Evaluation of a Microwave-Assisted Extraction Technique for the Determination of Polychlorinated Biphenyls and Organochlorine Pesticides in Sediments

Abstract The efficiency of microwave-assisted extraction (MAE) was evaluated for the analysis of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in fish. An isotope dilution method was used for quantification via analysis of the samples by gas chromatography and mass spectrometry. MAE solvent, temperature, and time were optimized, and observed concentrations were compared. The MAE results were also compared to those of other extraction techniques (Soxhlet extraction, pressurized liquid extraction, saponification, and homogenization). Concentrations of PCBs and OCPs obtained by MAE at 120C for 10 min were comparable to those by the other techniques. The results suggest that MAE can be used for the analysis of PCBs and OCPs in fish.

Download Full-text

Pressurized Liquid Extraction and Microwave-Assisted Extraction in the Determination of Organochlorine Pesticides in Fish Muscle Samples

Journal of AOAC International ◽

10.1093/jaoac/91.1.174 ◽

2008 ◽

Vol 91 (1) ◽

pp. 174-180 ◽

Cited By ~ 1

Author(s):

Mercedes Barriada-Pereira ◽

Iván Iglesias-García ◽

María J Gonzlez-Castro ◽

Soledad Muniategui-Lorenzo ◽

Purificación López-Maha ◽

...

Keyword(s):

Organochlorine Pesticides ◽

Fish Muscle ◽

Extraction Methods ◽

Liquid Extraction ◽

Pressurized Liquid Extraction ◽

Microwave Assisted Extraction ◽

Microwave Assisted ◽

Assisted Extraction ◽

Relative Standard

Abstract This paper describes a comparative study of 2 extraction methods, pressurized liquid extraction (PLE) and microwave-assisted extraction (MAE), for the determination of organochlorine pesticides (OCPs) in fish muscle samples. In both cases, samples were extracted with hexaneacetone (50 + 50), and the extracts were purified by solid-phase extraction using a carbon cartridge as the adsorbent. Pesticides were eluted with hexaneethyl acetate (80 + 20) and determined by gas chromatography with electron-capture detection. Both methods demonstrated good linearity over the range studied (0.0050.100 g/mL). Detection limits ranged from 0.029 to 0.295 mg/kg for PLE and from 0.003 to 0.054 mg/kg for MAE. For most of the pesticides, analytical recoveries with both methods were between 80 and 120, and the relative standard deviations were <10. The proposed methods were shown to be powerful techniques for the extraction of OCPs from fish muscle samples. Although good recovery rates were obtained with both extraction methods, MAE provided advantages with regard to sample handling, cost, analysis time, and solvent consumption. Acceptable validation parameters were obtained although MAE was shown to be more sensitive than PLE.

Download Full-text

Development of a Microwave-Assisted Extraction Method for the Determination of Organochlorine Pesticides in Mussel Tissue

Food Analytical Methods ◽

10.1007/s12161-013-9744-z ◽

2013 ◽

Vol 7 (6) ◽

pp. 1271-1277 ◽

Cited By ~ 7

Author(s):

Emmanouil-Nikolaos Papadakis ◽

Archontoula Kyrgidou ◽

Zisis Vryzas ◽

Euphemia Papadopoulou-Mourkidou

Keyword(s):

Organochlorine Pesticides ◽

Extraction Method ◽

Microwave Assisted Extraction ◽

Mussel Tissue ◽

Microwave Assisted ◽

Assisted Extraction

Download Full-text

Rapid Method for the Determination of Organochlorine Pesticides and PCBs in Fish Muscle Samples by Microwave-Assisted Extraction and Analysis of Extracts by GC-ECD

Journal of AOAC International ◽

10.1093/jaoac/93.6.1987 ◽

2010 ◽

Vol 93 (6) ◽

pp. 1987-1994 ◽

Cited By ~ 8

Author(s):

Angelika M Wilkowska ◽

Marek Biziuk

Keyword(s):

Organochlorine Pesticides ◽

Fish Muscle ◽

Food Samples ◽

Fat Content ◽

Clupea Harengus ◽

Microwave Assisted Extraction ◽

Extraction Solvent ◽

Microwave Assisted ◽

Assisted Extraction

Abstract A procedure for the multiresidue determination of organochlorine pesticides and polychlorinated biphenyls in fish muscle samples has been developed. The method is based on the microwave-assisted extraction (MAE) of food samples from an acetonitrilewater (95 5, v/v) mixture followed by SPE cleanup of the extracts and analysis by GC with an electron capture detector. MAE operational parameters, such as the extraction solvent, temperature, and time, were optimized with respect to the extraction efficiency of the target compounds from food samples with 1013 fat content. The chosen extraction technique allows reduction of the solvent consumption and extraction time when compared with methods already used. Acetonitrile is a good extraction solvent for low-fat matrixes (220 fat content), such as fish samples, because it does not significantly dissolve the highly polar proteins, salts, and sugars commonly found in food and gives high recoveries of a wide polarity range of analytes. For purification, SPE using LC-Florisil was shown to be sufficient for the removal of coextracted substances. Recoveries >78 with RSD values <15 were obtained for all compounds under the selected conditions. Method quantification limits were in the 510 g/kg range. The method was applied to the analysis of samples of herring (Clupea harengus) purchased at the local fish market. The method is rapid and reliable for the determination of organochlorine analytes in fish muscle.

Download Full-text