摘要
目的:建立饮用水中2,4-二氯酚,2,4,6-三氯酚和五氯酚的直接进样液相色谱串联质谱(LC-MS/MS)的同时快速检测方法。方法:水样过滤后直接进样测定,采用Waters SunFireTMC18(100 mm×2.1 mm,3.5μm)色谱柱分离,以甲醇+2 mmol/L乙酸铵水溶液(62+38,v/v)作为流动相,流速0.2 ml/min,采用电喷雾质谱电离,多反应监测模式(MRM)对目标化合物定性及定量分析,外标法定量。结果:3种氯酚的线性相关系数均大于0.9999;2,4-二氯酚、2,4,6-三氯酚和五氯酚的定量限(LOQ)分别为0.34μg/L、0.56μg/L和0.15μg/L;三种氯酚的高、中、低3个添加水平的平均加标回收率在96.0%～98.6%之间,相对标准偏差为0.8%～2.0%。结论:该方法灵敏度高、操作简单快速,适用于饮用水中氯酚的快速分析。
Objective：To establish a fast method for simultaneous determination of 2,4 - dichlorophenol, 2,4,6 - trichlorophenol and pentachlorophenol in drink water by LC - MS/MS with direct injection. Methods： The water samples were filtered and then injected into LC - MS/MS instrument. The separation was carried out by a Waters SunFireTM C18 （100 mm × 2.1 mm, 3.5μm） column using a mobile phase of methanol ＋ 2 mmol/L ammonium acetate water solution （62 ＋ 38, v/v） with a flow rate of 0.20 ml/min. The target compounds were confirmed and quantified by electrospray ionization mass spectrometry under multiple reactions monitoring （MRM） mode with exter- nal standard method. Results ： The correlation coefficients of 3 chlorophenols were more than 0. 9999. The limits of quantification （LOQ） of 2,4 - dichlorophenol, 2,4,6 - trichlorophenol and pentachlorophenol were 0.34 μg/L, 0.56μg/L and 0.15μg/L respectively. The average spiked recoveries of 3 chlorophenols at three concentration levels were between 96.0 % and 98.6 % , and the relative standard deviations （RSDs） ranged from 0.8% to 2.0%. Conclusion： The method was sensitive, simple and fast, and suitable for the fast determination and confirmation of chlorophenols in drinking water
出处
《中国卫生检验杂志》
北大核心
2013年第3期619-621,共3页
Chinese Journal of Health Laboratory Technology
