摘要
为了有效监测环境水体中的有机氯农药(OCPs)残留,本研究开发了一种低消耗、弱基质效应、经济便捷的固相微萃取技术测定水中13种OCPs残留的方法。应用具有强选择性的硅橡胶(SR)薄膜为固相吸附材料,制备了简便易操作的固相萃取瓶,通过优化萃取方式、萃取时间、洗脱溶剂以及洗脱方式等条件,选择涡旋10 min进行SR薄膜对目标物的萃取,利用5 mL V_(正己烷):V_(乙酸乙酯)=1:1溶液洗脱SR薄膜上目标物,采用气相色谱仪进行检测。结果表明:方法检出限在0.001~0.132μg/L之间,定量限为0.2μg/L;决定系数(R^(2))>0.9973;在0.2、1、20μg/L 3个添加水平下,13种农药在水中OCPs的平均回收率在73%~109%之间,相对标准偏差在0.5%~13%之间(n=5)。利用该方法对巢湖、南淝河等合肥市内主要河流进行了13种OCPs残留的检测,结果发现13种OCPs的最高检出质量浓度为3.64μg/L。与已所报道的方法相比,该方法具有灵敏度高、操作简便、成本低等特点,在环境水体OCPs多残留痕量监测领域具有良好的应用前景。
To effectively monitor the residues of organochlorine pesticides(OCPs)in environmental water,this study developed a low-cost,weak matrix effect,and economically convenient solid-phase microextraction method to determine 13 OCPs residues in water.This approach used a highly selective silicone rubber(SR)thin film as the solid-phase adsorbent to prepare an easy-operate extraction bottle.After the optimization of the extraction mode,extraction time,elution solvent,and elution mode,vortexing for 10 min was selected for the adsorption of target compounds by the SR film,and 5 mL of V(hexane):V(ethyl acetate)=1:1 was used to elute the target compounds from SR film.The detection of 13 OCPs was performed by gas chromatography.The results showed that the limits of detection for the 13 OCPs ranged from 0.001 to 0.132μg/L,and the limit of quantification was 0.2μg/L.The linearity was good with the determination coefficients(R^(2))higher than 0.9973.The average recoveries of 13 OCPs in water spiked at three levels of 0.2,1,and 20μg/L were in a range of 73%-109%with relative standard deviations of 0.5%-13%(n=5).The method was finally employed for the monitoring of the 13 OCPs in several water samples collected from Chao Lake,Nanfei River and other major rivers in Hefei City,and the highest detection mass concentration was 3.64μg/L.Compared with the previously reported methods,the proposed method features high sensitivity,simplicity in operation,and low cost,showing promising prospects in the multi-residue determination of OCPs in environmental water.
作者
薛佳莹
李赐云
蒋晴晴
徐绘茹
吴祥为
花日茂
XUE Jiaying;LI Ciyun;JIANG Qingqing;XU Huiru;WU Xiangwei;HUA Rimao(Anhui Provincial Key Laboratory of Hazardous Factors and Risk Control of Agri-food Quality Safety/College of Resources and Environment,Anhui Agricultural University,Hefei 230036,China)
出处
《农药学学报》
CAS
CSCD
北大核心
2024年第6期1181-1190,共10页
Chinese Journal of Pesticide Science
基金
安徽省重点研究与开发计划(2022l07020016)
安徽省高等学校科学研究重点项目(No.2023AH050985)
安徽省研究生教育质量工程项目(2023yjshhsfkc011).
关键词
有机氯农药
硅橡胶薄膜
固相微萃取
气相色谱-电子捕获检测器
环境水体
残留
organochlorine pesticides
silicone rubber film
solid-phase microextraction
gas chromatography-electron capture detector
environmental water
residue
