Detection of Residual Pesticides in Foods

A special issue of Foods (ISSN 2304-8158). This special issue belongs to the section "Food Engineering and Technology".

Deadline for manuscript submissions: closed (15 December 2020) | Viewed by 37121

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Department of Chemistry and Physics, Universidad de Almería, Almeria, Spain
Interests: food safety; pesticides; analytical method development; chromatography; mass spectrometry; high-performance liquid chromatography
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Dear Colleagues,

Pesticides are used worldwide, and despite the fact that organic farming is increasing, they are still widely applied in different countries with pesticide regulations and monitoring programs. This Special Issue will cover the topic of the presence of pesticide residues in food, paying special attention to the use of modern analytical techniques based on chromatographic techniques coupled to mass spectrometry. Extraction methods should be generic in order to allow the detection of pesticides with different physic-chemical properties. Thus, in addition to targeted pesticides, the scope of this analysis can be increased if high-resolution mass spectrometry is used, performing targeted, nontargeted, and unknown analyses, including the detection of metabolites or unexpected pesticides.

Prof. Roberto Romero-González
Guest Editor

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Keywords

  • Pesticide residues
  • Food
  • Legislation
  • Generic methods
  • Chromatographic techniques
  • Mass spectrometry
  • Metabolites
  • Untargeted analysis

Published Papers (10 papers)

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Editorial

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3 pages, 181 KiB  
Editorial
Detection of Residual Pesticides in Foods
by Roberto Romero-González
Foods 2021, 10(5), 1113; https://doi.org/10.3390/foods10051113 - 18 May 2021
Cited by 7 | Viewed by 2235
Abstract
Pesticides are used worldwide [...] Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)

