Clossed-vessel assisted microwave extraction of polychlorinated biphenyls in marine mussels

被引:13
作者
Carro, N
García, I
Llompart, M
机构
[1] Ctr Control Calidad Medio Marino, Vilagarcia de Arousa 36611, Pontevedra, Spain
[2] Fac Quim, Dept Quim Analit Nutr & Bromatol, Santiago De Compostela 15706, Spain
关键词
Microwave Assisted Solvent Extraction (MASE) polychlorinated biphenyls (PCBs); sample preparation; gas chromatography-electron capture detector marine mussels;
D O I
10.1051/analusis:2000142
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A reliable and simple procedure to extract polychlorinated biphenyls (PCBs) from marine mussels using microwave energy is proposed. Freeze-dried mussels were subjected to MASE (Microwave Assisted Solvent Extraction) in a closed-vessel microwave system with n-pentane-sodium hydroxide (5 %) or dichloromethane-pentane (1:1) at different temperatures (70 and 90 degreesC), the extraction time was 10 minutes. Sample extract cleanup procedure was performed by using alumina. Gas chromatography-mass spectrometry and gas chromatography-electron capture detector were employed for individual congener identification and determination. The influence of the following variables on microwave extraction of PCBs has been studied: extraction temperature,, solvent volume, solvent nature, cleanup procedure time and volume of sodium hydroxide solution. Recoveries for PCBs were between 77 and 106 % with relative standard deviation between 2 to 20 %. Validation of the extraction process was carried out by processing a certified reference material. Microwave Assisted Solvent Extraction was compared to Soxhlet extraction.
引用
收藏
页码:720 / 724
页数:5
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