加速溶剂萃取-气相色谱/气相色谱-质谱法测定土壤中7种多氯联苯
Determination of 7 Polychlorinated Biphenyls in Soil Samples by Accelerated Solvent Extraction-Gas Chromatography/ Gas Chromatography-Mass Spectrometry
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摘要: 建立了土壤样品中7种多氯联苯(PCB 28、PCB 52、PCB 101、PCB 118、PCB 138、PCB 153、PCB 180)的分析方法。土壤样品通过加速溶剂萃取、磺化法结合Florisil 固相萃取小柱净化、电子捕获检测器气相色谱分析测定,并结合气相色谱-质谱进一步确证。结果表明,方法回收率为80.06%~100.28%,相对标准偏差(RSD,n=6)为1.01%~6.28%,检出限为0.15~0.50 μg/kg。用优化的方法测定复杂基质的土壤样品中多氯联苯,具有提取效率高、净化效果好、结果准确可靠、对环境污染小等优点。Abstract: A method for the determination 7 polychlorinated biphenyls (PCB 28, PCB 52, PCB 101, PCB 118, PCB 138, PCB 153 and PCB 180) in soil samples was developed. Solid samples were pretreated with accelerated solvent extraction and purified with sulfonation combining with Florisil solid phase extraction (SPE) and the concentrations of PCBs in soil samples were quantified by gas chromatograph with electron capture detector (GC-ECD) and further confirmed by gas chromatography-mass spectrometry (GC-MS). The detection limits of method (LMD) for PCBs were 0.15~0.50 μg/kg and the recoveries were 80.06%~100.28% with the precisions of 1.01%~6.28% RSD. The method has been applied to the determination of PCBs in complex matrix soil sample with characters of high efficiency, good purification effect, high precision and accuracy and environment friendly.
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Keywords:
- polychlorinated /
- biphenyls /
- soil /
- gas /
- chromatography /
- gas
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