Research

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13 pages, 1714 KiB  
Article
Dynamics of the Degradation of Acetyl-CoA Carboxylase Herbicides in Vegetables
by Miroslav Jursík, Kateřina Hamouzová and Jana Hajšlová
Foods 2021, 10(2), 405; https://doi.org/10.3390/foods10020405 - 12 Feb 2021
Cited by 4 | Viewed by 2163
Abstract
(1) Background: Aryloxyphenoxy-propionates and cyclohexanediones are herbicides most widely used in dicot crops worldwide. The main objective of the study was to determine the dynamics of herbicide residues in carrot, lettuce, cauliflower, and onion in order to suggest a low level of residues [...] Read more.
(1) Background: Aryloxyphenoxy-propionates and cyclohexanediones are herbicides most widely used in dicot crops worldwide. The main objective of the study was to determine the dynamics of herbicide residues in carrot, lettuce, cauliflower, and onion in order to suggest a low level of residues in harvested vegetables. (2) Methods: Small plot field trials were carried out in four vegetables in the Czech Republic. The samples of vegetables were collected continuously during the growing season. Multiresidue methods for the determination of herbicide residues by LC-MS/MS were used. Non-linear models of degradation of individual herbicides in vegetables were calculated using the exponential decay formula. Action GAP pre-harvest intervals for the 25% and 50% maximum residue limit (MRL) and 10 µg kg−1 limit (baby food) were established for all tested herbicides. (3) Results: The degradation dynamics of fluazifop in carrot, onion, and cauliflower was significantly slower compared to quizalofop and haloxyfop. The highest amount (2796 µg kg−1) of fluazifop residues was detected in cauliflower 11 days after application. No residue of propaquizafop and cycloxydim was detected in any vegetable samples. (4) Conclusions: Aryloxyphenoxy-propionate herbicide (except propaquizafop) could contaminate vegetables easily, especially vegetables with a short growing season. Vegetables treated with fluazifop are not suitable for baby food. Lettuce and cauliflower treated by quizalofop are not suitable for baby food, but in onion and carrot, quizalofop could be used. Propaquizafop and cycloxydim are prospective herbicides for non-residual (baby food) vegetable production. Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)
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12 pages, 1743 KiB  
Article
Determination of Three Typical Metabolites of Pyrethroid Pesticides in Tea Using a Modified QuEChERS Sample Preparation by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry
by Hongping Chen, Xinlu Wang, Pingxiang Liu, Qi Jia, Haolei Han, Changling Jiang and Jing Qiu
Foods 2021, 10(1), 189; https://doi.org/10.3390/foods10010189 - 18 Jan 2021
Cited by 21 | Viewed by 3427
Abstract
Pyrethroid pesticides are widely used on tea plants, and their residues of high frequency and concentration have received great attention. Until recently, the residues of typical metabolites of pyrethroid pesticides in tea were unknown. Herein, a modified “quick, easy, cheap, effective, rugged and [...] Read more.
Pyrethroid pesticides are widely used on tea plants, and their residues of high frequency and concentration have received great attention. Until recently, the residues of typical metabolites of pyrethroid pesticides in tea were unknown. Herein, a modified “quick, easy, cheap, effective, rugged and safe” (QuEChERS) method for the determination of three typical metabolites of pyrethroid pesticides in tea, using ultra performance liquid chromatography tandem mass spectrometry, was developed. The mixture of florisil, octadecylsilane, and graphite carbon black was employed as modified QuEChERS adsorbents. A Kinetex C18 column achieved good separation and chromatographic peaks of all analytes. The calibration curves of 3-phenoxybenzoic acid (3-PBA) and 4-fluoro-3-phenoxybenzoic acid (4-F-3-PBA) were linear in the range of 0.1–50 ng mL−1 (determination coefficient R2 higher than 0.999), and that of cis-3-(2-chloro-3,3,3-trifluoroprop-1-en-1-yl)-2,2-dimethylcyclopropanecarboxylic acid (TFA) was in the range of 1–100 ng mL−1 (R2 higher than 0.998). The method was validated and recoveries ranged from 83.0% to 117.3%. Intra- and inter-day precisions were lower than or equal to 13.2%. The limits of quantification of 3-PBA, 4-F-3-PBA, and TFA were 5, 2, and 10 μg kg−1, respectively. A total of 22 tea samples were monitored using this method, and 3-PBA and TFA were found in two green tea samples. Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)
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15 pages, 1031 KiB  
Article
Pesticides and Environmental Contaminants in Organic Honeys According to Their Different Productive Areas toward Food Safety Protection
by Sara Panseri, Elisabetta Bonerba, Maria Nobile, Federica Di Cesare, Giacomo Mosconi, Francisco Cecati, Francesco Arioli, Giuseppina Tantillo and Luca Chiesa
Foods 2020, 9(12), 1863; https://doi.org/10.3390/foods9121863 - 14 Dec 2020
