混合無機酸消解-固相萃取-高效液相色譜-串聯質譜法分析貝類殼體中的3種全氟磺酸化合物

楊 錦, 汪 磊, 陳 晨, 張 姣, 孫紅文

(環境污染過程與基準教育部重點實驗室(南開大學),天津300071)

混合無機酸消解-固相萃取-高效液相色譜-串聯質譜法分析貝類殼體中的3種全氟磺酸化合物

楊 錦, 汪 磊＊, 陳 晨, 張 姣, 孫紅文

(環境污染過程與基準教育部重點實驗室(南開大學),天津300071)

建立了采用混合無機酸消解-固相萃取(SPE)-高效液相色譜-電噴霧電離串聯質譜(HPLC-ESI-MS/MS)分析貝類殼體中的3種全氟磺酸化合物的方法。將貝殼粉經硝酸/鹽酸混合酸消解,用氫氧化鈉調節消解液的pH值至6后采用Oasis WAX固相萃取柱富集凈化,然后采用內標法通過HPLC-ESI-MS/MS在分時段選擇反應監測模式下分析上述全氟磺酸化合物。結果表明,該方法對于貝殼中全氟丁烷磺酸、全氟己烷磺酸和全氟辛烷磺酸的檢出限(LOD)分別為0.28,0.42和0.43ng/g,加標回收率為94.88%～96.24%。采用此方法對渤海灣兩種雙殼貝類殼體進行的采樣分析也表明,貝殼中3種目標污染物的含量范圍為

混合酸消解;固相萃取;高效液相色譜-串聯質譜;全氟磺酸;貝類殼體

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)為代表的全氟磺酸類化合物是全氟化合物中的一類重要物質,它們被廣泛應用于紡織、造紙、包裝、農藥、地毯、皮革、裝潢、聚合物添加劑、表面活性劑及滅火泡沫等民用和工業產品生產領域[1]。含全氟磺酸化合物產品的大量使用使其以各種途徑進入全球范圍內的各種環境介質,尤其是水體中[2]。該類物質由于具有表面活性劑性質,含有水溶性官能團,在水中的溶解度大(如PFOS為570m g/L),因此能在水體中大量長期存在,造成海水、地下水和飲用水水源污染[3]。……