scholarly journals Development of a Microwave-Assisted Extraction Protocol for the Simultaneous Determination of Mycotoxins and Pesticide Residues in Apples by LC-MS/MS

2021 ◽  
Vol 11 (22) ◽  
pp. 10931
Author(s):  
Natasa P. Kalogiouri ◽  
Emmanouil-Nikolaos Papadakis ◽  
Maria G. Maggalou ◽  
George S. Karaoglanidis ◽  
Victoria F. Samanidou ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Simultaneous Determination ◽  
Pesticide Residues ◽  
Matrix Effects ◽  
Critical Issue ◽  
Microwave Assisted Extraction ◽  
Extraction Solvent ◽  
Microwave Assisted ◽  
Assisted Extraction

The possible presence of contaminants, pesticide residues and mycotoxins, in agricultural commodities is a critical issue for food safety, causing great concern. In this work, a simple and rapid analytical method employing liquid chromatography–tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous determination of pesticide residues and mycotoxins in apples. Microwave-assisted extraction (MAE) was used for sample preparation. The MAE protocol was optimized after evaluating the effects of the following extraction parameters: (a) extraction solvent, (b) acidic environment, (c) temperature, and (d) extraction time. The multiresidue MAE-LC-MS/MS method was validated for linearity, accuracy (bias and precision), limits of detection (LODs), limits of quantification (LOQs), and matrix effect. The validation of the method was carried out according to the SANTE/12682/2019 document. The method demonstrated good linearity with R2 ≥ 0.99, acceptable accuracy in the recovery rate range 70–116%, acceptable interassay precision with RSD% ≤ 20, and low LODs and LOQs in the ranges 0.005–0.015 μg/g and 0.01–0.03 μg/g, respectively. Matrix effects were observed only for the 25% of the analytes. The performance of the MAE-LC-MS/MS method was compared to that of the QuEChERS sample preparation method, and the MAE-LC-MS/MS method proved to be rapid and effective.

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.

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.

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