Residual Monitoring Research Articles

Quantum Dots‐Engineered Flexible Hydrogel as Plant‐Wearable Sensor for on‐Site Profiling Dynamic Pesticide Degradation

AbstractEngineering wearable devices for in situ and on‐site monitoring of pesticide residues from plants in a non‐destructive manner is of great research value but remains a huge challenge. In this study, a plant‐wearable fluorescence sensor CdTe CDs@PVA@AG, is designed and constructed by embedding CdTe QDs in polyvinyl alcohol (PVA) and agarose (AG)‐co‐assembled double‐network hydrogel to transmit on‐the‐scene pesticides residues messages. Harnessing red emission and stimuli‐responsive performance of CdTe QDs, as well as hydrogel's excellent flexibility, high adhesion, and porous network, CdTe CDs@PVA@AG is endowed with quantitative response to thiram at ≈µm level within 2 min through promoting fluorescence silence in conjunction with the transformation of images into primary colors as digital signals. More interestingly, CdTe CDs@PVA@AG is capable of being tightly pasted onto various crops’ surfaces and then is not only explored to appraise pesticide residue levels but also to profile the dynamic pesticide degradation, in a non‐destructive manner. This work opens up a new avenue to engineer plant‐wearable devices for in situ, on‐site, and non‐destructive capturing of the pesticide residue information from crops, favoring the accurate monitoring of the health status of crops, and rapid and healthy development of smart agriculture.

Adoption of Hygienic Meat Production and Handling Practices among Value Chain Stakeholders of Chevon and Carabeef in Kerala, India

This study investigated the adoption of hygienic practices in Kerala's chevon and carabeef value chain, focusing on production and handling methods. Using a stratified multistage sampling approach, the research examined three stakeholder groups: farmers (producers), traders, and retailers. For farmers, the assessment covered hygiene practices in feeding, environmental management, livestock health, and biosecurity. For traders and retailers, evaluation parameters included animal welfare standards, handling protocols, transportation compliance, regulatory adherence, traceability systems, slaughter hygiene, packaging methods, and waste management practices. Demographic analysis revealed that participants were predominantly middle-aged males with secondary education and substantial industry experience. The findings indicated moderate adoption of hygiene practices across all stakeholder categories. The domain-specific analysis highlighted critical areas requiring improvement: antimicrobial resistance management, residue monitoring, biosecurity protocols, and general hygiene practices throughout the value chain. For meat traders and retailers specifically, the study identified regulatory compliance, product traceability, personal and environmental hygiene, and waste management as key areas needing enhancement. These findings underscore the necessity for targeted interventions to improve hygiene standards across Kerala's red meat value chain.

Antibiotic Residues in Animal Products from Some African Countries and Their Possible Impact on Human Health.

This review investigates the levels of antibiotic residues in animal products, types of antibiotics, and their possible impact on human health in Africa. The literature search involved the use of a systematic survey using data that were published from Africa from 2015 to 2024. The search terms used the Boolean operators with keywords such as antibiotics, antibiotic residues, antibiotics in animal products in Africa, and impact on human health. Only research conducted in Africa was used in the present study. The findings showed that the most prevalent groups of antibiotic residues were aminoglycoside, macrolides, β-lactams, fluoroquinolones, tetracyclines sulfonamides, and phenicols. Tetracycline showed the most prevalent antibiotic residue with 43% mostly from East Africa, followed by sulfonamides at 19%, and β-lactams at 16%; most of the antibiotic residue levels were higher than the World Health Organization permissible limit. Noncompliance with withdrawal periods and maximum residue limits for antibiotics used in food-producing animals may lead to negative outcomes such as allergic reactions, teratogenicity, carcinogenicity, microbiome alterations, and, most notably, antibiotic resistance. As a result, there is a need for constant monitoring of antibiotic residues in animal products in addition to the consideration of alternatives to antibiotics in order to avoid their health implications.

Method Validation for Estimation of Imidacloprid and its Metabolites in Maize and Soil by LCMS-MS.

