固相萃取-高效液相色谱串联质谱法同时检测地表水中的2,4-二氯酚、2,4,6-三氯酚和五氯酚  

Simultaneous Determination of 2,4-Dichlorophenol,2,4,6-Trichlorophenol and Pentachlorophenol in Surface Water by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction

作　　者：杨秋红[1] 程小艳[2] 杨坪[2] 钱蜀 但德忠[1] 

机构地区：[1]四川大学建筑与环境学院,成都610065 [2]四川省环境监测中心站,成都610041

出　　处：《分析化学》2011年第8期1208-1212,共5页Chinese Journal of Analytical Chemistry

摘　　要：建立了简便、快速、同时测定地表水中2,4-二氯酚、2,4,6-三氯酚和五氯酚的固相萃取-高效液相串联质谱方法。HLB固相萃取小柱富集水样中待测物质,经二氯甲烷-丙酮(1∶1,V/V)混合溶液洗脱后,氮吹浓缩,溶剂转换为甲醇,采用高效液相色谱串联质谱检测,选择反应监测模式(SRM),进行特征母离子-子离子采集信号。本方法对2,4-二氯酚、2,4,6-三氯酚和五氯酚检测的线性方程分别为Y=2524 X-6029、Y=1809 X-11341、Y=2296 X-2894,相关系数分别为0.9993、0.9996和0.998;检出限(LOD)分别为2.0,3.0和0.1ng/L;定量限(LOQ)分别为6.7,10.1和0.3ng/L;7次加标回收相对标准偏差在2.2%～14.7%之间;回收率为70.5%～102.3%,能很好地满足水源地监测的需求。A novel method was developed for the simultaneous determination of 2,4-dichlorophenol,2,4,6-trichlorophenol and pentachlorophenol in surface water by HPLC-MS/MS with solid phase extraction.The sample was concentrated by HLB extraction cartridge,and then eluted with dichloromethane and acetone eluants.The solvent was changed into methanol after drying by nitrogen blow.Quality and quantity analysis was carried out by HPLC-MS/MS with SRM mode.Under the experimental condition,the linear regress equations were Y=2524X-6029,Y=1809X-11341 and Y=2296X-2894,the correlation coefficients were 0.9993,0.9996 and 0.9989,the detection limits were 2.0,3.0 and 0.1 μg/L,the limits of quantification were 6.7,10.1 and 0.32 ng/L respectively,and a recovery ranged of 70.5%-102.3% with a RSD between 2.2% and 14.7%（n=7） were obtained.The method has good innovative,advanced and practical value.

关 键 词：氯酚 固相萃取 高效液相串联质谱法 地表水 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]