Pesticide Residues
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Nasra M. Abd El-Mageed ◽  
Ideisan I. Abu-Abdoun ◽  
Kaltham A. H. Kayaf ◽  
Abdulla S. Janaan

The occurrence of pesticide residues in representative samples collected from imported dates palm fruits during 2020 to United Arab Emirates (UAE) was investigated to ensure compliance with the standard specifications and requirements by the regulatory and supervisory authorities, maintain the health and safety of consumers and improve food safety. An accurate, rapid, and reliable method for the simultaneous determination of pesticide multi-residues in 230 samples imported dates by liquid chromatography coupled with tandem mass spectrometry (LC–ESI (+)-MS/MS) operating in multiple reaction monitoring (MRM) mode and modified quick, easy, cheap, effective, rugged, safe (QuEChERS) method was used. The performance of the analytical method was validated in accordance with EU SANCO guidelines (SANTE/12682/2019) for monitoring pesticide multi-residues to check compliance with existing regulations, especially for European Community. Residues level of 343 compounds were determined in 230 samples. Results indicated that the percentage of samples with residues above the maximum residue levels (MRL) was 4.34% in dates samples, whereas samples with residues within MRL were 7.39% in dates samples. A total of 230 samples of 88.26% were free from detectable residues. Out of the 343 pesticides tested, 11 pesticides were found above the limit of detection, according to UAE, Codex, and European regulations. The main purpose of this work is to inform citizens and traders who have concerns about food safety on the capability of the MOCCAE on quality assurance regarding pesticide residue in imported food.

R. Kaur ◽  
D. Singh ◽  
A. Kumari ◽  
G. Sharma ◽  
S. Rajput ◽  

2021 ◽  
Vol 11 (22) ◽  
pp. 10931
Natasa P. Kalogiouri ◽  
Emmanouil-Nikolaos Papadakis ◽  
Maria G. Maggalou ◽  
George S. Karaoglanidis ◽  
Victoria F. Samanidou ◽  

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.

2021 ◽  
Vol 18 (4) ◽  
pp. 79-86
Divya Kottadiyil ◽  
Shital Deore ◽  
P. Sivaperumal

In recent years, exposure to pesticides has gained widespread attention due to their adverse health effects. Long-term exposure to pesticides has shown hazardous effects on vital functions of the human nervous and reproductive systems. Therefore, it is crucial to determine the extent of pesticide exposure in humans. Primarily, it is quite challenging to determine trace levels of pesticide residues in biological matrices. Hence, a quick, multi-residue extraction procedure was experimented for pesticide residue analysis in human serum. Herein, the original QuEChERS extraction method was modified for achieving the best possible recoveries. A total of 15 representative pesticides from each class were selected and fortified into the human serum samples. The extraction was performed by employing acidified solution containing acetonitrile and ethyl acetate followed by vortex and centrifugation. The obtained aqueous layer was collected and vapourised to dryness and d-SPE clean-up was conducted utilising PSA. The extracted sample was injected into the GC-MS/MS system under MRM mode. The method development parameters such as linearity, % RSD, accuracy, LOD, LOQ and % ME were assessed. The results obtained for the serum matrix were found to be within the criteria mentioned in European Union SANTE/12682/2019 guidelines for method validation. The developed solitary method is quick, simple and highly efficient for routine pesticide residue analysis. Hence, a wide spectrum of pesticides can be analysed utilising the proposed method for human serum.

2021 ◽  
Qun Zhang ◽  
Chen Ma ◽  
Yun Duan ◽  
Xiaopeng Wu ◽  
Daizhu Lv ◽  

Abstract The presence of pesticide residues in cowpea raises serious health concerns. In this study, a novel, sensitive, high-performance method was developed to simultaneously analyse the residues of 35 pesticides in cowpea samples from growing areas in Hainan provinces of China, from November in 2018 and June in 2021, using modified QuEChERS sample pretreatment coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). The limits of detection (LOD) and quantification (LOQ) values of 35 pesticides in the cowpea matrix ranged from 0.3 µg/kg to 2.5 µg/kg and 1.0 µg/kg to 8.0 µg/kg, respectively. Twenty-seven different pesticides were detected, and twelve of them were banned pesticides on legumes in China. Residues for ten pesticides in 17.1% of the samples exceeded their MRLs with the highest exceedance of 380%, 80.8% of samples contained one or more pesticide residues, and the most frequently detected pesticide was chlorfenapyr with a detection rate of 46.3%. In addition, the pesticide triazophos was detected through different years and regions. Furthermore, the chronic dietary exposure risk (%ADI) of the detected pesticides showed less than 100% in Chinese people of different age groups, which was evaluated by the national estimated acceptable daily intake.

Foods ◽  
2021 ◽  
Vol 10 (11) ◽  
pp. 2731
Shaowen Liu ◽  
Aijuan Bai ◽  
Le Song ◽  
Nan Zou ◽  
Yongtao Han ◽  

A convenient and fast multi-residue method for the efficient identification and quantification of 72 pesticides belonging to different chemical classes in red and white grape wines has been developed. The analysis was based on gas chromatography tandem quadrupole mass spectrometric determination (GC–MS/MS). The optimization strategy involved the selection of the amount of multi-walled carbon nanotubes (MWCNTs) and the number of cleanup procedure cycles for multi-plug filtration cleanup (m-PFC) to achieve ideal recoveries and reduce the sample matrix compounds in the final extracts. The optimized procedure obtained consistent recoveries between 70.2 and 108.8% (70.2 and 108.8% for white wine, and 72.3 and 108.4% for red wine), with relative standard deviations (RSDs) that were generally lower than 9.2% at the three spiking levels of 0.01, 0.05 and 0.1 mg/kg. The linearity was studied in the range between 0.002 and 0.1 mg/kg using pesticide standards prepared both in pure solvent and in the presence of the matrix, showing coefficients of determination (R2) higher than 0.9495 for all the pesticides. To improve accuracy, matrix-matched calibration curves were used for calculating the quantification results. Finally, the method was used successfully for detecting pesticide residues in commercial grape wines.

PLoS ONE ◽  
2021 ◽  
Vol 16 (11) ◽  
pp. e0258508
Sihua Peng ◽  
Aqiang Wang ◽  
Yuyang Lian ◽  
Xi Zhang ◽  
Bei Zeng ◽  

In order to achieve rapid detection of thiamethoxam residues in mango, cowpea and water, this study modified the screen printed carbon electrode (SPCE) to make a specific molecular imprinting sensor (Thiamethoxam-MIP/Au/rGO/SPCE) for thiamethoxam. An integrated smartphone platform was also built for thiamethoxam residue analysis. The performance of the complete system was analyzed by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The system was then applied for the rapid determination of thiamethoxam residues in water, mango and cowpea samples. The results showed that the molecular sensor showed good linearity in the range 0.5–3.0 μmol/L of thiamethoxam. The detection limit of thiamethoxam was 0.5 μmol/L. Moreover, the sensor had good reproducibility and anti-interference performance. The average recovery rates of the pesticide residues in water, mango and cowpea samples were in the range of 90–110% with relative standard deviations < 5%. The rapid detection system for thiamethoxam residue constructed in this study was simple, reliable, reproducible and had strong anti-interference. It has broad application prospects in the field detection of thiamethoxam residue, and serves as a valuable reference for the further development of rapid detection technology of pesticide residues in the field of environment and food safety.

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