高效液相色谱-电喷雾离子源-串联三重四极杆质谱法分析地表水中高氯酸盐  

Determination of Perchlorate in Surface Water by High Performance Liquid Chromatography-Electrospray Ion Source-Tandem Mass Spectrometry

作　　者：谢永洪[1] 杨坪[1] 钱蜀 姚欢[1] 谢振伟[1] 万旭[1] 葛军[1] 

机构地区：[1]四川省环境监测中心站,四川成都610041

出　　处：《中国环境监测》2014年第1期164-168,共5页Environmental Monitoring in China

摘　　要：建立了高效液相色谱-电喷雾离子源-串联三重四极杆质谱（ HPLC-ESI-MS/MS）测定地表水中高氯酸盐的方法。以Dionex IonPac AG20阴离子交换柱为分析柱，弱碱性的0.056％氨水/5 mmol/L乙酸氨为流动相，1.0 mL/min的流速，电喷雾负离子模式电离，MS/MS串联质谱为检测器，多反应监测（ MRM）模式检测高氯酸盐。方法检出限达0.043μg/L，线性范围为0.2～50μg/L，线性相关系数为0.9994，含量分别约为2、6、30μg/L的实际样品进样10次得到的相对标准偏差分别为2.47％、4.55％、0.49％，样品加标回收率在80％～109％，将该法与 US EPA method314.0进行比对，结果基本吻合。A method was developed for determination of perchlorate in surface water based on high performance liquid chromatography-electrospray ion source-tandem mass spectrometry （ HPLC-ESI-MS/MS） . The anion exchange column of Dionex IonPac AG20 was used as the analytical column with the weakly alkaline mobile phase of 0.056% ammonia/5 mmol/L Ammonium acetate and the flow rate of 1.0 mL/min.-ESI MS/MS was used as the detector and the perhclorate was detected under multiple reaction monitoring（ MRM） mode. The detection limit of the developed method was 0.043 μg/L and the linear range was 0.2-50μg/L with the linear correlation coefficient of 0.999 4, the relative standard deviation for about 2, 6, 30 μg/L sample were 2.47%, 4.55%, 0.49%, respectively. Content recovery percentages ranging from 80% to 109% were obtained and the analysis results were of agreement with that analyzed by US EPA method314.0.

关 键 词：高效液相色谱-电喷雾离子源-串联三重四极杆质谱 高氯酸盐 地表水 

分 类 号：X832[环境科学与工程—环境工程]