固相萃取-UPLC-MS/MS法测定水中17种全氟化合物

SPE-UPLC-MS/MS for Determination of 17 PFCs in Water

基于固相萃取-超高效液相色谱串联质谱建立了生活饮用水及水源水中17种全氟化合物的测定方法。水样经WAX固相萃取柱富集后用超高效液相色谱串联质谱测定,采用Cortecs C18色谱柱进行分离,流动相为含2 mmol/L乙酸铵的水和甲醇/乙腈(80∶20),采用多反应监测(MRM)模式测定,电喷雾电离源(ESI),负离子扫描。通过管材及捕集柱优化,在采样、样品前处理、检测等全过程消除了背景干扰。17种全氟化合物的标准曲线线性相关系数(R2)均大于0.99,定量限范围为0.083~1.56 ng/L。加标4种不同浓度时,生活饮用水(出厂水、管网水)的加标回收率为65.0%~117.8%,相对标准偏差为0.13%~17.93%;水源水的加标回收率为67.0%~117.8%,相对标准偏差为0.60%~18.71%。与国标中规定的11种全氟化合物的超高效液相色谱串联质谱检测方法相比,该方法灵敏度高、稳定性好,提高了检测效率,可实现饮用水中17种痕量全氟化合物从源头到龙头的全流程高效准确检测。

A method for determination of 17 perfluorinated compounds(PFCs)in drinking water and source water was established based on solid phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The water sample was extracted by WAX solid phase extraction(SPE)column and determined by UPLC-MS/MS.The separation was performed on a Cortecs C18 column with mobile phases of water containing 2 mmol/L ammonium acetate and methanol/acetonitrile(80∶20),and PFCs were analyzed by using multiple reaction monitoring(MRM)mode,negative electrospray ionization and negative ion scanning.Background interference was eliminated in the whole process of sampling,sample pre-treatment and detection through optimization of the pipe material and trap column.The linear correlation coefficients(R2)of 17 PFC standard curves were all greater than 0.99,and the limits of quantification ranged from 0.083 ng/L to 1.56 ng/L.When adding standard solutions of 4different concentrations,the recoveries of drinking water(product water and pipe water)were 65.0%-117.8% and the relative standard deviations(RSD)were 0.13%-17.93%.The recoveries of source water were 67.0%-117.8%,and the RSD were 0.60%-18.71%.Compared with 11 PFCs detection methods proposed in the national standard,this method has the advantages of high sensitivity,good stability and high detection efficiency,which can detect 17 trace PFCs in drinking water from source to tap.