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Development of Analytical Methods to Analyze Pesticide Residues

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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (28 February 2022) | Viewed by 38055

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Dr. Thierry Dagnac

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Galician Agency for Food Quality—Agronomic and Agrarian Research Centre (AGACAL-CIAM), Unit of Organic Contaminants, Apartado 10, 15080 A Coruña, Spain
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Dr. Pilar Sandín-España

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Instituto Nacional de Investigacion y Tecnologia Agraria y Alimentaria, Plant Protection Products Unit, Madrid, Spain
Interests: pesticides; by-products; degradation; phytotoxicity; herbicide; degradation products; transformation products; quantitative structure–activity relationship; photodegradation; chlorination
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Dear Colleagues,

Plant protection products have been used in agriculture throughout the world since the middle of the 20th century to control pests, diseases and weeds in crops and it is known that the use of pesticides provides unquestionable benefits in increasing agricultural production. However, since pesticide residues can widely dispersed from their application areas, they can reach environment and food chain constituting a potential risk to consumers. In this sense, authorities and agricultural sector try to establish a high level of protection to human, animal health and the environment, preventing the approval of hazardous substances with a major environmental impact, establishing legal directives to control their levels through e.g. the Maximum Residue Levels, and searching on and on for pesticides less persistent and toxic for human consumers.

The analysis of pesticide residues in food and environmental samples has received increasing attention in the last few decades and different techniques are used since pesticides include a variety of compounds with very different physico-chemical characteristics and large differences in polarity, volatility and thermal stability. Analysis of pesticides still remains a challenge due to the low detection levels required by regulatory bodies and the complex nature of the matrices in which the target compounds are present. Therefore, analytical methodologies with efficient sample preparation and very low level detection and identification to provide the sensitivity, selectivity, and specificity needed to meet EU legislation for the analysis of pesticides in environmental and food samples are strongly required.

This special issue aims to attract contributions, original research or review articles, on all aspects related to the optimization and the validation of analytical methods for the determination of pesticides in different matrices such as food or environmental compartments and also to describe the recent advances and future trends and innovations. Studies focused on “green” sample preparation, monitoring and identification of pesticide degradation products by high resolution mass spectrometry are also welcome.

You may choose our Joint Special Issue in Chemistry.

Dr. Thierry Dagnac
Dr. Pilar Sandín-España
Guest Editors

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Keywords

Pesticide residue analysis
Chromatography
Extraction procedure
Green Sample preparation
Degradation products
Mass spectrometry
Analytical method validation
Trace levels

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Development of Analytical Methods to Analyze Pesticide Residues in Chemistry

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Editorial

Jump to: Research, Review

4 pages, 220 KiB

Open AccessEditorial

Development of Analytical Methods to Analyze Pesticide Residues

by Pilar Sandín-España and Thierry Dagnac

Molecules 2023, 28(7), 3074; https://doi.org/10.3390/molecules28073074 - 30 Mar 2023

Cited by 1 | Viewed by 1855

Abstract

Pesticides are compounds applied on crops to eliminate or control pests, diseases and weeds and it is known that their use provides unquestionable benefits in increasing agricultural production [...] Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

Research

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15 pages, 3018 KiB

Open AccessArticle

The Binary Mixtures of Lambda-Cyhalothrin, Chlorfenapyr, and Abamectin, against the House Fly Larvae, Musca domestica L.

by Doaa F. El Sherif, Nagat H. Soliman, Khalid S. Alshallash, Nevin Ahmed, Mervat A. R. Ibrahim, Kholoud A. Al-Shammery and Areej A. Al-Khalaf

Molecules 2022, 27(10), 3084; https://doi.org/10.3390/molecules27103084 - 12 May 2022

Cited by 5 | Viewed by 2759

Abstract

The house fly Musca domestica L. is one of the medical and veterinary pests that can develop resistance to different insecticides. Mixing insecticides is a new strategy for accelerating pest control; furthermore, it can overcome insect resistance to insecticides. This study aims to evaluate three insecticides, chlorfenapyr, abamectin, and lambda-cyhalothrin, individually and their binary mixtures against 2nd instar larvae of M. domestica laboratory strain. Chlorfenapyr exhibited the most toxic effect on larvae, followed by abamectin then the lambda-cyhalothrin. The half-lethal concentrations (LC₅₀) values were 3.65, 30.6, and 94.89 ppm, respectively. These results revealed that the high potentiation effect was the mixture of abamectin/chlorfenapyr in all the mixing ratios. In contrast, the tested combination of lambda-cyhalothrin/abamectin showed an antagonism effect at all mixing ratios against house fly larvae. The total protein, esterases, glutathione-S-transferase (GST), and cytochrome P-450 activity were also measured in the current investigation in the larvae treated with chlorfenapyr. Our results indicate that GST may play a role in detoxifying chlorfenapyr in M. domestica larvae. The highest activity of glutathione-S-transferase was achieved in treated larvae with chlorfenapyr, and an increase in cytochrome P-450 activity in the larvae was observed post-treatment with Abamectin/chlorfenapyr. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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16 pages, 1450 KiB

