磁性多壁碳纳米管固相萃取-气相色谱-质谱法检测水样中的13种邻苯二甲酸酯类化合物

摘要

A method based on solid phase extraction (SPE) with magnetic multi-walled carbon nanotubes (MWCNTs) as adsorbent was developed for the determination of 13 phthalate acid esters (PAEs) in water samples by gas chromatography-mass spectrometry (GC-MS). The factors affecting the extraction efficiency, such as extraction time, pH of water sample, desorp-tion solvent, and desorption time, were carefully investigated. The optimized conditions were as follows: extraction time, 10 min; pH of water samples, 5 - 7 ; desorption solvent, 2 mL acetone; desorption time, 5 min. The extraction efficiencies were 89. 7% - 100. 5% under the optimized conditions. The method was sensitive with the detection limits (S/N = 3) between 0.08 - 0.47 μg/L for the 13 PAEs. The developed method was successfully applied for the analysis of tap water, bottle drinking water and lake water, and none of the 13 PAEs was detected. The recoveries ranged from 84. 5% to 107. 5% for the 3 real spiked samples, and the relative standard deviations were between 1.9% and 12. 8%. The developed method has proved convenient, time-saving, accurate, sensitive, and environmental-friendly, and can be used for the determination of PAEs in water samples.%建立了磁性多壁碳纳米管(MWCNTs)固相萃取结合气相色谱-质谱检测水样中13种邻苯二甲酸酯类化合物( PAEs)的方法.优化了萃取时间、水样pH值、解吸溶剂的种类和用量、解吸时间等影响萃取效率的主要条件.最终确定萃取时间为10 min,水样pH 5 ～7,解吸溶剂为2mL丙酮,解吸时间为5 min.在优化的条件下,各组分的萃取回收率为89.7％ ～100.5％.方法具有较高的灵敏度,检出限(信噪比(S/N)为3)为0.08～0.47 μg/L.3种实际样品的加标回收率为84.5％ ～107.5％,相对标准偏差为1.9％ ～12.8％.该方法操作简便、省时,准确、灵敏、环保,可用于水样中PAEs的检测,并成功地应用于自来水、瓶装饮用水和湖水样品的分析,13种PAEs均未检出.