摘要
克百威和3-羟基克百威是一对典型的农药母体及其代谢产物,由于其水溶性高、毒性大,可通过地表水或地下水进行长距离迁移,对人类健康和环境安全造成危害。以往通常采用液相萃取或固相萃取的方式提取样品中的克百威和3-羟基克百威,但这些方法操作繁琐、耗时较长,不利于室内模拟实验中多组样品的检测。为实现克百威与3-羟基克百威在地下水中的快速定量,本文建立了一种小体积液液萃取的前处理方法进行提取,并采用气相色谱-质谱(GC-MS)进行检测,对影响克百威和3-羟基克百威萃取效率的因素进行了研究。通过实验对比不同萃取剂、不同pH、不同离子强度条件下克百威与3-羟基克百威的回收率,优化了前处理条件。结果表明,选择二氯甲烷作为萃取剂且用量为1mL,调节水样pH=5,氯化钠用量为40g/L时克百威和3-羟基克百威的回收率最高,分别为75.1%~98.6%、55.0%~66.3%。性能评价结果显示,方法精密度和方法准确度满足测试要求(相对标准偏差<10%,n=5),克百威和3-羟基克百威的方法检出限分别为15.3μg/L、10.2μg/L。该方法操作简便、快速、消耗溶剂少,与传统的液液萃取法相比,本方法耗时约为前者的1/8,消耗溶剂量约比前者小2个数量级,能够满足室内模拟实验需求。
BACKGROUND:Carbofuran and 3-hydroxycarbofuran are typical pesticides with the relationship of parent and metabolite.Due to high water solubility and toxicity,carbofuran and 3-hydroxycarbofuran can be transported through surface water or groundwater for long distances,causing harm to human health and environmental safety.In the past,carbofuran and 3-hydroxycarbofuran in samples were usually extracted by liquid or solid phase extraction.However,these methods are cumbersome to operate and time-consuming,which is not conducive to the detection of multiple sets of samples in indoor simulation experiments.OBJECTIVES:In order to realize the rapid quantification of carbofuran and 3-hydroxycarbofuran in groundwater.METHODS:A small volume liquid-liquid extraction pretreatment method was established for extraction,combined with gas chromatography-mass spectrometry to detect factors affecting the extraction efficiency of carbofuran and 3-hydroxycarbofuran.To improve the extraction efficiency of carbofuran and 3-hydroxycarbofuran,factors such as the type of extraction solvent,pH and dosage of NaCl were optimized.RESULTS:Results showed that the extraction efficiency of carbofuran and 3-hydroxycarbofuran was highest when 1mL methylene chloride was selected as the extraction agent under pH=5,and 40g/L NaCl was added in the water samples.The extraction recoveries for carbofuran and 3-hydroxycarbofuran were 75.1%-98.6%and 55.0%-66.3%,respectively.The performance evaluation results showed that the instrument precision and method precision meet test requirements(n=5,relative standard deviation<10%).The detection limits of carbofuran and 3-hydroxycarbofuran in water were 15.3μg/L and 10.2μg/L,respectively.CONCLUSIONS:This method is simple and fast with less solvent.Compared with the traditional liquid-liquid extraction method,this method takes about 1/8 time of the former,and consumes about two orders of magnitude less solvent than the former,which can meet the needs of indoor simulation experiments.
作者
周添
刘菲
ZHOU Tian;LIU Fei(Beijing Key Laboratory of Water Resources and Environmental Engineering,China University of Geosciences(Beijing),Beijing 100083,China)
出处
《岩矿测试》
CSCD
北大核心
2021年第3期358-364,共7页
Rock and Mineral Analysis
基金
中国地质调查局地质调查项目“地下水中有机污染组分对补给方式的响应——水样测试分析质量控制”(DD20190323)。
关键词
克百威
3-羟基克百威
小体积液液萃取
气相色谱-质谱法
carbofuran
3-hydroxycarbofuran
small volume liquid-liquid extraction
gas chromatography-mass spectrometry