Open AccessArticle

Analysis of Pesticide Residues by QuEChERS Method and LC-MS/MS for a New Extrapolation of Maximum Residue Levels in Persimmon Minor Crop

by Pilar Sandín-España, Miguelina Mateo-Miranda, Carmen López-Goti, Elena Seris-Barrallo and José-Luis Alonso-Prados

Molecules 2022, 27(5), 1517; https://doi.org/10.3390/molecules27051517 - 23 Feb 2022

Cited by 9 | Viewed by 2735

Abstract

According to EU guidance SANCO/7525/VI/95 Rev. 10.3, residue data extrapolation from a surrogate major crop to a minor crop can be used for setting maximum residue levels (MRLs) with a reduced number of residue trials and representative selected pesticides. In this work, a QuEChERS method (citrate-buffered version and PSA with MgSO₄ clean-up) and LC-ESI-MS/MS for the determination of boscalid, pyraclostrobin, fludioxonil, fluopyram and tebuconazole in persimmon was developed and validated according to EU Commission guidelines and afterwards used for the determination of residues in four field trials. Residue levels at harvest for each pesticide ranged between 0.347 and 0.028 mg/kg. After comparing EFSA residue data on apples, as the surrogate major crop, and conducting a consumer risk assessment, a proposal of residue data extrapolation to set MRLs in persimmons was performed. The results showed that pesticide residues in persimmons at harvest were consistently lower than residues in apples when substances were applied according to the same critical GAP. MRLs were set at 0.5 mg/kg for fludioxonil, 0.6 mg/kg for boscalid, 0.3 mg/kg for tebuconazole, 0.4 mg/kg for fluopyran and 0.3 mg/kg for pyraclostrobin. The ratio of the MRLs for apple/persimmon varied between 2.5 for boscalid and 1.25 for fluopyram, suggesting that residue extrapolation can be feasible, promoting the process of pesticide registration for minor crops and the settlement of MRL. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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16 pages, 1752 KiB

Open AccessArticle

Targeted Multiresidue Method for the Analysis of Different Classes of Pesticides in Agro-Food Industrial Sludge by Liquid Chromatography Tandem Mass Spectrometry

by Niki C. Maragou, George Balayiannis, Evangelos Karanasios, Emilia Markellou and Konstantinos Liapis

Molecules 2021, 26(22), 6888; https://doi.org/10.3390/molecules26226888 - 15 Nov 2021

Cited by 6 | Viewed by 1904

Abstract

Sludge generated after washing of fruits and vegetables during agro-food processes is a complex matrix and selective methods for the identification and quantification of pesticides’ residues are necessary in order to achieve a sustainable and effective management of the total sewage. The present work describes the development and validation of a reliable, simple and fast analytical method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of 47 pesticides of different chemical classes, including organosphosphates, pyrethroids, neonicotinoids, triazoles and others, in sludge samples after QuEChERS sample preparation. The necessity of the individual steps of QuEChERS was investigated and the LC-ESI-MS/MS conditions were optimized to achieve maximum sensitivity of the target analytes. The method limits of detection (LODs) ranged between 0.0005 mg/kg (imidacloprid) and 0.05 mg/kg (beta cyfluthrin). The recoveries ranged between 71–120% and the repeatability of the method was ≤25% expressed as relative standard deviation. The method was applied to sludge samples generated after washing of fruits in an agro-fruit-packaging unit in Greece. The results showed the presence of 37 pesticides’ active substances with concentrations ranging from low ppbs, such as fludioxinil (5 μg/kg) up to low ppms such as beta cyfluthrin (3.5 mg/kg) and with their sum concentration reaching up to 19 mg/kg. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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13 pages, 626 KiB

Open AccessArticle

Optimization of a Multiresidue Analysis of 65 Pesticides in Surface Water Using Solid-Phase Extraction by LC-MS/MS

by Bahar Nakhjavan, Jason Bland and Maryam Khosravifard

Molecules 2021, 26(21), 6627; https://doi.org/10.3390/molecules26216627 - 1 Nov 2021

