顶空固相微萃取-气相色谱法测定水中痕量多氯酚  

Determination of trace polychlorophenols in water using HS/SPME-GC/ECD

作　　者：王玉飞[1] 李继革[1] 施家威[1] 

机构地区：[1]宁波市疾病预防控制中心,宁波市毒物研究与控制重点实验室,浙江宁波315010

出　　处：《中国卫生检验杂志》2013年第14期2891-2892,共2页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立顶空固相微萃取(HS/SPME)-气相色谱法测定水中痕量2,4,6-三氯酚、2,3,4,6-四氯酚和五氯酚的测定方法。方法水样经盐酸酸化和氯化钠饱和,60℃搅拌平衡10 min,聚丙烯酸酯萃取头(PA,85μm)萃取10 min后,在280℃下解吸3.0 min,用HP-5毛细管色谱柱分离,ECD检测器检测。结果三种多氯酚在0.05μg/L^10μg/L范围均具有良好的线性,相关系数r均大于0.999,水中检出限均小于0.002μg/L,方法回收率在89.7%~111.3%之间,方法的相对标准偏差均小于6.8%。结论顶空固相微萃取气相色谱法同时测定水中2,4,6-三氯酚、2,3,4,6-四氯酚和五氯酚,方法无需有机溶剂;具有环保、快速、准确、灵敏的优点,适用于水中痕量多氯酚的检测。Objective To establish a method for determination of trace 2,4,6 - trichlorophenol, 2,3,4,6 - tetrachlorophenol and pentachlorophenol in water samples by gas chromatography with headspace solid - phase microextraction （ HS/SPME ）. Methods The samples were acidified with hydrochloric acid and saturated with sodium chloride to maintain an agitating equilibrium at 60 ℃ for lOmin, then extracted for 10 min using a 85 txm polyacrylate coated fiber and desorbed at 280℃ for 3.0 min, and finally detected with GC/ECD. Results The linear ranges of the method for the three polychlorophenols were from 0.05 μg/L to 10 μg/L with the correlation coefficients （r） above 0. 999. The average recoveries were in the range of 89.7% - 111.3% and the relative standard deviations were less than 6.8% with the detection limits less than 0. 002 μg/L. Conclusion The method is rapid, sensitive, solvent - free and it is suitable for determination of trace polychlorophenols in water samples.

关 键 词：固相微萃取 2  4  6-三氯酚 2  3  4  6-四氯酚 五氯酚 水 气相色谱法 

分 类 号：O657.71[理学—分析化学]