杨 锦, 汪 磊, 陈 晨, 张 姣, 孙红文

(环境污染过程与基准教育部重点实验室(南开大学),天津300071)

混合无机酸消解-固相萃取-高效液相色谱-串联质谱法分析贝类壳体中的3种全氟磺酸化合物

杨 锦, 汪 磊＊, 陈 晨, 张 姣, 孙红文

(环境污染过程与基准教育部重点实验室(南开大学),天津300071)

建立了采用混合无机酸消解-固相萃取(SPE)-高效液相色谱-电喷雾电离串联质谱(HPLC-ESI-MS/MS)分析贝类壳体中的3种全氟磺酸化合物的方法。将贝壳粉经硝酸/盐酸混合酸消解,用氢氧化钠调节消解液的pH值至6后采用Oasis WAX固相萃取柱富集净化,然后采用内标法通过HPLC-ESI-MS/MS在分时段选择反应监测模式下分析上述全氟磺酸化合物。结果表明,该方法对于贝壳中全氟丁烷磺酸、全氟己烷磺酸和全氟辛烷磺酸的检出限(LOD)分别为0.28,0.42和0.43ng/g,加标回收率为94.88%～96.24%。采用此方法对渤海湾两种双壳贝类壳体进行的采样分析也表明,贝壳中3种目标污染物的含量范围为

混合酸消解;固相萃取;高效液相色谱-串联质谱;全氟磺酸;贝类壳体

Abstract:For the analysis of perfluorobutane sulfonate(PFBS),perfluorohexane sulfonate(PFHxS)and perfluorooctane sulfonate(PFOS)in shells,an extraction method of mixed inorganic acid digestion coup led with solid phase extraction(SPE)was established.The target com pounds were determ ined by high performance liquid Chromatography-tandem mass spectrometry(HPLC-MS/MS).The shell pow derwas at first digested with the mixture of nitric acid and hydrochloric acid,then the digestion solution was adjusted to pH6with sodium hydroxide,and cleaned up with Oasis WAX SPE cartridge.The perfluoro sulfonated Chemicals were quantified with HPLC-MS/MS using electrospray ionization in negativeionmode with internal standard method.The limits of detection(LOD s)were of0.28ng/g for PFBS,0.42ng/g for PFHxS and0.43ng/g for PFOS,and matrix recoveries of the perfluoro sulfonated Chemicals were 94.88%-96.24%.The analytical results for the shells of two bivalves from Bohai Bay show ed this p retreatment method is suitable for the determination of perfluoro sulfonated acids(PFSAs)in shells.Concentrations of PFSAs in the shells ranged from

Key words:mixed acid digestion;solid phase extraction(SPE);high performance liquid Chromatography-tandem mass spectrometry(HPLC-MS/MS);perfluoro sulfonated Chemicals;shells

以全氟辛烷磺酸(PFOS)为代表的全氟磺酸类化合物是全氟化合物中的一类重要物质,它们被广泛应用于纺织、造纸、包装、农药、地毯、皮革、装潢、聚合物添加剂、表面活性剂及灭火泡沫等民用和工业产品生产领域[1]。含全氟磺酸化合物产品的大量使用使其以各种途径进入全球范围内的各种环境介质,尤其是水体中[2]。该类物质由于具有表面活性剂性质,含有水溶性官能团,在水中的溶解度大(如PFOS为570m g/L),因此能在水体中大量长期存在,造成海水、地下水和饮用水水源污染[3]。……