Cited by 21 | Viewed by 3871

Abstract

An analytical method was developed and validated for simultaneous quantitation of 65 pesticides, including one single solid-phase extraction (SPE) procedure in surface water by liquid chromatography coupled to tandem mass spectroscopy. Different parameters that have an influence on extraction efficiency were evaluated in this research. Different types of cartridges, elution solvents, and sorbent drying time were investigated, and the most appropriate one was selected. Moreover, various pretreatment techniques were applied to remove sediments from water without the loss of pesticides. Centrifugation was introduced as the best option at the beginning of sample preparation to resolve the clogging of the sorbent cartridges. The recoveries of all pesticides ranged from 70% to 120%, with a relative standard deviation of less than 13.7%. The feasibility of the method was evaluated on 10 surface water samples with different concentrations of sand, sediment, and particles. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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17 pages, 2323 KiB

Open AccessArticle

Occurrence of Fungicides in Vineyard and the Surrounding Environment

by Meruyert Sergazina, Lua Vazquez, Maria Llompart and Thierry Dagnac

Molecules 2021, 26(20), 6152; https://doi.org/10.3390/molecules26206152 - 12 Oct 2021

Cited by 7 | Viewed by 2772

Abstract

Seventeen fungicides were determined in different matrices from vineyard areas, including vine leaves, soils, grapes and water, using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). For leaf analysis, ultrasound-assisted extraction (UAE) was performed evaluating different solvents. UAE was compared with other extraction techniques such as vortex extraction (VE) and matrix solid-phase dispersion (MSPD). The performance of the UAE method was demonstrated on vine leaf samples and on other types of samples such as tea leaves, underlining its general suitability for leaf crops. As regards other matrices, soils were analyzed by UAE and microwave-assisted extraction (MAE), grapes by UAE and waters by SPE using cork as the sorbent. The proposed method was applied to 17 grape leaf samples in which 14 of the target fungicides were detected at concentrations up to 1000 μg g⁻¹. Furthermore, the diffusion and transport of fungicides was demonstrated not only in crops but also in environmental matrices. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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12 pages, 1343 KiB

Open AccessArticle

Simultaneous Analysis of Fenpropimorph and Fenpropimorph Acid in Six Different Livestock Products Using a Single-Sample Preparation Method Followed by Liquid Chromatography–Tandem Mass Spectrometry

by Seon Wook Kim, Da Jung Lim and In Seon Kim

Molecules 2021, 26(19), 5791; https://doi.org/10.3390/molecules26195791 - 24 Sep 2021

Cited by 3 | Viewed by 1829

Abstract

Pesticides in livestock products must be measured to ensure food safety. We developed a single-sample preparation method followed by liquid chromatography–tandem mass spectrometry (LC-MS/MS) for simultaneous determination of fenpropimorph and fenpropimorph acid in six different livestock products. The extraction method was a modification of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and was validated according to the CODEX guidelines. The matrix-matched calibration curves for fenpropimorph and fenpropimorph acid exhibited good linearity, with coefficients of determination (R² values) higher than 0.998. The limit of detection (LOD) and the limit of quantitation (LOQ) were 1.25 and 5.0 µg kg⁻¹, respectively. The average recovery values ranged from 61.5% to 97.1% for samples fortified to the LOQ, 2 × LOQ, and 10 × LOQ. The method fully complied with the CODEX guidelines and was successfully applied to real samples obtained from domestic markets. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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16 pages, 14002 KiB

Open AccessArticle

Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

by Harischandra Naik Rathod, Bheemanna Mallappa, Pallavi Malenahalli Sidramappa, Chandra Sekhara Reddy Vennapusa, Pavankumar Kamin, Udaykumar Revanasiddappa Nidoni, Bheemsain Rao Kishan Rao Desai, Saroja Narsing Rao and Paramasivam Mariappan

Molecules 2021, 26(7), 1837; https://doi.org/10.3390/molecules26071837 - 25 Mar 2021

Cited by 9 | Viewed by 3246

Abstract

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg⁻¹ for Capsicum and 0.10 to 9.55 µg·kg⁻¹ (LOD) and 0.35 to 33.43 µg·kg⁻¹ (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSD_wR) by spiking of mixed pesticides standards at 100 µg·kg⁻¹ recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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13 pages, 1073 KiB

Open AccessArticle

Validation of a Rapid Multiresidue Method for the Determination of Pesticide Residues in Vine Leaves. Comparison of the Results According to the Different Conservation Methods

by Salem Hayar, Rawan Zeitoun and Britt Marianna Maestroni

Molecules 2021, 26(4), 1176; https://doi.org/10.3390/molecules26041176 - 22 Feb 2021