Validation of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was performed for estimation of imidacloprid (IM) and its metabolites in maize leaves, immature kernels, mature kernels, stalk, and soil using liquid chromatograph tandem mass spectrometry, coupled with electrospray ionization. The extraction in different matrices of maize and soil was performed using acetonitrile +0.1% formic acid followed by clean-up with primary secondary amine sorbent and anhydrous magnesium sulfate. The method was validated in terms of selectivity, linearity, limit of detection, limit of quantification, matrix effect, ion ratios, quality control, robustness, accuracy, and precision. The validation of all parameters was done in accordance with European Commission's Directorate-General for Health and Food Safety (DG SANTE) guidelines. A linear relationship with high correlation coefficients R2 > 0.99 was obtained for solvents and different matrices viz., maize leaves, immature kernels, mature kernels, stalk, and soil. The recovery and relative standard deviations were ˃78% and ˂5.4%, respectively. This method permits a simple, sensitive, accurate, cost-effective, precise, and rapid extraction of IM and its metabolites from maize leaves, immature kernels, mature kernels, stalks, and soil. This can help the residue analysts to address effective residue estimation, regular monitoring of residues and can also aid in the regulatory and food safety concerns about the usage of IM in maize.

Detection of glyphosate, glufosinate, and their metabolites in multi-floral honey for food safety

Beehives can accumulate environmental contaminants as bees gather pollen, propolis, and water from their surroundings, contaminating hive products like honey. Moreover, in multifloral environments, bees can interact with plants treated with different pesticides, often causing higher pesticides concentrations in multi-floral honey than in mono-floral varieties. Glyphosate and glufosinate are both widely used herbicides. Glyphosate accounted for one-third of herbicide sales in Europe in 2017 and continues to raise health concerns, including its potential carcinogenicity. While the European Commission extended glyphosate’s authorisation for another 10 years in 2023, concerns remain about its impact on biodiversity and human health. This study aimed to monitor the presence of glyphosate, glufosinate, and their metabolites in 100 samples of multifloral honey representing Italian production by analysis using IC-HRMS. Results indicated that 12% of honey samples contained glyphosate residues ranging from > LOQ to 45 ng g−1, with the highest concentrations detected in the Puglia region. No sample exceeded the maximum residue levels set by EU regulations. Glufosinate and its metabolites were not detected in any samples. These findings underscore the need for continued monitoring of pesticide residues in honey, particularly given the potential ‘cocktail effect’ of multiple contaminants and their combined toxicity. This study highlights the importance of safeguarding consumer health, especially in vulnerable populations, by addressing gaps in data on pesticide residue levels.

Rapid pesticide residues detection by portable filter-array hyperspectral imaging.

The detection of pesticide residues in agricultural products is crucial for ensuring food safety. However, traditional methods are often constrained by slow processing speeds and a restricted analytical scope. This study presents a novel method that uses filter-array-based hyperspectral imaging enhanced by a dynamic filtering demosaicking algorithm, which significantly improves the speed and accuracy of detecting pesticide residues. Our approach enhances the spatial and spectral resolution of hyperspectral images, thereby providing a rapid and cost-effective alternative to conventional methods with an image integration time of 20ms. Tested on both synthetic datasets and real agricultural samples, this technology demonstrates superior performance under high noise conditions and exceptional precision in spectral reconstruction at critical color edges. The practicality of this system is demonstrated by integrating a hyperspectral microfilter array with a smartphone's imaging sensor, thereby showcasing the feasibility of deploying this advanced detection technology in everyday portable devices for quick and convenient monitoring of pesticide residues.

Monitoring of veterinary drug residues in mutton based on hyperspectral combined with explainable AI: A case study of OFX

Monitoring of veterinary drug residues in mutton based on hyperspectral combined with explainable AI: A case study of OFX

Green Pre-Treatment Strategy Using Ionic Liquid-Based Aqueous Two-Phase Systems for Pesticide Determination in Strawberry Samples.

