全自动在线固相萃取-液质联用测定水中两类溴代阻燃剂  

Rapid determination of hexabromocyclododecane and tetrabromobisphenol A in water by fully automated online solid phase extraction and ultraperformance liquid chromatography-tandem mass spectrometry

作　　者：张蓓蓓[1] 章勇[1] 穆肃[1] 胡冠九[1] 王荟[1] 

机构地区：[1]国家环境保护地表水环境有机污染物监测分析重点实验室、江苏省环境监测中心,南京210036

出　　处：《环境化学》2014年第3期477-484,共8页Environmental Chemistry

基　　金：2012年环保公益性行业科研专项课题(项目编号:201209016)资助

摘　　要：建立了全自动在线固相萃取(online SPE)-超高效液相色谱/三重四极杆串联质谱(UPLC-MS/MS)同时测定水中六溴环十二烷和四溴双酚A的方法.过滤后的水样经自动进样器上样至在线HLB萃取柱,经淋洗液清洗杂质后,采用反冲梯度洗脱将萃取柱上吸附的目标物洗脱到C18色谱分析柱上进行分离,采用串联质谱进行检测.4种目标化合物在相关线性范围内线性良好(r=0.9915—0.9981),回收率为83.2%—114%,相对标准偏差为7.6%—14.5%,方法检出限为0.003—0.014μg·L-1.本方法快速环保,灵敏度和精密度高,适用于测定受污水体中4种溴代阻燃剂的痕量残留.A new method for the analysis of hexabromocyclododecane and tetrabromobisphenol A in water, based on the use of fully automated online solid phase extraction followed by ultra-performance liquid chromatography-tandem mass spectrometry method （online SPE-UPLC-MS/MS）, is reported. The samples were first injected by auto-sampler to the online SPE column continuously, followed by clean-up step using loading pump with gradient program. Then the online SPE column was introduced to the analytical flow path by valve switching and the analytes were back-flushed to the analytical column using analytical pump for further determination. The HLB cartridge（2.1 mm×30 mm,20 μm）was employed as online SPE column and a BEH C18（2.1 mm×100 mm,1.7 μm）as analytical column, the flow of loading pump was set at 2.0 mL·min-1 while the analytical pump was 0.3 mL·min-1. Gradient programs were used for the sample clean-up and determination in both pumps. The injection volume was 5—15 mL and the total analysis time was 15 min. This method was fully validated in the terms of linearity （r=0.9915—0.9981）, limit of detection （0.003—0.014 μg·L-1）, precision （7.6%—14.5%） and accuracy （83.2%—114%）. The results showed that the proposed method could be used for the determination of trace level brominated flame retardants in water.

关 键 词：六溴环十二烷 四溴双酚A 全自动在线固相萃取-超高效液相色谱 串联质谱 受污水体 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]