Cited by 11 | Viewed by 2548

Abstract

The QuEChERS method was applied to the determination of pesticide residues in vine (Vitis vinifera) leaves by LC-MSMS. The method was validated in-house for 33 pesticides representing 17 different chemical groups, that are most commonly used in grape production. Recoveries for the pesticides tested ranged from 75 to 104%, and repeatability and reproducibility relative standard deviations (RSD_r% and RSD_Rw%) were less than 20%. The method was applied to the analysis of pesticide residues in 17 market brands of vine leaves processed according to three different preservation methods and sampled from the Lebanese market. Dried vine leaves were more contaminated with pesticide residues than those preserved in brine or stuffed vine leaves. The systemic fungicides were the most frequently detected among all the phytosanitary compounds usually applied to grape production. Brine-preserved and stuffed vine leaves contained lower concentrations of the residues but still contained a cocktail of different pesticides. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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Review

Jump to: Editorial, Research

21 pages, 484 KiB

Open AccessReview

Analytical Extraction Methods and Sorbents’ Development for Simultaneous Determination of Organophosphorus Pesticides’ Residues in Food and Water Samples: A Review

by Krishna Veni Veloo and Nur Amirah Syahirah Ibrahim

Molecules 2021, 26(18), 5495; https://doi.org/10.3390/molecules26185495 - 10 Sep 2021

Cited by 16 | Viewed by 3799

Abstract

Extensive use of organophosphorus pesticides in agriculture leads to adverse effects to the environment and human health. Sample preparation is compulsory to enrich target analytes prior to detection as they often exist at trace levels and this step is critical as it determines the concentration of pollutants present in samples. The selection of a suitable extraction method is of great importance. The analytical performance of the extraction methods is influenced by the selection of sorbents as sorbents play a vital role in the sensitivity and selectivity of an analytical method. To date, numerous sorbent materials have been developed to cater to the needs of selective and sensitive pesticides’ detection. Comprehensive details pertaining to extraction methods, developed sorbents, and analytical performance are provided. This review intended to provide a general overview on different extraction techniques and sorbents that have been developed in the last 10 years for organophosphorus pesticides’ determinations in food and water samples. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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28 pages, 1167 KiB

Open AccessReview

Application of Compound-Specific Isotope Analysis in Environmental Forensic and Strategic Management Avenue for Pesticide Residues

by Eun-Ji Won, Hee-Young Yun, Dong-Hun Lee and Kyung-Hoon Shin

Molecules 2021, 26(15), 4412; https://doi.org/10.3390/molecules26154412 - 21 Jul 2021

Cited by 11 | Viewed by 4756

Abstract

Unintended pesticide pollution in soil, crops, and adjacent environments has caused several issues for both pesticide users and consumers. For users, pesticides utilized should provide higher yield and lower persistence while considering both the environment and agricultural products. Most people are concerned that agricultural products expose humans to pesticides accumulating in vegetation. Thus, many countries have guidelines for assessing and managing pesticide pollution, for farming in diverse environments, as all life forms in soil are untargeted to these pesticides. The stable isotope approach has been a useful technique to find the source of organic matter in studies relating to aquatic ecology and environmental sciences since the 1980s. In this study, we discuss commonly used analytical methods using liquid and gas chromatography coupled with isotopic ratio mass spectrometry, as well as the advanced compound-specific isotope analysis (CSIA). CSIA applications are discussed for tracing organic pollutants and understanding chemical reactions (mechanisms) in natural environments. It shows great applicability for the issues on unintended pesticide pollution in several environments with the progress history of isotope application in agricultural and environmental studies. We also suggest future study directions based on the forensic applications of stable isotope analysis to trace pesticides in the environment and crops. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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28 pages, 1398 KiB

Open AccessReview

Non-Occupational Exposure to Pesticides: Experimental Approaches and Analytical Techniques (from 2019)

by Lucía Vera-Herrera, Daniele Sadutto and Yolanda Picó

Molecules 2021, 26(12), 3688; https://doi.org/10.3390/molecules26123688 - 16 Jun 2021

Cited by 6 | Viewed by 3709

Abstract

Background: Pesticide residues are a threat to the health of the global population, not only to farmers, applicators, and other pesticide professionals. Humans are exposed through various routes such as food, skin, and inhalation. This study summarizes the different methods to assess and/or estimate human exposure to pesticide residues of the global population. Methods: A systematic search was carried out on Scopus and web of science databases of studies on human exposure to pesticide residues since 2019. Results: The methods to estimate human health risk can be categorized as direct (determining the exposure through specific biomarkers in human matrices) or indirect (determining the levels in the environment and food and estimating the occurrence). The role that analytical techniques play was analyzed. In both cases, the application of generic solvent extraction and solid-phase extraction (SPE) clean-up, followed by liquid or gas chromatography coupled to mass spectrometry, is decisive. Advances within the analytical techniques have played an unquestionable role. Conclusions: All these studies have contributed to an important advance in the knowledge of analytical techniques for the detection of pesticide levels and the subsequent assessment of nonoccupational human exposure. Full article

(This article belongs to the Special Issue Development of Analytical Methods to Analyze Pesticide Residues)

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