Pesticides used in agriculture can contaminate foods like fruits and vegetables, posing health risks to consumers and highlighting the need for effective residue monitoring. This study explores aqueous two-phase systems (ATPSs) comprising phosphonium or ammonium ionic liquids (ILs) combined with ammonium sulfate as an alternative pre-treatment method for extracting and concentrating the pesticides clomazone, pyraclostrobin, and deltamethrin from strawberry samples. Liquid-liquid equilibrium measurements for each ATPS were conducted, followed by extraction experiments to determine the most efficient systems for pesticide extraction. Results showed that all three pesticides migrated effectively to the IL-rich phase across the tested ATPSs. For the most promising system, tetrabutylphosphonium salicylate ([TBP][Sal]) with ammonium sulfate, extraction efficiencies for each pesticide exceeded 98% under optimized conditions for parameters such as pH, temperature, and ATPS composition. Application of this ATPS to strawberries resulted in significant pesticide preconcentration, reaching mg/L levels suitable for detection by liquid chromatography. The method's sustainability was supported by green chemistry metrics, with AGREEprep and AGREE scores of 0.68 and 0.55, respectively, underscoring its alignment with eco-friendly practices.

Facile and rapid preparation of fluorinated imprinted adsorbent for magnetic solid phase extraction of liquid-crystal monomers.

Anew fluorinated imprinted adsorbent (MIA) for magnetic solid phase extraction (MSPE) ofliquid crystal monomer (LCM) pollutantswas one-pot prepared within 3.5h using 4-[difluoro(3,4,5-trifluorophenoxy)methyl]-3,5-difluoro-4'-ethyl-biphenyl (DFBP) as template and 1H,1H,2H,2H-heptadecafluorodecyl acrylate/vinylanthracene as dual monomers. The structure, morphology, and magnetic properties of MIA fabricated were investigated by various characterization techniques. Under the optimal conditions the prepared MIA presented satisfactory specific recognition performance. The recognition factor and adsorption capacity towards DFBP were 2.7 and 15.9mg/g, respectively. The specific recognition behaviors of MIA/MSPE towards DFBP were surveyed by means of adsorption kinetics and adsorption isotherms. Combining MSPEwith HPLC coupled to a diode array detector (DAD), asensitive, reliable and anti-interference method for the monitoring of LCMs residuals in various environmental water and soil samples was established. The achieved enrichment factors were 132-248 and 96-204 in water and soil samples, respectively. The corresponding limits of detection were 0.0017-0.0051μg/L and 0.087-0.28μg/kg, respectively. Moreover, confirmatory experiments were adopted to inspect the accuracy of theestablished MIA/MSPE-HPLC/DAD approach. To the best of our knowledge, this is the first time that an imprinted material has been used forspecific isolation and capture of LCMs which have been classified as emerging organic pollutants.

Synthesis of a bimetal-organic framework-cobalt oxide nanoflowers (Ni/Co-MOF@Co3O4 NFs) for sensitive tebuconazole extraction from fruit juice and water samples using micro-solid phase extraction-HPLC-DAD

Tebuconazole (TBZ) is a widely used triazole fungicide that poses potential risks to human health and the environment due to its persistence in food and water. Effective monitoring of TBZ residues is crucial for ensuring food safety and environmental protection. This study presents a novel method for synthesizing Ni/Co-MOF@Co3O4 nanoflowers (NFs) and their application in extracting TBZ from water and fruit juice samples via micro-solid phase extraction (µ-SPE). Ni/Co-MOF@Co3O4 NFs was synthesized using the hydrothermal technique followed by calcination. The synthesized nanoflowers were characterized through SEM, XRD, and FT-IR analyses. Optimal extraction conditions were established at pH 8, using 10 mg of adsorbent, with adsorption and desorption times of 3 and 2 min, respectively. TBZ analysis was conducted using HPLC with a Poroshell 120 EC-C18 column and a diode array detector (DAD). The method demonstrates excellent recovery rates (90–102 %) and RSD% of 3.7 % in spiked fruit juice and natural water samples. The analytical performance showed a wide linear range (1–2000 µg L−1) with a high correlation coefficient (R2 = 0.9998), a detection limit of 4.0 ng L−1, and a quantification limit of 13.0 ng L−1. This approach is fast, simple, and highly sensitive, offering a reliable technique for detecting trace levels of TBZ in food and water environments.

