Cai Mei-Qiang, Su Jie, Hu Jian-Qiang, Wang Qian, Dong Chun-Ying, Pan Sheng-Dong, Jin Mi-Cong
School of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310018, China.
School of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310018, China.
J Chromatogr A. 2016 Aug 12;1459:38-46. doi: 10.1016/j.chroma.2016.06.086. Epub 2016 Jul 1.
A planar graphene oxide-based magnetic ionic liquid nanomaterial (PGO-MILN) was synthesized. The prepared PGO-MILN was characterized by transmission electronmicroscopy (TEM) and Fourier-transform infrared spectrometry (FTIR). The results of adsorption experiments showed that the PGO-MILN had great adsorption capacity for 2-chlorophenol (2-CP), 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP) and pentachlorophenol (PCP). Based on the adsorption experimental data, a sensitive magnetic method for determination of the five CPs in environmental water samples was developed by an effective magnetic solid-phase extraction (MSPE) procedure coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The effects of main MSPE parameters including the solution pH, extraction time, desorption time, and volume of desorption solution on the extraction efficiencies had been investigated in detail. The recoveries ranged from 85.3 to 99.3% with correlation coefficients (r) higher than 0.9994 and the linear ranges were between 10 and 500ngL(-1). The limits of detection (LODs) and limits of quantification (LOQs) of the five CPs ranged from 0.2 to 2.6ngL(-1) and 0.6 to 8.7ngL(-1), respectively. The intra- and inter- day relative standard deviations (RSDs) were in the range from 0.6% to 7.4% and from 0.7% to 8.4%, respectively. It was confirmed that the PGO-MILN was a kind of highly effective MSPE materials used for enrichment of trace CPs in the environmental water.
合成了一种基于平面氧化石墨烯的磁性离子液体纳米材料(PGO-MILN)。采用透射电子显微镜(TEM)和傅里叶变换红外光谱(FTIR)对制备的PGO-MILN进行了表征。吸附实验结果表明,PGO-MILN对2-氯苯酚(2-CP)、2,4-二氯苯酚(2,4-DCP)、2,4,6-三氯苯酚(2,4,6-TCP)、2,3,4,6-四氯苯酚(2,3,4,6-TeCP)和五氯苯酚(PCP)具有较大的吸附容量。基于吸附实验数据,通过有效的磁性固相萃取(MSPE)程序结合高效液相色谱-串联质谱(LC-MS/MS),建立了一种灵敏的磁性方法用于测定环境水样中的五种氯酚。详细研究了主要MSPE参数,包括溶液pH值、萃取时间、解吸时间和解吸溶液体积对萃取效率的影响。回收率在85.3%至99.3%之间,相关系数(r)高于0.9994,线性范围在10至500ngL(-1)之间。五种氯酚的检测限(LOD)和定量限(LOQ)分别为0.2至2.6ngL(-1)和0.6至8.7ngL(-1)。日内和日间相对标准偏差(RSD)分别在0.6%至7.4%和0.7%至8.4%范围内。证实了PGO-MILN是一种用于富集环境水中痕量氯酚的高效MSPE材料。