全自动固相萃取-UPLC-MS/MS法测定水中17种全氟化合物  

Determination of 17 perfluorinated compounds in water by fully-automated SPE-UPLC-MS/MS

作　　者：刘田 周宇齐 宋洲 吉义平 杨杰 方志成 LIU Tian;ZHOU Yu-qi;SONG Zhou;JI Yi-ping;YANG Jie;FANG Zhi-cheng(Hubei Geological Research Laboratory,Wuhan 430034,China;Hubei Key Laboratory of Resources and Eco-Environment Geology(Hubei Geological Bureau),Wuhan 430034,China)

机构地区：[1]湖北省地质实验测试中心,湖北武汉430034 [2]资源与生态环境地质湖北省重点实验室,湖北省地质局,湖北武汉430034

出　　处：《化学研究与应用》2025年第2期410-418,共9页Chemical Research and Application

基　　金：湖北省地质局科研项目(KJ2021-18、KJ2022-36、KJ2023-39)资助。

摘　　要：建立了全自动固相萃取-超高效液相色谱-三重四极杆串联质谱法(SPE-UPLC-MS/MS)检测水中17种全氟化合物(perfluorinated compounds,PFCs)。样品经全自动固相萃取仪富集、洗脱后,用电喷雾离子源(ESI)在选定的多反应监测(MRM)负模式下确定目标化合物并使用同位素内标法定量。考察了水样前处理洗脱液和样品瓶残留对目标物测定的影响,通过优化固相萃取条件,以及用甲醇润洗采样瓶去除采样瓶中PFCs残留、避免交叉污染,提高了目标物回收率。结果表明:17种PFCs的标准曲线线性相关系数(R^(2))均大于0.99,线性范围在1.00~100μg/L之间,检出限范围为0.2~0.9 ng/L。17种PFCs的低、中、高浓度加标回收率分别为62.5%~116%、66.8%~119%和64.7%~115%,相对标准偏差分别为1.79%~15.9%、0.40%~8.96%和0.98%~8.76%(n=6)。应用此方法检测了某电镀厂附近河塘17种PFCs的污染状况,表明该方法具有实际应用意义。A method for the determination of 17 perfluorinated compounds(PFCs)in water using fully automated solid-phase extraction ultra-high performance liquid chromatography triple quadrupole tandem mass spectrometry(SPE-UPLC-MS/MS)was established.After the water sample enriched and eluted by the fully automated SPE instrument,the target compounds determined by the electrospray ion source(ESI)under the selected negative mode of multi reaction monitoring(MRM)and quantified by the isotope internal standard method.The effects of sample pretreatment elution liquid,and residue in sample bottles on the determination of the target substance were examined,by optimizing solid-phase extraction conditions,and washing the sampling bottles with methanol to remove PFCs residues and avoid cross-contamination,the recovery rate of the target substance were improved.The linear correlation coefficients(R^(2))of the standard curves for 17 PFCs are all greater than 0.99,with a linear range of 1.00~100μg/L and a detection limit range of 0.2~0.9 ng/L.The recovery rates of 17 PFCs at low,medium,and high concentrations ranged from 62.5%~116%,66.8%~119%,and 64.7%~115%,respectively,with relative standard deviations of 1.79%~15.9%,0.40%~8.96%,and0.98%~8.76%(n=6).This method was applied to detect the pollution status of 17 PFCs in a river pond near a certain electroplating plant,indicating that the method has practical application significance.

关 键 词：全氟化合物 全自动固相萃取 液相色谱-三重四极杆串联质谱 

分 类 号：O657.6[理学—分析化学]