Volume 28, Number 8, October 2000Luminescence spectroscopy: applications and recent trends
|Page(s)||720 - 724|
Clossed-vessel assisted microwave extraction of polychlorinated biphenyls in marine musselsN. Carro1, I. García1 and M. Llompart2
1 Centro de Control de Calidad del Medio Marino, Peirao de Vilaxoán s/n. 36611, Vilagarcía de Arousa, Pontevedra, Spain
2 Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Química, Avda das Ciencias s/n. 15706, Santiago Compostela, Spain
(Received January 13, 2000; revised September 13; accepted September 19, 2000.)
Abstract. 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 °C), 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.
Key words: Microwave Assisted Solvent Extraction (MASE) -- polychlorinated biphenyls (PCBs) -- sample preparation -- gas chromatography-electron capture detector -- marine mussels.
© EDP Sciences, Wiley-VCH 2000