衍生化固相微萃取与气相色谱-质谱联用测定生活垃圾渗沥液中双酚A

Determination of Bisphenol A in Landfill Leachate by Solid Phase Microextraction with Headspace Derivatization and Gas Chromatography-Mass Spectrometry

建立了固相微萃取-顶空衍生化与色谱-质谱联用技术测定水中双酚A定量分析方法.对影响萃取和衍生化过程的参数进行了条件优化,实验选用聚丙烯酸酯（PA）萃取纤维,在搅拌速度为1200 r/min、溶液离子强度100g/L、pH2和25℃的条件下萃取60min后,N,O双（三甲基硅烷基）三氟乙酰胺（BSTFA）顶空衍生化5 min.方法的线性范围是0.09～200 μg/L;检出限0.03μg/L;相对标准偏差为3.88%.应用本方法对广州大田山垃圾填埋场的垃圾渗沥液中的双酚A进行了测定.

A method of headspace derivatization solid phase microextraction （SPME） coupled with gas chromatography-mass spectrometry （GC-MS） for determination of bisphenol A （BPA） in landfill leachate has been developed. Using 85-μm polyacrylate （PA） fibers,the influence of several parameters on the SPME and derivatization procedure like the extraction time of the fiber in the aqueous sample, derivatization time and temperature, the desorption time and temperature, pH value as well as salt content of the sample have been studied. The derivatization was carried out at room temperature without damaging the fiber coating. A linear response of silylated BPA compounds over a concentration range from 0. 09 to 200μg/L, the detection limit of 0. 03μg/L （3 s criteria） were obtained. The proposed method has been applied for the determination of BPA in landfill leachate.