固相萃取-液相色谱-串联质谱法测定氯化消毒副产物二氯对苯醌

目的 建立饮水中新型氯化消毒副产物二氯对苯醌的固相萃取-液相色谱-串联质谱检测方法。方法 水样经0.45 μm滤膜过滤，用 Oasis HLB 固相萃取小柱富集进样，以含0.25%甲酸甲醇溶液-0.25%甲酸的水溶液为流动相，梯度洗脱，经Agilent ZORBAX Eclipse XDB-C18色谱柱（2.1 mm×50 mm，1.8 μm） 分离后，采用四极杆串联质谱仪电喷雾负离子模式和多反应监测（MRM）模式进行检测。结果 二氯对苯醌在2～100 μg/L的范围内回归方程为Y = 12.978x + 0.285，线性相关系数r = 0.9937；方法检出限为0.01 μg/L，定量下线限为0.03 μg/L。管网末梢自来水加标回收率为80.0％～85.0％，相对标准偏差(RSD)为3.4%～4.1%。结论 方法的灵敏度和准确度较高，适用于饮用水中二氯对苯醌的测定。

Determination of chlorination by-products 2,6-dichloro-1,4-benzoquinone in drinking water by HPLC-MS/M

Objective The aim of this study was to establish a method for the determination of 2,6-dichloro-1,4-benzoquinone(DCPQ) in water by liquid chromatography tandem mass spectrometry(HPLC-MS/MS). Methods The sample was extracted with Oasis HLB solid phase extraction column after filtrated with 0.45 μm membrane, then separated using an Agilent ZORBAX Eclipse XDB-C18 column with 0.25% formic acid and methanol aqueous solution as the mobile phase for gradient elution. And the tandem mass spectral acquisition was accomplished in the negative electrospray ionization utilizing multiple reaction monitoring. Results The linear range of the method was from 2 to 100 μg/L with the correlative coefficient above 0.9937. The limit of detection was 0.01 μg/L and the limit of quantification(LOQs) was 0.03 μg/L. The mean recoveries for tap water samples at spiked concentrations levels of 2-100 μg/L ranged from 80.0% to 85.0% with RSDs of 3.4%-4.1% (n=6). Conclusion The method is sensitive and accurate and it could be used for determination of DCPQ in drinking water.