气相色谱-质谱法测定灌溉水中16种痕量多环芳烃  

Determination of 16 trace polycyclic aromatic hydrocarbons in irrigation water by gas chromatography-mass spectrometry

作　　者：李创 潘扬昌[1] 韦英亮[1] LI Chuang;PAN Yangchang;WEI Yingliang(Guangxi Zhuang Autonomous Region Center for Analysis and Test Research,Nanning 530022,China)

机构地区：[1]广西壮族自治区分析测试研究中心,南宁530022

出　　处：《化学分析计量》2023年第12期23-27,共5页Chemical Analysis And Meterage

基　　金：2021年广西科技计划项目(桂科AB21220068)。

摘　　要：建立气相色谱-质谱测定灌溉水痕量多环芳烃残留检测方法。水样加入2种替代物2-氟联苯和对三联苯-d_(14),通过二氯甲烷萃取,硅胶固相萃取柱净化,以二氯甲烷-正己烷(体积比为2∶8)混合溶剂洗脱,浓缩定容后加入萘-d_(8)、苊烯-d_(10)、菲-d_(10)、䓛-d_(12)和苝-d_(12)5种氘代多环芳烃混合物作为内标。选择离子扫描模式检测,目标物以保留时间和与标准物质质谱图比较进行定性,采用平均相对响应因子内标法定量。方法检出限为1~7 ng/L,线性范围为1~100μg/L,灌溉水加标回收率为82%~110%,精密度2.0%~10.6%。2种替代物回收率范围79%~105%,说明样品前处理过程稳定可靠,样品基体效应对分析结果的影响可以忽略。该方法操作简便、准确、高效,适用于基质相对复杂的灌溉水痕量多环芳烃残留检测。A method for the determination of trace polycyclic aromatic hydrocarbons(PAHs)residues in irrigation water by gas chromatography-mass spectrometry was established.Two surrogate standards,2-fluorobiphenyl and Pterphenyl-d_(14),were added to the water sample,extracted by dichloromethane,purified by silica gel solid phase extraction column,and eluted by mixed solvent of dichloromethane and hexane(volume ratio 2∶8).After concentration and constant volume,deuterated polycyclic aromatic hydrocarbons mixtures of naphthalene-d_(8),acenaphthene-d_(10),phenanthrene-d_(10),chrysene-d_(12) and perylene-d_(12) were added as internal standards and detected by gas chromatography mass spectrometry use selective ion scan mode.The qualitative analysis was conducted in terms of retention time and comparison with that mass spectrum of reference materials.The quantitative method was the internal standard method with average relative response factor.The detection limits of the method were 1-7 ng/L,and the linear ranges were 1-100μg/L.The recovery rates of irrigation water with standards were 82%-110%,and the precisions were 2.0%-10.6%.The recovery rates of the two surrogate standards ranges from 79%to 105%,indicating that the sample pretreatment process was stable and reliable,and the influence of sample matrix effect on the analysis results could be ignored.The method is simple,accurate and efficient,and is suitable for the determination of trace PAHs residues in irrigation water with relatively complex matrix.

关 键 词：气相色谱-质谱法 灌溉水 多环芳烃 

分 类 号：O657.7[理学—分析化学]