自动固相萃取-气相色谱-质谱法测定生活饮用水中60种半挥发性有机物

目的提出一种同时测定生活饮用水中60种半挥发性有机物的自动固相萃取-气相色谱-质谱联用法。方法1 L水样中加入5 m L甲醇,通过自动固相萃取装置使用LC-Florisil固相萃取柱对水样进行富集,再分别用5 m L二氯甲烷和5 m L乙酸乙酯洗脱,氮吹浓缩定容至1 m L,进样分析。结果60种半挥发性有机物在(0.125~4.00)μg/L的含量范围内具有较好的线性,其相关系数均≥0.99,方法检出限为(0.002~0.06)μg/L,检测限为(0.01~0.26)μg/L,回收率范围70.8%~129%,精密度(RSD)范围0.2%~21.5%。结论该方法实现了前处理过程自动化,具有准确度高、操作简单和溶剂使用量少等优点,适用于同时测定生活饮用水中60种半挥发性有机物。

Determination of 60 Semi-Volatile Organic Compounds in Drinking Water Using Automatic Solid Phase Extraction-Gas Chromatography-Mass Spectrometry

Objectives To develop a method for simultaneous determination of 60 semi-volatile organic compounds in domestic drinking water using automatic solid phase extraction-gas chromatography-mass spectrometry( GC-MS). Methods 5 m L methanol was added to 1 L water sample. Then the water sample was enriched by LCFlorisil SPE using automatic solid phase extraction equipment,and was eluted with 5 m L dichloromethane and 5 m L ethyl acetate,the eluent was concentrated with nitrogen to 1 m L and determined. Results The 60 semi-volatile organic compounds showed a good linearity in the range of( 0. 125-4. 00) μg/L,and the correlation coefficients were all more than 0. 99. The method detection limits was in the range of 0. 002-0. 04 μg/L and the detection limits was in the range of 0. 01-0. 17 μg/L. The recoveries ranged from 70. 8% to 129% and the relative standard deviations( RSD) ranged from 0. 2% to 21. 5%. Conclusions The method has realized the automatic pretreatment which has advantages of high accuracy,simple operation and less solvent. This method was suitable for simultaneous determination of 60 semi-volatile organic compounds in domestic drinking water.