自动固相萃取-GC/MS测定水中多环芳烃和有机氯农药  

Determination of PAHs and OCPs in Surface Water by Gas Chromatography/Mass Spectrometry with Automatic Solid-phase Extraction

作　　者：李斌[1] 解启来[1] 刘昕宇[1,2] 汤嘉骏 徐晨[1] 

机构地区：[1]华南农业大学资源环境学院,广东广州510642 [2]珠江流域水环境监测中心,广东广州510611

出　　处：《环境科学与技术》2014年第5期102-106,共5页Environmental Science & Technology

基　　金：广东省地质调查项目(1212010511216)

摘　　要：采用自动固相萃取-气相色谱／质谱技术，建立了地表水中痕量多环芳烃和有机氯农药的检测方法。调节水样pH〈2，加入1％甲醇，使用C18固相萃取柱富集，3mL丙酮＋3mL二氯甲烷洗脱后浓缩定容。采用气相色谱／质谱联用的全扫描模式进行分析，选择特征离子定量，方法检出限为0．026-8．772ng／L。加标水平为0．1μg/L时，样品加标回收率在74．8％～109％之间，RSD为0．01％～14．5％。该方法自动化程度高、快速、准确、重复性好，能满足地表水体中持久性有机污染物分析的要求。To determine trace amount of PAHs and OCPs in surface water a method was developed using gas chromatography/mass spectrometry with automatic solid-phase extraction. The steps elucidated in this paper were to adjust pH of the water sample to pH〈2, and add 1% methanol, then enrich the sample by C18 extraction cartridge; thereafter, PAHs and OCPs absorbed in the cartridge was eluted by 3 mL acetone plus 3 mL dichloromethane; the sample being concentrated, analysis was conducted by gas chromatography/mass spectrometry using the all-scan mode, and selective ion mass was used in quantitative measurement. Results of the experiment were limits of detection ranged from 0.026 to 8.772 ng/L; when average spiked recoveries for the fishery products at the spiked level attained 0.1 μg/L, ranging from 74.8% to 109%, RSD ranged from 0.01% to 14.5%. It was concluded that the method thus set up was rapid, accurate, sensitive and reliable, and could meet the requirement for analyzing persistent organic pollutants in surface water.

关 键 词：多环芳烃 有机氯农药 自动固相萃取 气相色谱 质谱 地表水 

分 类 号：X830.2[环境科学与工程—环境工程]