液相色谱/质谱法测定水中硝基苯酚类化合物

摘要

建立了液液萃取(LLE)-液相色谱/质谱法(LC-MS)测定水中7种硝基苯酚类化合物的方法.考察了pH值、盐加入量、萃取溶剂种类及体积等影响因素,确定pH<2、盐30 g、萃取剂二氯甲烷:乙酸乙酯(1:2,V:V)、用量150 mL为最优实验条件.结果表明,该方法对7种硝基苯酚类化合物分离度好,加标回收率为62.7%~89.9%,相对标准偏差RSD(n=6)为5.59%~16.8%,方法检出限为0.019~0.050 μg/L.本方法简单、灵敏度高,可满足水中硝基苯酚类化合物的分析要求.%A method for the determination of 7 kinds of nitrophenol compounds in water was established by liquid-liquid extraction and liquid chromatography-mass spectrometry. The parameters affected the extraction efficiency,such as pH,salt addition,extraction solvent and volume,were studied. Extraction efficiency reached a maximum when pH<2,the salt addition were 30 g,extraction solvent were dichloromethane:ethyl acetate=1:2(V:V) and volume were 150 mL,respectively. The result demonstrated that nitrophenol compounds can be separated completely with the recoveries range of 62.7%~89.9%. The relative standard deviation RSD (n=6) were in the range of 5.59%~16.8%,and the method detection limits were from 0.019 μg/L to 0.050 μg/L. The method was simple,high sensitive and applicable to the determination of nitrophenol compounds in water.