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

作　　者：程启明[1,2] 黄青[2] 廖祯妮[2] 杨建文 吴道聪 苏丽[1] 

机构地区：[1]广西大学农学院,广西南宁530004 [2]中国科学院城市环境研究所,城市环境与健康重点实验室,福建厦门361021 [3]红河千山生物工程有限公司,云南泸西652400

出　　处：《分析科学学报》2015年第1期115-118,共4页Journal of Analytical Science

基　　金：中国科学院重点部署项目(No.KZZD-EW-16-02)

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。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.

关 键 词：阿特拉津 二甲戊乐灵 灯盏花 土壤 气相色谱-质谱法 

分 类 号：O657.63[理学—分析化学]