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 dichlo-romethane 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.%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=2524X-6029、Y= 1809X-11341、Y= 2296X- 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0.1 ng/L;定量限(LOQ)分别为6.7,10.1和0.3 ng/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.
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