Analysis of Organochlorine Pesticides in Soil Using Optimized FMAE-GC/MS

2012 ◽  
Vol 518-523 ◽  
pp. 2348-2351
Author(s):  
Shan Shan He ◽  
Yu Jun Wang ◽  
Ling Cao ◽  
Yan Xin Wang ◽  
Chuang Ju Dong
Keyword(s):  
Organochlorine Pesticides ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Microwave Assisted Extraction ◽  
Good Recovery ◽  
Extraction Solvent ◽  
Microwave Assisted ◽  
Assisted Extraction ◽  
Relative Standard

A focused microwave-assisted extraction (FMAE) was optimized and coupled to gas chromatography–mass spectrometry for the determination of organochlorine pesticides in soil samples. According to the result, the combination of 20 min extraction time at 48 °C and a mixture of 1+1 of n-hexane-acetone as extraction solvent is the best conditions. The recovery values is 72.8%～96.4% in the above conditions. The relative standard deviation was 4.39%~13.18%. We have good recovery values when spiked 20ng, 40ng and 60ng standard into 5.00g soil sample.

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

2008 ◽  
Vol 91 (1) ◽  
pp. 174-180 ◽  
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.

scholarly journals 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

2010 ◽  
Vol 93 (6) ◽  
pp. 1987-1994 ◽  
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.

Determination of organophosphate ester flame retardants and plasticizers in soil samples by microwave-assisted extraction coupled with silica gel/alumina multilayer solid-phase extraction and gas chromatography-mass spectrometry

2017 ◽  
Vol 9 (6) ◽  
pp. 986-993 ◽  
Author(s):  
Kunyan Cui ◽  
Jiaxin Wen ◽  
Feng Zeng ◽  
Xi Zhou ◽  
Shoucong Li ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Flame Retardants ◽  
Solid Phase ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Microwave Assisted Extraction ◽  
Microwave Assisted ◽  
Assisted Extraction

The performances of commonly used solid phase extraction materials for separating organophosphate esters from potential co-extracted interferents were evaluated.

Determination of organochlorine pesticides in horticultural samples by microwave assisted extraction followed by GC-ECD

2005 ◽  
Vol 85 (4-5) ◽  
pp. 325-333 ◽  
Author(s):  
Mercedes Barriada-Pereira ◽  
María José González-Castro ◽  
Soledad Muniategui-Lorenzo ◽  
Purificación López-Mahía ◽  
Darío Prada-Rodríguez ◽  
...  
Keyword(s):  
Organochlorine Pesticides ◽  
Microwave Assisted Extraction ◽  
Microwave Assisted ◽  
Assisted Extraction

scholarly journals Determination of trans fatty acids in foodstuffs by gas chromatography-mass spectrometry after simultaneous microwave-assisted extraction-esterification

2010 ◽  
Vol 75 (6) ◽  
pp. 803-812 ◽  
Author(s):  
Snezana Kravic ◽  
Zvonimir Suturovic ◽  
Jaroslava Svarc-Gajic ◽  
Zorica Stojanovic ◽  
Mira Pucarevic
Keyword(s):  
Mass Spectrometry ◽  
Sample Preparation ◽  
Preparation Method ◽  
Reference Method ◽  
Gas Chromatography Mass Spectrometry ◽  
Microwave Assisted Extraction ◽  
Sample Preparation Method ◽  
Microwave Assisted ◽  
Assisted Extraction

A sample preparation method based on the simultaneous microwave-assisted extraction-esterification (SMAEE) was developed for the determination of the fatty acid composition of foodstuffs by gas chromatography-mass spectrometry. The proposed sample preparation method was validated by comparison with the reference Soxhlet extraction method followed by derivatisation by ester formation and the same determination step. The fatty acid compositions and the extraction efficiencies obtained using the proposed SMAEE method and the reference method were statistically similar. The results showed that compared to the conventional method, the SMAEE method offered the advantages of short sample preparation time, low consumption of expensive organic solvents and lower energy consumption. This good agreement between results provided by both the SMAEE and the reference method demonstrates the usefulness of the former as a routine method for the treatment of food samples prior to trans fatty analysis.

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