Rapid and enhanced detection of sulfonamide antibiotic using task-specific ionic liquids nanoconfined in tunable nanoporous carbons.

The development of a novel multifunctional adsorbent for the sensitive detection and capture of antibiotic residues in environmental and food samples presents a significant challenge. In this study, we synthesized a pioneering nanocomposite, ILs@PC, by encapsulating task-specific ionic liquids (ILs) within nitrogen-doped porous carbon (PC) derived from metal-triazolate frameworks. This ILs@PC nanocomposite functions as a multifunctional adsorbent in dispersive solid-phase extraction (DSPE), enabling simultaneous sorptive removal, sensitive detection, and molecular sieve selection. The ILs@PC demonstrated enhanced adsorption efficiency and sensitivity for sulfonamide antibiotics (SAs) compared to the pristine PC, attributed to the nanoconfinement effect of the ILs and the influence of pore volume on this effect. When integrated with high-performance liquid chromatography (HPLC), the ILs@PC-based DSPE method achieved a detection limit of 0.75-1.88μgL-1 for SAs, along with satisfactory recoveries of 86.0%-111.9%. Additionally, a portable syringe device was developed to facilitate rapid on-site extraction and enrichment of SAs. The practicality of this method was validated through its successful application in detecting SAs in real samples, including lake water and milk. This approach highlights its potential for efficient and rapid monitoring of antibiotic residues in both environmental and food systems.

Monitoring of pesticide residues in Brazilian infant formulas using the suspect screening methodology by GC-HRMS

Monitoring of pesticide residues in Brazilian infant formulas using the suspect screening methodology by GC-HRMS

Monitoring of pesticide residues in some vegetables from locally markets in Gharbia governorate

Monitoring of pesticide residues in some vegetables from locally markets in Gharbia governorate

A simple lable-free aptasensor based on liquid exfoliated graphene modified electrode for chloramphenicol detection in milk

Antibiotic residues in animal derived foods considered as one of the most serious food contamination poses significant risks to human health. Conventional methods for antibiotic residue detection rely on expensive and bulky instruments, complicated sample pretreatment and time-consuming, thus limiting their applications. Consequently, developing miniaturized and low-cost analytical technology for ultrasensitive monitoring and accurate evaluation of antibiotic residues in foods is of great significance. Herein, a simple and label-free electrochemical sensing platform for the highly sensitive detection of chloramphenicol (CAP) in milk was demonstrated by employing aptamer specific for CAP as a biological recognition element and liquid exfoliated graphene (LEG) modified indium tin oxide electrode (LEG/ITO) as substrate. LEG is believed to be the most economic few-layer graphene with remarkable electrical properties and larger specific surface area not only promotes electron transfer but also provides a large number of binding sites for aptamers to be assembly immobilized via the π–π stacking of DNA bases. Under optimal experimental factors, the aptasensor displayed a wider linear range for detecting CAP (1 fM ∼ 100 nM), accompanied by a limit of detection (LOD) (1 fM), as well as satisfactory performance with specificity, reproducibility, and stability. In addition, the designed strategy allowed the direct analysis of actual milk samples and the recovery rates were from 97.92 % to 103.34 %, rendering a ideal sensing strategy for quantitative determination of various analytes in food by adapting the specific aptamer.

