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

依力哈木·扎依尔; 杨艳伟; 朱英; 胡小键; 陆一夫

doi:10.13421/j.cnki.hjwsxzz.2020.01.014

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

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

摘要

摘要:
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 mL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 mL二氯甲烷和5 mL乙酸乙酯洗脱，氮吹浓缩定容至1 mL，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。

Abstract:
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 mL methanol was added to 1 L water sample. Then the water sample was enriched by LC-Florisil SPE using automatic solid phase extraction equipment, and was eluted with 5 mL dichloromethane and 5 mL ethyl acetate, the eluent was concentrated with nitrogen to 1 mL 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.

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