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全自动固相萃取-气相色谱-质谱法测定饮用水源中16种多环芳烃
引用本文:聂丹丹,徐斌,代飞飞. 全自动固相萃取-气相色谱-质谱法测定饮用水源中16种多环芳烃[J]. 现代预防医学, 2016, 0(23): 4358-4361
作者姓名:聂丹丹  徐斌  代飞飞
作者单位:潍坊市疾病预防控制中心,山东 潍坊 261061
摘    要:目的 建立全自动固相萃取-气相色谱/质谱联用法快速检测饮用水源中16种多环芳烃,了解本市饮用水源中多环芳烃的污染状况。方法 水样用盐酸调pH<2,再加入30ml甲醇混匀上样,上样流速为10 ml/min,被测物质经Thermo HyperSep C18小柱富集后,用乙酸乙酯和二氯甲烷洗脱,采用程序升温,TG-5MS色谱柱分离,质谱检测,利用保留时间和选择离子监测(SIM)模式进行定性定量。结果 16种化合物相关系数大于0.998,检出限(MDL)为0.006 9ng/L~0.074ng/L,样品平均加标回收率在82.5%~119.2%之间,相对标准偏差(RSD)6.07%~9.97%。结论 该方法具有较高的准确度与精密度,操作简便、快速,溶剂用量少,适合于水中16种多环芳烃的测定。

关 键 词:多环芳烃  气相色谱/质谱法  全自动固相萃取  饮用水源

Simultaneous detection of 16 polycyclic aromatic hydrocarbons in source water by fully automatic SPE-gas chromatography - mass spectrometry
NIE Dan-dan,XU Bin,DAI Fei-fei. Simultaneous detection of 16 polycyclic aromatic hydrocarbons in source water by fully automatic SPE-gas chromatography - mass spectrometry[J]. Modern Preventive Medicine, 2016, 0(23): 4358-4361
Authors:NIE Dan-dan  XU Bin  DAI Fei-fei
Affiliation:Weifang Center for Disease Control and Prevention,Weifang,Shandong 261061,China
Abstract:Objective To establish a gas chromatography-mass spectrometry (GC-MS) with fully automatic solid-phase extraction (SPE) for determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water and to know the status of PAHs pollution in source water. Methods After the pH of water sample was adjusted to less than 2,30 ml of methanol was added and the sample solution was extracted with Thermo HyperSep C18 solid phase column,and then eluted with ethyl acetate and methylene chloride,and then separated with TG-5MS chromatographic column using temperature programming,and finally quantitatively and qualitatively detected by retention time and selected ion monitoring mode (SIM). Results The correlation coefficients were greater than 0.998,and the detection limits (MDL) were 0.0069 ng/L~0.074 ng/L.The average recoveries of the method ranged from 82.5% to 119.2% with the relative standard deviations (RSDs) of 6.07%~9.97%. Conclusion The method is simple,rapid,sensitive,accurate and it is suitable for the simultaneous determination of 16 PAHs in source water.
Keywords:Polycyclic aromatic hydrocarbons  GC-MS  Full automatic SPE  Source water
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