固相微革取-气相色谱-质谱联用测定海水与沉积物中邻苯二甲酸酯类污染物

邻苯二甲酸酯(PAEs)是塑化剂产品中使用最广泛的一类化合物,准确分析海洋中邻苯二甲酸酯的种类、组成及浓度水平,对认识PAEs在海洋环境的迁移变化及生态效应具有重要意义.本研究建立了固相微萃取-气相色谱-质谱联用技术分析海水与沉积物中PAEs的方法,确定了萃取时间、萃取温度等最佳实验条件.本方法测定海水与沉积物中PAEs含量的精密度为±10%,检出限分别为0.04~0.32 ng/L和0.12~1.60μg/kg;除邻苯二甲酸二甲酯(DMP)外,海水中PAEs回收率为68.0%~114.0%,沉积物中PAEs回收率为76.4%~105.0%.利用本方法测得长江口及其邻近海域水体与沉积物中PAEs的浓度分别为0.270~1.39μg/L和0.79~34.8μg/kg.实验表明,本方法操作简单,准确度高,大大缩减了海水萃取体积,能够应用于近岸海水与沉积物中PAEs含量的准确分析.

Determination of Phthalic Acid Esters in Seawater and Sediment by Solid-phase Microextraction and Gas Chromatography-Mass Spectrometry

Phthalic acid esters ( PAEs) are one class of the most important plasticizers which are widely used in the production of plastic products. The accurate analysis of PAEs in seawater and sediment would be of great significance to study the transformation of PAEs and their ecological effects in marine environment. In this study, the method of gas chromatography with mass spectrum detector ( GC-MSD) coupled with solid-phase microextraction had been established to analyze the concentration of PAEs in seawater and sediment, and various experimental conditions such as extraction time and extraction temperature were optimized. Under the optimum conditions, the precision was less than 10. 0%, and the limits of detection were 0. 04-0. 32 μg/L and 0. 12-1. 60μg/kg. Except dimethyl phthalate (DMP), the recovery of PAEs in seawater and sediment ranged from 68. 0% to 114. 0% and 76. 4% to 105. 0%, respectively. Moreover, the concentrations of PAEs measured with the method were 0 . 270-1 . 39 μg/L and 0 . 74-34 . 8 μg/kg in seawater and sediment samples of Changjiang River Estuary and its adjacent area, respectively. In conclusion, the analytical method is easy to operate and reduces the extraction volume of seawater water, thus it meets the requirements of the analysis of PAEs in coastal seawater and sediment.