固相萃取法与GC-FPD联用分析海水中13种有机磷  

Determination of 13 Kinds of Organophosphorus Pesticides in Seawater by Solid Phase Extraction Coupled with Gas Chromatography-flame Photometric Detector

作　　者：彭诗琪 赵嘉辉 黄晓玲 吴志鹏 张傲 陈婷 赖华杰 PENG Shi-qi;ZHAO Jia-hui;HUANG Xiao-ling;WU Zhi-peng;ZHANG Ao;CHEN Ting;LAI Hua-jie(CAS Testing Technical Services(Guangzhou)Co.,Ltd.,Guangzhou 510650,China;New Materials Research Institute of CASCHEM(Chongqing)Co.,Ltd.,Chongqing 400700,China;Guangzhou Institute of Chemistry,Chinese Academy of Science,Guangzhou 510650,China)

机构地区：[1]中科检测技术服务(广州)股份有限公司,广东广州510650 [2]中科广化(重庆)新材料研究院有限公司,重庆400700 [3]中国科学院广州化学有限公司,广东广州510650

出　　处：《化学试剂》2022年第2期273-278,共6页Chemical Reagents

基　　金：广东省省级科技计划项目-粤东中科检测技术服务中心项目(2017A040403030)。

摘　　要：有机磷农药的广泛使用导致其不可避免地进入到环境中,不仅会影响生态环境,而且还会通过食物链富集进入到人体中,对人类健康造成影响。建立了固相萃取与GC-FPD联用的方法,并成功用于海水样品中敌敌畏等13种有机磷的分析。在中性条件下,100 mL水样经过HLB固相萃取小柱富集后,以二氯甲烷为洗脱溶剂进行洗脱,以HP-5柱为分离色谱柱,FPD为检测器,实现了对13种有机磷的分离及检测。对固相萃取柱和洗脱溶剂的种类、仪器条件等进行了探究,比较了C18、HLB、PSD 3种固相萃取柱对有机磷的吸附性能以及丙酮、二氯甲烷、乙酸乙酯3种溶剂的洗脱能力,考察了海水的基质效应对有机磷分析的影响。在最优的分析条件下,13种有机磷可实现基线分离,线性良好,相关系数均大于0.995,回收率在58.3%~114.0%之间,所建方法适用于海水样品中敌敌畏等13种有机磷的同时测定。The widespread abuse of organophosphorus pesticides leads to the inevitable release into environment,which not only affects the ecological environment,but also causes harm to human health through the enrichment of the food chain.The method of solid phase extraction(SPE)coupled with GC-FPD was established and successfully applied for the determination of 13 kinds of organophosphorus pesticides in seawater samples such as dichlorvos,etc.Under neutral condition,100 mL water sample was enriched by HLB column,and then dichloromethane was used for elution.The separation and determination of 13 kinds of organophosphorus pesticides was completed by using HP-5 as the chromatography column and FPD as the detector.The types of solid phase extraction column,elution solvent,and instrument condition were optimized.The adsorption performance of C18,HLB and PSD solid phase extraction columns for organophosphorus pesticides and the elution capacity of acetone,dichloromethane and ethyl acetate were compared,and the matrix effect was investigated.Under the optimized conditions,the separation baseline of analytes was achieved.The linear coefficients of analytes were more than 0.995,and the recovery rates were 58.3~114.0%.The established method was suitable for simultaneous determination of 13 kinds of organophosphorus pesticides.

关 键 词：有机磷农药 海水 固相萃取 气相色谱 基质效应 敌敌畏 

分 类 号：O657.7[理学—分析化学]