磁固相萃取/离子色谱法测定土壤中草甘膦  

Determination of Glyphosate Residues in Soil Samples by Ion Chromatography Combined with Magnetic Solid Phase Extraction

作　　者：杨健[1] 李振宇[1] 祝艳[1] 杨德志 杨亚玲[2] YANG Jian;LI Zhen-yu;ZHU Yan;YANG De-zhi;YANG Ya-ling(Kunming Environmental Monitoring Center,Kunming 650028,China;Faculty of Life Science and Technology,Kunming University of Science and Technology,Kunming 650500,China)

机构地区：[1]昆明市环境监测中心,云南昆明650028 [2]昆明理工大学生命科学与技术学院,云南昆明650500

出　　处：《分析测试学报》2018年第9期1051-1055,共5页Journal of Instrumental Analysis

摘　　要：利用离子色谱结合磁固相萃取技术,建立了一种简单快速测定土壤样品中草甘膦残留的新方法,并对提取溶剂、离子色谱条件以及净化吸附剂进行了优化。样品经水提取后,先用乙腈沉淀杂质,再用Fe_3O_4磁性纳米材料净化处理,经IonPac AS11-HC离子色谱柱分离,以30 mmol/L KOH为淋洗液,电导检测器进行检测。结果表明,草甘膦在0. 05~2. 0 mg/L范围内线性关系良好,相关系数为0. 999 7,检出限为13μg/L,定量下限为45μg/L。对采自三七和灯盏花种植基地的土壤样品进行加标回收实验,在50、100、200μg/L加标水平下的回收率为83. 2%~94. 5%,日内相对标准偏差(RSD)为1. 9%~3. 1%,日间RSD为1. 9%~3. 7%。该方法具有操作简单、快速、灵敏、结果准确可靠的特点,完全满足国家标准的检测要求。Combined with magnetic solid phase extraction,a simple and rapid ion chromatographic method was established for the detection of glyphosate residues in soil samples.Experimental conditions such as extraction solvent,conditions of ion chromatography and purification material were also optimized.After extracted with water,the samples were precipitated with acetonitrile to eliminate the impurities,then purifed with Fe 3O 4 magnetic nanoparticles.The supernatant was separated on an IonPac AS11-HC column with 30 mmol/L KOH as the eluent,and a conductivity detector was used for the detection.Results showed that a good linearity was obtained in the range of 0.05-2.0 mg/L(r 2=0.999 7).The limits of detection and quantitation for the analyte were 13μg/L and 45μg/L,respectively.The recoveries for the soil samples at spiked levels of 50,100 and 200μg/L were between 83.2%and 94.5%,with the intra-day and inter-day RSDs of 1.9%-3.1%and 1.9%-3.7%,respectively.The method is simple,rapid,sensitive and reliable,and could fully meet the detection requirements in the national standard.

关 键 词：离子色谱 磁固相萃取 草甘膦 土壤样品 

分 类 号：O657.75[理学—分析化学] F767.2[理学—化学]