自动顶空固相微萃取与气相色谱-质谱联用同时测定饮用水中的4种氯酚  

Determination of four chlorophenols in drinking waters using gas chromatography-mass spectrometry coupled with auto headspace solid-phase micro extraction

作　　者：朱惠芳[1] 胡美华[1] 胡贵祥[1] 

机构地区：[1]南昌市疾病预防控制中心,江西南昌330038

出　　处：《现代预防医学》2015年第11期2037-2039,2041,共4页Modern Preventive Medicine

摘　　要：目的建立同时检测生活饮用水中2-氯酚、2,4-二氯酚、2,4,6-三氯酚、五氯酚的自动顶空固相微萃取气相色谱-质谱联用方法。方法用聚丙烯酸酯（PA）进行萃取,对萃取时间、离子强度、震荡频率进行了优化,采用进样口温度：280℃;离子源温度：220℃;接口温度：280℃;柱温为程序升温：初温40℃保持3 min,以20℃/min升至180℃,保持1 min,以20℃/min升至240℃,保持5 min,不分流进样。质谱采用电子轰击离子源（EI）,选择离子方式（SIM）检测,外标法定量。结果方法的最小检出限为0.008～0.020μg/L,相对标准偏差3.17%～6.31%,回收率为85.6%～120.0%。结论样品处理简单,检测速度快,检出限较国标方法降低,可作为检测水中四种氯酚含量的有效方法。Objective To establish a method for simultaneous determination of four chlorophenols including 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol in drinking waters by gas chromatography-mass spectrometry with auto headspace solid-phase micro extraction. Methods The samples were extracted by polyacryiate （PA） and the factors such as extraction temperature, ion strength and the stir speed were optimized. The best analysis conditions were as follows： injector temperature： 280℃, ion source temperature： 220℃, interface temperature： 280℃. The initial column temperature was set at 40℃ and held for 3 min. Then the temperature increased to 180℃ at 20℃/min which was held for 1 min. Finally the temperature increased to 240℃ at 20℃/min which was held for 5 min. The mode of injection was splitless. EI and SIM modes were used in the MS detection and the external standard was used for quantification. Results The detection limits ranged from 0.008 to 0.02 Ixg/L. The RSDS were between 3.17 % and 6.31% and the recoveries were from 85.6 % to 120 %. Conclusion The pretreatment method was simple and fast and the LODS were much lower than those of national standard method. It was a suitable method to determine 4 chlorophenols in drinking waters.

关 键 词：自动顶空固相微萃取 气相色谱-质谱联用 多种氯酚 生活饮用水 

分 类 号：R115[医药卫生—公共卫生与预防医学]