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| Determination of 19 Polychlorinated Biphenyls in Environmental Sludge Samples by Microwave-assisted Micro-solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry |
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| DOI： |
| KeyWord:microwave-assisted micro-solid phase extraction gas chromatography-mass spectrometry（GC-MS） polychlorinated biphenyls(PCBs) environmental analysis sludge |
| Author | Institution |
| ZHANG Yan,JIANG Zhi-bin，JIAO Zhe*,L? Si-hao，FAN Hong-bo，HUANG Wei-qing |
东莞理工学院化学与环境工程学院 |
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| Abstract: |
| A microwave assisted micro-solid phase extraction（MAE-μ-SPE） combined with gas chromatography-mass spectrometric（GC-MS） method was developed for the determination of 19 polychlorinated biphenyls（PCBs） in environmental sludge sample.Target PCBs compounds were extracted from the sludge sample into extraction solvent enhanced by microwave field,followed by adsorption with adsorbent in the micro-solid phase extraction device.The copper（Ⅱ） isonicotinate（Cu（4-C5H4N-COO）2（H2O）4） coordination polymer was prepared and used as the adsorbent.Variables affecting extraction procedures were systematically investigated,and the experimental conditions of MAE-μ-SPE were optimized.The major optimized parameters were as follows:extraction temperature:60 ℃,extraction time:25 min,desorption time:25 min,desorption solvent:150 μL ethyl acetate.Then,a GC-MS method for determination of 19 PCBs was studied.The detection limits（S/N=3） of the method ranged from 0.2 ng/g to 2.5 ng/g,and the relative standard deviations（RSD） were lower than 14%.The mean recoveries were in the range of 81.4%-102.1%.The experimental results demonstrated that the developed MAE-μ-SPE/GC-MS method combining extraction,cleanup,and concentration in one step,was suitable for analysis of trace PCBs in complex samples. |
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