花生壳活性炭固相萃取/超高效液相色谱法测定河水中的18种多环芳烃  

Determination of Trace Polycyclic Aromatic Hydrocarbons by Solid Phase Extraction Coupled with Ultra-high Performance Liquid Chromatography

作　　者：项小燕[1,2] 林锡煌[3] 何立芳[1] 胡志彪[1] 林金清[2] 

机构地区：[1]龙岩学院化学与材料工程学院,福建龙岩364000 [2]华侨大学材料科学与工程学院,福建厦门361021 [3]国家海洋局第三海洋研究所,福建厦门361005

出　　处：《分析测试学报》2017年第1期96-100,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(21246008);福建省自然科学基金项目(2016J01060);福建省教育厅B类项目(JB14096)

摘　　要：建立了固相萃取/超高效液相色谱-二极管阵列检测(SPE/UPLC-PDA)联用技术测定河水中18种痕量多环芳烃(PAHs)的快速分析方法。通过优化固相萃取条件、流动相体系、色谱条件等因素,7 min内实现了18种多环芳烃的高效分离。在0.05~50 mg/L浓度范围内,18种多环芳烃的浓度与对应峰面积呈良好线性关系,相关系数为0.999 1~0.999 9,检出限为0.08~2.03 ng/L,样品加标回收率为74.5%~103.6%,相对标准偏差(RSD,n=6)为0.5%~2.3%。将该方法应用于九龙江流域龙岩段周边水样的检测,结果可靠。该方法简单环保、灵敏准确、操作快速,可显著提高河水中痕量PAHs的分析效率。A novel method for the simultaneous determination of 18 PAHs in river was established by solid-phase extraction coupled with ultra-high performance liquid chromatography（SPE/UPLC）.The effects of solid phase,elution system and gradient elution were optimized.Under the optimal conditions,18 PAHs could be separated in 7 min.The calibration curves of 18 PAHs showed good linearity between peak area and concentration in the range of 0.05-50 mg/L,with correlation coefficients of 0.999 1-0.999 9.The detection limits were between 0.08 ng/L and 2.03 ng/L,with relative standard deviations（RSDs） of 0.5%-2.3%.The spiked recoveries were in the range of 74.5%-103.6%.It provided a reliable method for the study of PAHs in the Longyan section of Nine Longjiang River Basin.The method is simple,sensitive,accurate and efficient,and could significantly improve the analysis efficiency of trace PAHs in rivers.

关 键 词：花生壳活性炭 固相萃取 多环芳烃 超高效液相色谱法 

分 类 号：O657.72[理学—分析化学] O625.15[理学—化学]