固相萃取-液质联用法测定废水中的PFOS和PFOA  

Determination of PFOA and PFOS in Waste Water Using SPE-HPLC-MS/MS Method

作　　者：陈燕 李康柏 廖敏立 许嘉宁 邹琴 

机构地区：[1]广东省工程技术研究所广东省绿色产品认证检测中心,广东广州510440

出　　处：《广东化工》2016年第9期223-224,共2页Guangdong Chemical Industry

基　　金：广东省省级科技计划项目(2014B070705008)

摘　　要：建立了固相萃取-HPLC-MS/MS同时测定工业废水中PFOS和PFOA的方法。水样经过WAX小柱富集和净化后,采用5 mmol/L乙酸铵水溶液和甲醇作为流动相进行洗脱,质谱采用多反应监测模式,外标法定量分析。两种PFCs在1.0~45μg/L范围内线新关系良好,相关系数大于0.99,PFOS、PFOA的方法检出限和定量限分别为0.5、0.2 ng/L和2.0 ng/L、1.2 ng/L,回收率可高达70%~101%。应用本法分析某高新区内6家纺织皮革类企业的处理后废水中的PFOS和PFOA含量,测得两种全氟化合物的浓度在0.54~5.24μg/L之间。A solid phase extraction（SPE） high performance liquid chromatography（HPLC） method coupled with triplequard spectrometry was developed for the determination of PFOA and PFOS in waste water. Water sample was concentrated and purified through WAX column, and then separated by methonal 5 mmol/L ammonium acetate as the mobile phases. Two PFCs were quantified by external standard in multiple-reaction monitoring mode. The calibration curve of two PFCs were linear in the range of 1.0~45 μg/L with the correlation coefficients〉0.99. The limit of detection and quantitation of the method were 0.2, 0.5 ng/L and 1.2, 2.0 ng/L by the sequence of PFOA, PFOS, respectively. The recoveries were between 70 %~101 %.Our method was applied in the determination of PFOA and PFOS in six real samples which collected in one hi-tech development zone, the result were between 0.54 μg/L^5.24 μg/L.

关 键 词：固相萃取 液质联用 PFOS PFOA 工业废水 

分 类 号：O65[理学—分析化学]