Cited by 20 | Viewed by 3389
Abstract
Monitoring contaminant residues in honey helps to avoid risks to human health, as it is a natural product widely consumed in all population groups, including the most vulnerable, such as children and the elderly. This is important for organic honey production that may [...] Read more.
Monitoring contaminant residues in honey helps to avoid risks to human health, as it is a natural product widely consumed in all population groups, including the most vulnerable, such as children and the elderly. This is important for organic honey production that may be negatively influenced by geographical area pollution. Considering the importance of collecting data on the occurrence of various xenobiotics in different geographical areas, this study aimed to investigate the presence of contaminant residues (persistent organic pollutants (POPs) and pesticides, including glyphosate and metabolites) in organic honey samples from different production areas using different analytical methods, in order to confirm their incidence and possible impact on the food safety traits of organic production. Regarding POPs, traces of benzofluoroanthene and chrysene were detected in honey from intensive orchards and arable lands. Traces of all polychlorobiphenyl (PCB) congeners were detected at different percentages in almost all of the samples, regardless of the origin area. Traces of polybromodiphenylethers (PBDE 28, 33, and 47) were found in different percentages of samples from all of the geographical areas examined. Traces of organochlorines (OCs) and organophosphates (OPs) were identified in honey samples belonging to all of the geographical areas. No glyphosate, glufosinate, and aminomethylphosphonic acid (AMPA) residues were detected. Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)
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25 pages, 296 KiB  
Article
Optimization of Method for Pesticide Detection in Honey by Using Liquid and Gas Chromatography Coupled with Mass Spectrometric Detection
by Mariana O. Almeida, Silvia Catarina S. Oloris, Vanessa Heloisa F. Faria, Márcia Cassimira M. Ribeiro, Daniel M. Cantini and Benito Soto-Blanco
Foods 2020, 9(10), 1368; https://doi.org/10.3390/foods9101368 - 26 Sep 2020
Cited by 29 | Viewed by 4271
Abstract
This study aimed to optimize and validate a multi-residue method for identifying and quantifying pesticides in honey by using both gas and liquid chromatographic separation followed by mass spectrometric detection. The proposed method was validated to detect 168 compounds, 127 of them by [...] Read more.
This study aimed to optimize and validate a multi-residue method for identifying and quantifying pesticides in honey by using both gas and liquid chromatographic separation followed by mass spectrometric detection. The proposed method was validated to detect 168 compounds, 127 of them by LC-MS/MS (liquid chromatography tandem mass spectrometric detection) and 41 by GC-MS/MS (gas chromatography tandem mass spectrometric detection). The limit of detection (LOD) and limit of quantification (LOQ) values for the analytes determined by LC-MS/MS were 0.0001–0.0004 mg/kg and 0.0002–0.0008 mg/kg, respectively. For GC-MS/MS analyses, the LOD and LOQ values were 0.001–0.004 mg/kg and 0.002–0.008 mg/kg. In total, 33 samples of commercial honey produced by apiaries in six Brazilian states were analyzed with the validated method. Residual amounts of 15 analytes were detected in 31 samples (93.9%). The method described in the present study was able to detect an extensive and broad range of pesticides with very high sensitivity. Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)
23 pages, 1555 KiB  
Article
Multifamily Determination of Phytohormones and Acidic Herbicides in Fruits and Vegetables by Liquid Chromatography–Tandem Mass Spectrometry under Accredited Conditions
by Ángel Grande Martínez, Francisco Javier Arrebola Liébanas, Rosario Santiago Valverde, María Elena Hernández Torres, Juan Ramírez Casinello and Antonia Garrido Frenich
Foods 2020, 9(7), 906; https://doi.org/10.3390/foods9070906 - 09 Jul 2020
Cited by 10 | Viewed by 2678
Abstract
A 7-min multifamily residue method for the simultaneous quantification and confirmation of 8 phytohormones and 27 acidic herbicides in fruit and vegetables using ultra high-performance liquid chromatography (UHPLC) coupled to tandem mass spectrometry (MS/MS) was developed, validated according to SANTE 12682/2019, and accredited [...] Read more.
