Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
J Chromatogr A. 2013 Jul 26;1300:165-72. doi: 10.1016/j.chroma.2013.05.004. Epub 2013 May 13.
In this work, amino modified multi-walled carbon nanotubes/polydimethylsiloxane (multi-walled carbon nanotubes-4,4'-diaminodiphenylmethane/polydimethylsiloxane, MWCNTs-DDM/PDMS) was synthesized, and utilized as a novel coating for stir bar sorptive extraction (SBSE) of seven phenols (phenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, 2,4-dimethylphenol, p-choro-m-cresol and 2,4,6-trichlorphenol) in environmental water and soil samples, followed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The prepared MWCNTs-DDM/PDMS coated stir bar was characterized and good preparation reproducibility was obtained with the relative standard deviations (RSDs) ranging from 4.7% to 11.3% (n=9) in one batch, and from 4.8% to 13.9% (n=8) among different batches. Several parameters affecting the extraction of seven target phenols by MWCNTs-DDM/PDMS-SBSE including extraction time, stirring rate, pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.14μg/L (2-nitrophenol) to 1.76μg/L (phenol) and the limits of quantification (LOQs, S/N=10) were found to be in the range of 0.46μg/L (2-nitrophenol) to 5.8μg/L (phenol). The linear range was 5-1000μg/L for phenol and 4-nitrophenol, 1-1000μg/L for 2-nitrophenol and 2-1000μg/L for other phenols, respectively. The RSDs of the developed method were in the range of 6.2-11.6% (n=8, c=10μg/L) and the enrichment factors were from 6.5 to 62.8-fold (theoretical enrichment factor was 100-fold). The proposed method was successfully applied to the analysis of phenols in environmental water and soil samples, and good recoveries were obtained for the spiked samples. The proposed method is simple, highly sensitive and suitable for the analysis of trace phenols in environmental samples with complex matrix.
在这项工作中，合成了氨基改性的多壁碳纳米管/聚二甲基硅氧烷（多壁碳纳米管-4,4'-二氨基二苯甲烷/聚二甲基硅氧烷，MWCNTs-DDM/PDMS），并将其用作新型搅拌棒吸附萃取（SBSE）的涂层，用于环境水样和土壤样品中七种酚类化合物（苯酚、2-氯苯酚、2-硝基苯酚、4-硝基苯酚、2,4-二甲基苯酚、对氯间甲酚和 2,4,6-三氯苯酚）的萃取，然后采用高效液相色谱-紫外检测（HPLC-UV）进行分析。制备的 MWCNTs-DDM/PDMS 涂层搅拌棒进行了表征，在一批次中，其制备重现性良好，相对标准偏差（RSD）范围为 4.7%至 11.3%（n=9），而在不同批次之间，RSD 范围为 4.8%至 13.9%（n=8）。研究了影响 MWCNTs-DDM/PDMS-SBSE 萃取七种目标酚类化合物的几个参数，包括萃取时间、搅拌速度、pH 值、离子强度、洗脱溶剂和洗脱时间。在最佳实验条件下，发现七种酚类化合物的检测限（LOD，S/N=3）范围为 0.14μg/L（2-硝基苯酚）至 1.76μg/L（苯酚），定量限（LOQ，S/N=10）范围为 0.46μg/L（2-硝基苯酚）至 5.8μg/L（苯酚）。苯酚和 4-硝基苯酚的线性范围为 5-1000μg/L，2-硝基苯酚的线性范围为 1-1000μg/L，而其他酚类化合物的线性范围为 2-1000μg/L。该方法的 RSD 范围为 6.2-11.6%（n=8，c=10μg/L），富集因子为 6.5 至 62.8 倍（理论富集因子为 100 倍）。该方法成功应用于环境水样和土壤样品中酚类化合物的分析，对加标样品的回收率良好。该方法简单、灵敏度高，适用于分析复杂基质环境样品中的痕量酚类化合物。
