高效液相色谱-串联质谱法测定水体中三氯酚的6种同分异构体

Determination of Six Isomers of Trichlorophenol in Water by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了同时测定水体中6种三氯酚(2,3,4-三氯酚、2,3,5-三氯酚、2,3,6-三氯酚、2,4,5-三氯酚、2,4,6-三氯酚、3,4,5-三氯酚)的高效液相色谱-串联质谱法(HPLC-MS/MS)。水样经0.22μm水系滤膜过滤后直接进样,经Waters Atlantis^(TM) Premier BEH C18 AX柱(2.1×100 mm,1.7μm)分离,用0.5%NH_(3)·H_(2)O和乙腈进行梯度洗脱,采用电喷雾离子源负离子扫描,以多反应监测模式(MRM)检测,能在6 min内实现6种三氯酚质谱的同时分离分析。在0.02 mg/L~0.5 mg/L范围内,6种三氯酚线性关系良好,相关系数r^(2)大于0.9994,检出限为0.42~3.01μg/L;在0.02、0.05、0.1 mg/L三个浓度水平下回收率为100.9%~117.7%(n=5),相对标准偏差为0.6%~4.9%。该方法操作简便快捷,灵敏度和精密度高,满足饮用水实际检测的要求。

A fast and simultaneous determination method for six trichlorophenols(TCPs)has been developed,which was accomplished by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).All of six TCPs isomers(2,3,4-TCP,2,3,5-TCP,2,3,6-TCP,2,4,5-TCP,2,4,6-TCP,3,4,5-TCP)could be separated perfectly in this method.After the filtration through a 0.22μm water-based filter membrane,the samples were directly injected and separated on a Waters Atlantis^(TM) Premier BEH C18 AX Column(100 mm×2.1 mm,1.7μm),with 0.5%mass concentration ammonia solution and acetonitrile as the mobile phases.The electrospray ion source negative ion mode and multi-reaction monitoring(MRM)were applied in this method.The separation and determination of six TCPs could achieve within 6 minutes.Good linearity could be obtained in the range of 0.02-0.5 mg/L,with the linear correlation coefficient(r^(2))greater than 0.9994.The detection limits were in a range of 0.42-3.01μg/L.The recovery rates at the three concentration levels of 0.02 mg/L,0.05 mg/L and 0.1 mg/L were ranged from 100.9%to 117.7%(n=5),and the relative standard deviations were 0.6%to 4.9%.This method has the following advantages such as simplification,quickness,high sensitivity and precision,and meets the requirements of actual detection for drinking water.