超高效液相色谱-串联质谱法检测生活饮用水中卤代苯醌类消毒副产物

Determination of halobenzoquinone disinfection byproducts in drinking water by high performance liquid chromatography-tandem mass spectrometry

目的 建立测定生活饮用水中4种卤代苯醌类消毒副产物的超高效液相色谱-串联质谱法。方法 采用固相萃取柱Oasis HLB富集水样,在电喷雾离子源(ESI)和质谱多反应监测(MRM)模式下,建立固相萃取-液相色谱-串联质谱法测定饮用水中的2,6-二氯对苯醌、2,5-二氯对苯醌、2,5-二溴对苯醌、四氯-1,2-苯醌等4种卤代苯醌类消毒副产物。结果 在5 ng/L~500 ng/L线性范围内,4种卤代苯醌化合物的线性良好,相关系数均在0.998 5~0.999 4,可以进行定量检测。该方法的最低检出限为0.22 ng/L~0.51 ng/L,定量限为0.85 ng/L~2.33 ng/L。4种卤代苯醌在50 ng/L、100 ng/L、200 ng/L 3个浓度的加标量下,回收率在70.0%~96.4%(n=6),相对标准偏差为1.5%~4.7%。结论 本研究建立的方法灵敏度较高,能够满足对日常生活饮用水中4种卤代苯醌类消毒副产物的分析测量需要。

Objective This paper aims to establish a method for the simultaneous determination of 4 halobenzoquinone compounds in drinking water by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods Four halobenzoquinone compounds(2, 6-dichloro-p-benzoquinone, 2, 5-dichloro-p-benzoquinone, 2, 5-dibromo-p-benzoquinone, tetrachloro-1, 2-benzoquinone) in drinking water were concentrated by Oasis HLB solid phase extraction column and analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with electrospray ion source(ESI) and monitored in multiple reaction monitoring(MRM) mode. Results The method was fully validated to cover concentration ranges of 5 ng/L-500 ng/L for the 4 halobenzoquinones, and the linearity was good with correlation(r) between 0.998 5 and 0.999 4. Quantification detection is carried out. The limits of detection were 0.22 ng/L-0.51 ng/L for all the halobenzoquinones, while the limits of quantification were 0.85 ng/L-2.33 ng/L. The average recoveries of the studied halobenzoquinones spiked at levels of 50 ng/L,100.0 ng/L and 200 ng/L ranged from 70.0% to 96.4%(n=6) with the relative standard deviation(RSD) between 1.5 % and 4.7 %(n=6). Conclusion This validated method was sensitive to quantify the concentration of the 4 halobenzoquinone disinfection byproducts in water.