A 7-min multifamily residue method for the simultaneous quantification and confirmation of 8 phytohormones and 27 acidic herbicides in fruit and vegetables using ultra high-performance liquid chromatography (UHPLC) coupled to tandem mass spectrometry (MS/MS) was developed, validated according to SANTE 12682/2019, and accredited according to UNE-EN-ISO/IEC 17025:2017. Due to the special characteristics of these kinds of compounds, a previous step of alkaline hydrolysis was carried out for breaking conjugates that were potentially formed due to the interactions of the analytes with other components present in the matrix. Sample treatment was based on QuEChERS extraction and optimum detection conditions were individually optimized for each analyte. Cucumber (for high water content commodities) and orange (for high acid and high water content samples) were selected as representative matrices. Matrix-matched calibration was used, and all the validation criteria established in the SANTE guidelines were satisfied. Uncertainty estimation for each target compound was included in the validation process. The proposed method was applied to the analysis of more than 450 samples of cucumber, orange, tomato, watermelon, and zucchini during one year. Several compounds, such as 2,4-dichlorophenoxyacetic acid (2,4-D), 4-(3-indolyl)butyric acid (IBA), dichlorprop (2,4-DP), 2-methyl-4-chlorophenoxy acetic acid (MCPA), and triclopyr were found, but always at concentrations lower than the maximum residue level (MRL) regulated by the EU. Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)
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21 pages, 2065 KiB  
Article
Evaluation of Pesticide Residue Dynamics in Lettuce, Onion, Leek, Carrot and Parsley
by Tereza Horská, František Kocourek, Jitka Stará, Kamil Holý, Petr Mráz, František Krátký, Vladimír Kocourek and Jana Hajšlová
Foods 2020, 9(5), 680; https://doi.org/10.3390/foods9050680 - 25 May 2020
Cited by 14 | Viewed by 4832
Abstract
The dynamics of 32 active substances contained in pesticide formulations (15 fungicides and 17 insecticides) were analyzed in iceberg lettuce, onion, leek, carrot, and parsley. Pesticide residues were monitored from the time of application until harvest. In total, 114 mathematical models of residue [...] Read more.
The dynamics of 32 active substances contained in pesticide formulations (15 fungicides and 17 insecticides) were analyzed in iceberg lettuce, onion, leek, carrot, and parsley. Pesticide residues were monitored from the time of application until harvest. In total, 114 mathematical models of residue dissipation were developed using a first-order kinetic equation. Based on these models, it was possible to predict the action pre-harvest interval (the time between the last pesticide application and crop harvest) needed to attain a targeted action threshold (value significantly lower than the maximum limit) for low-residue vegetable production. In addition, it was possible to determine an action pre-harvest interval based on an action threshold of 0.01 mg kg−1 to produce vegetables intended for zero-residue production. The highest amount of pesticide residues were found in carrot and parsley leaves several days after treatment, and pesticide dissipation was generally slow. Lower amounts were found in leeks and lettuce, but pesticide dissipation was faster in lettuce. According to our findings, it seems feasible to apply reduced pesticide amounts to stay below unwanted residue levels. However, understanding the effectivity of reduced pesticide application for controlling relevant pest organisms requires further research. Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)
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13 pages, 1420 KiB  
Article
Development and Application of a Novel Pluri-Residue Method to Determine Polar Pesticides in Fruits and Vegetables through Liquid Chromatography High Resolution Mass Spectrometry
by Lorena Manzano-Sánchez, José Antonio Martínez-Martínez, Irene Domínguez, José Luis Martínez Vidal, Antonia Garrido Frenich and Roberto Romero-González
Foods 2020, 9(5), 553; https://doi.org/10.3390/foods9050553 - 01 May 2020
Cited by 14 | Viewed by 3968
Abstract
Nowadays, highly polar pesticides are not included in multiresidue methods due to their physico-chemical characteristics and therefore, specific analytical methodologies are required for their analysis. Laboratories are still looking for a pluri-residue method that encompasses the largest number of polar pesticides. The aim [...] Read more.
Nowadays, highly polar pesticides are not included in multiresidue methods due to their physico-chemical characteristics and therefore, specific analytical methodologies are required for their analysis. Laboratories are still looking for a pluri-residue method that encompasses the largest number of polar pesticides. The aim of this work was the simultaneous determination of ethephon, 2-hydroxyethylphosphonic acid (HEPA), fosetyl aluminum, glyphosate, aminomethylphosphonic acid (AMPA), N-acetyl-glyphosate and N-acetyl-AMPA in tomatoes, oranges, aubergines and grapes. For that purpose, an ultra high performance liquid chromatography (UHPLC) coupled to a high resolution single mass spectrometer Orbitrap-MS were used. Different stationary phases were evaluated for chromatographic separation, and among them, the stationary phase Torus DEA provided the best separation of the selected compounds. The QuPPe method was used for the extraction of the analytes, but slight modifications were needed depending on the matrix. The developed method was validated, observing matrix effect in all matrices. Intra- and inter-day precision were estimated, and relative standard deviation were lower than 19%. Recoveries were satisfactory, and mean values ranged from 70% to 110%. Limits of quantification were between 25 and 100 µg kg−1. Finally, the analytical method was applied to different fruits and vegetables (oranges, tomatoes, aubergines and grapes). Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)
