自制萃取头用于SPME-HPLC联用测定环境水样中的多环芳烃

摘要

采用原位聚合法在石英毛细管内制备了甲基丙烯酸-己二醇二甲基丙烯酸酯（MAA-EDMA）纤维作为固相微萃取（SPME）的萃取头,与高效液相色谱联用测定了环境水样中的多环芳烃.系统考察了萃取时间、解吸时间、盐浓度等实验条件对萃取效率的影响,建立了测定环境水样中的多环芳烃的SPME-HPLC方法.实验结果表明：方法的柱内（n=6）和柱间（n=6）精密度（RSD）分别小于4.45%和5.97%,实际样品的加标回收率在100.8%~108.9%之间；3种多环芳烃化合物的线性范围为10~4000μg/L,线性相关系数R2＞0.9496,检出限在1.008μg/L~2.876μg/L之间.所制备的Poly（MAA-EDMA）萃取头操作简便、稳定性好、成本低；方法快速、灵敏,适于测定环境水样中的多环芳烃.%An in-situ polymerization method was used in the preparation of a novel solid-phase microextraction (SPME) fiber,where methacrylic acid-ethylene glycol dimethacrylate (MAA-EDMA) was directly polymerization in fused silica capillary.Coupled to high performance liquid chromatography (HPLC),the prepared fiber was applied to the extraction and determination of polycyclic aromatic hydrocarbons (PAHs) in environmental waters.The experimental conditions of SPME,such as extraction time,desorption time and salt concentration were optimized.As a result,the run-to-run (n=6) and fiber-to-fiber (n=6) relative standard deviations of this method were lower than 4.45% and 5.97%,respectively;and the recoveries of PAHs were in the range of 100.8%~108.9%; the linear relationships between the concentration 10 μg/L and 4 000 μg/L for PAHs were obtained (R2>0.949 6);the limits of detection ranged from 1.008 μg/L to 2.876 μg/L in the optimal conditions.The prepared Poly(MAA-EDMA) fiber possesses some advantages including simplicity,good stability and low cost.The method was fast, sensitive,and suitable for the determination of PAHs in environmental waters.