直接进样-液相色谱-串联质谱法同时测定水中的5种苯胺类化合物

Determination of Aniline Compounds in Water by Direct InjectionLiquid Chromatography-Tandem Mass Spectrometry

建立了直接进样测定生活饮用水及其水源水中5种苯胺类化合物（苯胺、3-硝基苯胺、4-硝基苯胺、2,6-二氯-4-硝基苯胺和六硝基二苯胺）的液相色谱-串联质谱法。水样经0.22μm聚醚砜滤膜过滤后直接进样,目标化合物在HSS T3色谱柱上经梯度洗脱,于4 min完成分离,多反应监测模式检测。5种苯胺类化合物在各自线性范围内线性良好,相关系数R≥0.995。方法的检出限为0.773~1.88μg/L（S/N=3）,定量限为2.58~6.27μg/L（S/N=10）;峰面积的日内和日间相对标准偏差（RSD）分别为0.8%~1.9%和3.3%~4.9%;样品加标回收率为84.1%~105.0%,加标样品的RSD为1.0%~3.1%。应用本方法对35份水样进行了分析。结果表明,本方法准确、灵敏、快速,适用于生活饮用水及其水源水的常规分析,可为苯胺类化合物的污染评价提供技术支持。

A method of direct injection and liquid chromatography coupled with tandem mass spectrometric （LC-MS / MS） was developed for simultaneous determination of 5 aniline compounds including aniline, 3-nitroaniline, 4-nitroaniline, 2,6-dichloro-4-nitroaniline and hexanitrodiphenylamine in drinking water and source water. The samples were filtered using a 0. 22-μm polyethersulfone membrane prior to HPLC analysis. Five target compounds were chromatographically separated on an HSS T3 column with gradient elution. Chromatographic data were acquired by tandem mass spectrometric detection in multiple reaction monitoring （MRM） mode, and thus favorable resolutions of all target compounds were achieved within 4 min. Under the optimal analytical conditions, the peak area of each analyte and its concentration had a good correlation within the linear range （R≥0. 995）. The limit of detection （LOD） and limit of quantification （LOQ） of the method were 0. 773-1. 88 μg / L （S / N=3） and 2. 58-6. 27 μg / L （S / N=10）, respectively. The intra- and inter-day relative standard deviations （ RSDs） of the mix standard solution were 0. 8% -1. 9% and 3. 3% -4. 9% , respectively. The spiked recoveries of the analytes were 84. 1% -105% and the RSDs of the spiked samples were 1. 0% -3. 1% . This proposed method was applied in the analysis of 35 samples from drinking water, source water and surface water, which indicated that the novel LC-MS / MS method could detect 5 aniline compounds in water without any complicated sample pretreatment in an accurate, sensitive and rapid way, and it also could provide technique support for evaluation of the contamination caused by aniline compounds.