顶空-气相色谱法测定土壤和沉积物二硫代氨基甲酸酯(盐)类农药总量  

Determination of Total Dithiocarbamate (Salt) Pesticides in Soil and Sediment by Headspace Gas Chromatography

作　　者：姚智锴 胡家宝 陈泽炫 杨嘉慧 Yao Zhikai;Hu Jiabao;Chen Zexuan;Yang Jiahui(Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology,Guangdong Provincial Engineering Research Center for Hazard Identification and Risk Assessment of Solid Waste,Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,Guangzhou),Guangzhou 510070,China)

机构地区：[1]广东省科学院测试分析研究所(中国广州分析测试中心),广东省化学测量与应急检测技术重点实验室,广东省固体废物危险性鉴别与风险评估工程技术研究中心,广东广州510070

出　　处：《山东化工》2022年第15期115-118,共4页Shandong Chemical Industry

摘　　要：建立了顶空-气相色谱法测定土壤和沉积物中二硫代氨基甲酸酯(盐)类农药总量的方法,并利用代森锰锌作为目标物来进行分析。称取2 g的样品于顶空瓶中,在含有氯化亚锡的无机酸介质中,用80℃恒温水浴振荡器合成了二硫化碳,目标物采用Agilent HP-5色谱柱分离,用电子捕获检测器(ECD)检测,外标法定量。通过分析结果表明,二硫化碳浓度在0.200~20.0μg范围内线性关系良好,相关系数(R)为0.998;检出限为0.02 mg/kg,使用优化后的方法检出限比HJ 1054的检出限低0.02 mg/kg,低的百分比为40%;加标回收率为94.3%~98.1%;精密度为4.85%~11.1%(n=6)。该方法灵敏度高、操作简单、易于推广应用,适用于土壤和沉积物中硫代氨基甲酸酯(盐)类农药总量的测定。A method of determination of total dithiocarbamate( salt) pesticides in soil and sediment by Headspace Gas Chromatography was established.Mancozeb was used as the target for analysis. Weigh 2 g of sample into headspace bottle,and synthesized carbon disulfide in inorganic acid medium containing stannous chloride with an 80 ℃ constant temperature water bath oscillator.Carbon disulfide was separated by Agilent HP-5 column and detected with electron capture detector( ECD) and quantified cation by external standard method.As shown on the result,linear relationship of carbon disulfide was good in the range of 0.200 ~ 20.0 μg,and the correlation coefficient( R) was 0.998.The detection limit was 0.02 mg/kg,the detection limit of the optimized method is 0.02 mg/kg lower than that of HJ 1054,the low percentage is 40%. The recovery was 94.3% ~ 98.1%. The precision is 4.85% ~ 11.1%( n = 6). The method has the advantages of high sensitivity,simple operation and easy popularization and application.It applies to determination of total dithiocarbamate( salt) pesticides in soil and sediment.

关 键 词：衍生化 顶空-气象色谱仪 二硫代氨基甲酸酯(盐)类农药总量 代森锰锌 土壤 沉积物 

分 类 号：O657.7[理学—分析化学] X703.1[理学—化学]