯盏花及其土壤样品中2种除草剂残留。

【Abstract】 A multi-residue analytical method was developed for the rapid determination of atrizine and pendimethalin herbicides in soil and Erigeron breviscapus(Vant.)Hand-Mazz using accelerated solvent extraction(ASE)and gas chromatography-mass spectrometry(GC-MS)techniques.The target analytes were extracted with a mixture of acetone and dichloromethane(1∶1,V/V)using ASE and then purified through a Florisil column chromatography.The final extract volume was concentrated to 1 mL and analyzed using GC-MS with selective ion monitoring(SIM)mode.It was found that the linear ranges of the selected herbicides were 0.05-2.00mg/L,and the correlation coefficients were 0.9880-1.0000.At three spiked levels(0.1,0.5,1.0mg/L),the average recoveries of the 2herbicides ranged from 67.38%-104.02% in Erigeron breviscapus with the relative standard deviations(RSDs)3.21%-13.48% and71.69%-105.58%in soil with the RSDs 2.65%-18.26%,respectively.The limits of detection(LOD)were 3.00-4.10ng/g in Erigeron breviscapus and 1.50-2.50ng/g in soil.The method was successfully applied for analyzing the soil and Erigeron.breviscapus collected from Yunnan Province,China.

【基金】 中国科学院重点部署项目(No.KZZD-EW-16-02)
  • 【文献出处】 分析科学学报 ,Journal of Analytical Science , 编辑部邮箱 ,2015年01期
  • 【分类号】O657.63;S481.8
  • 【被引频次】8
  • 【下载频次】228
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