超高效液相色谱-串联四极杆质谱分析环境水样中对苯二胺  

Determine p-Phenylenediamine in Water Sample by UPLC-Tandem Mass Spectrometry

作　　者：熊杰[1] 钱蜀 李海霞[1] 谢永洪[1] 

机构地区：[1]四川省环境监测中心站,成都610041

出　　处：《四川环境》2013年第3期24-27,共4页Sichuan Environment

摘　　要：本文建立了超高效液相色谱-串联四极杆质谱分析环境水样中对苯二胺的分析方法。方法使用C18反相柱为分离柱,柱温30℃,流速0.3ml/min,80%甲醇+20%纯水作流动相,保留时间1.92min,使用具ESI(+)源的质谱作检测器。在此条件下,水样过0.45μm滤膜后可直接进样,进样体积10μl,检出限可达0.028μg/L,在0.10～4.00μg/L范围内线性良好(R=0.9998);相对标准偏差在0.7%～4.9%之间,样品加标回收率在88.2%～118%之间,应用到实际环境水样分析中也具有令人满意的结果。该方法灵敏度高,快速简单,适用于环境水样中对苯二胺的分析。A new method was developed for determine p-Phenylenediamine in water sample by ultra performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS）. Chromatographic separation was performed on C18 reversed phase column, the chromatographic conditions for the determination of p-Phenylenediamine are as follows： column temperature, 30℃, flowrate, 0.3mL/min, mobile phase, methanol （80%） ＋ water （20%）, retention time, 1.92min. The detection was performed by tandem mass spectrometry with eleetrospray ionization in positive mode （ ESI ＋ ）. Under above conditions, the detection limit was 0. 028μg/L. The calibration curve showed good linearity from 0. 1 to 4. 0 μg/L for p-Phenylenediamine with the correlation coefficient 0. 9998. The relative standard deviation was 0. 7% - 4. 9% . The recovery rate was 88.2% - 118%, precision and accuracy all can meet the demands of quality control. The proposed method was successfully applied to determine p-Pbenylenediamine in practical water sample. This method was highly sensitive, fast and simple, therefore can be used for determination of p-Phenylenediamine in water samples.

关 键 词：对苯二胺 水样 超高效液相色谱-串联四极杆质谱 

分 类 号：X832[环境科学与工程—环境工程]