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14 pages, 785 KiB  
Article
Organochlorine Pesticides and PCBs in Traditionally and Industrially Smoked Pork Meat Products from Bosnia and Herzegovina
by Brankica Kartalović, Krešimir Mastanjević, Nikolina Novakov, Jelena Vranešević, Dragana Ljubojević Pelić, Leona Puljić and Kristina Habschied
Foods 2020, 9(1), 97; https://doi.org/10.3390/foods9010097 - 17 Jan 2020
Cited by 11 | Viewed by 4287
Abstract
The aim of this study was to determine the concentration of 19 organochlorine pesticides (OCPs): (hexachlorocyclohexane (α-HCH, β-HCH, δ–HCH), lindane, aldrin, heptachlor, heptachlor epoxide, trans-chlordane, cis-chlordane, endosulfane I, endosulfane II, endosulfane sulfate, dichlorodiphenyltrichloroethane (DDT), dichlorodiphenyldichloroethylene (DDE), dieldrin, endrin, dichlorodiphenyldichloroethane (DDD), methoxychlor [...] Read more.
The aim of this study was to determine the concentration of 19 organochlorine pesticides (OCPs): (hexachlorocyclohexane (α-HCH, β-HCH, δ–HCH), lindane, aldrin, heptachlor, heptachlor epoxide, trans-chlordane, cis-chlordane, endosulfane I, endosulfane II, endosulfane sulfate, dichlorodiphenyltrichloroethane (DDT), dichlorodiphenyldichloroethylene (DDE), dieldrin, endrin, dichlorodiphenyldichloroethane (DDD), methoxychlor and endrin ketone and 6 polychlorinated biphenyls (PCBs) (PCB 28, PCB 52, PCB 101, PCB 153, PCB 138 and PCB 180). The samples were taken from pancetta, dry pork neck (budiola), pork tenderloin and sausages produced in Rakitno (Bosnia and Herzegovina), smoked in both a traditional smokehouse and in an industrial chamber. Instrumental analysis was performed using gas chromatography–mass spectrometry (GC–MS). The reliability of the results, i.e., quality control is ensured by standard laboratory practice, which involves participation in proficiency test, the use of blank samples, reference materials and implementation of recommendations given by the relevant international organizations. The concentrations of α-HCH, lindane, PCB 28, PCB 52 and PCB 153 were detected and quantified. The concentrations of OCPs and PCBs did not significantly vary depending on product type and the conditions of production. All the examined samples were for human consumption. Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)
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12 pages, 473 KiB  
Article
Dispersive Solid–Liquid Extraction Coupled with LC-MS/MS for the Determination of Sulfonylurea Herbicides in Strawberries
by Nho-Eul Song, Dong-Ho Seo, Ji Yeon Choi, Miyoung Yoo, Minseon Koo and Tae Gyu Nam
Foods 2019, 8(7), 273; https://doi.org/10.3390/foods8070273 - 22 Jul 2019
Cited by 15 | Viewed by 4441
Abstract
The monitoring of food quality and safety requires a suitable analytical method with simultaneous detection in order to control pesticide and herbicide residues. In this study, a novel analytical method, referred to as “dispersive solid–liquid extraction”, was applied to monitor seven sulfonylurea herbicides [...] Read more.
The monitoring of food quality and safety requires a suitable analytical method with simultaneous detection in order to control pesticide and herbicide residues. In this study, a novel analytical method, referred to as “dispersive solid–liquid extraction”, was applied to monitor seven sulfonylurea herbicides in strawberries. This method was optimized in terms of the amount of C18 and the volume of added water, and it was validated through satisfactory linearities (R2 > 0.99), recoveries of 70% to 84% with acceptable precisions, and limits of quantification lower than the maximum residue limits for the seven sulfonylurea herbicides in strawberries. The cleanup efficiency of the dispersive solid–liquid extraction technique was compared to that of the QuEChERS- (“quick, easy, cheap, effective, rugged and safe”) based method with dispersive solid phase extraction. The recoveries of the former were found to be comparable to those involving QuEChERS C18 cleanup (recoveries of 74%–87%). The method was used to determine sulfonylurea herbicide residues in ten strawberry samples. None of the samples had herbicide residues higher than that of limit of quantifications (LOQs) or maximum residue limits (MRLs). The results suggest that the dispersive solid–liquid extraction method combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) is effective for the analysis of sulfonylurea herbicide residues in strawberries. Full article
(This article belongs to the Special Issue Detection of Residual Pesticides in Foods)
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