Assessing Pesticide Exposure and Regulatory Challenges in Malaysia: A Review of Population Monitoring, Food Residue, and Environmental Contamination

AbstractPesticide applications do not always stay confined to their target. Human exposure to pesticides can lead to various health effects, such as cancer, reproductive toxicity, and neurodegenerative disorders. For that reason, stringent regulations govern pesticide registration and application before they enter the market. This objective of this article is to review studies conducted in Malaysia related to human biomonitoring and pesticide residue monitoring in the environment and food with the aim to explore the extent and pathway of pesticide exposure among the population, which indirectly allows us to examine the effectiveness of pesticide regulatory systems. Articles published from 2010 until 2024 from ScienceDirect, Scopus, and Google Scholar were explored. In Malaysia, biomonitoring of pesticide is conducted sporadically by independent researchers and does not provide a comprehensive understanding of the population's exposure through various routes of exposures. Additionally, the effectiveness of environmental regulatory measures remains unclear because of lack of monitoring data available publicly for interpretation. Moreover, dietary exposure assessments of pesticide residues in food are conducted randomly in Malaysia. This approach contrasts with other countries where the Total Diet Studies comprehensively evaluate the entire population's exposure to pesticide residues through dietary pathways. In summary, there is a need for a more comprehensive and systematic study of Malaysia's pesticide regulatory system specifically through biological, environmental, and food monitoring. Understanding the effectiveness of current regulations in controlling pesticide exposure is vital not only for public health but also for overall environmental well-being of the nation.

Density tunable dispersive solid phase extraction of four organochlorine pesticides from edible oil sample using rhodamine B as a sorbent prior to GC-MS analysis

In this study, a new method was used to evaluate the levels of four organochlorine pesticides in edible samples. In this method, a density tunable dispersive solid phase extraction procedure was coupled with gas chromatography-mass spectrometry. Rhodamine B was used as a sorbent, which was distributed throughout the oil matrix with the aid of evaporation of methanol. This process enabled the possibility of effective extraction and preconcentration of the target analytes. To achieve this goal, several factors affecting the extraction efficiency, including the type and volume of diluent, the amount of rhodamine B, the volume of methanol, and the temperature of the ultrasonic bath were carefully evaluated. This method provided low detection limits (from 0.21 to 0.36 ng g-1), wide linear range (1.1-100 ng g-1) and acceptable extraction recoveries (64-72%) and enrichment factors (102-115). The precision of the method was evaluated by calculating the relative standard deviation, which ranged from 3.6 to 6.8% for intra- and 3.1 to 8.8% for inter-day precisions. The investigated method reduced the interference of the matrix and provided the possibility of quantitative determination of the studied organochlorine pesticides in various oil samples (canola, corn, sunflower, and olive). This method introduced a reliable analytical tool for the monitoring of the pesticide residues in different oil samples by providing capabilities such as simplicity, sensitivity, and compatibility with the environment.

Autonomous residual monitoring of metallurgical digital twins

The importance of digital twin maintenance has recently surfaced through findings from industrial applications. Changes in actual physical systems affect the resemblance between digital and physical twins, which can be seen in the continuously changing variation in model residuals. In this study, a method that autonomously updates itself is proposed for monitoring multivariate residuals. It is independent of the models used and monitors normalised residuals based on the squared Mahalanobis distance. The main novelty comes from the normalisation, which is done by using autonomously updated mean and standard deviation values of recent residuals. The method was studied by using an offline simulation model of a grinding circuit in a phosphate concentrator and an online adaptive digital twin model of a flotation circuit in a gold mine. Its performance was compared with conventional squared Mahalanobis distance and principal component analysis methods. The proposed method detected abnormal residual deviations and had low dependence on the characteristics of initial training data, defined by mean and standard deviation. After training with different data sets, the median monitored values of squared Mahalanobis distance remained consistently at values corresponding to 50–57% chi-square distribution probabilities, whereas without autonomous updating, the corresponding values were in the ranges of 3–55% and 39–88% showing inconsistent performance due to the varying distributions of training data sets. The proposed method with transferable and self-configuring properties can advance the online performance monitoring of digital twins.

Development and validation of a gas chromatography method for quantifying metham sodium in diverse plant origin foods

To ensure food safety and public health, it is essential to establish dependable methods for the qualitative and quantitative analysis of pesticide residues in plant origin foods. This study developed and optimized a gas chromatographic method using the QuEChERS approach for detecting metham sodium residues in 22 plant origin foods. The method was refined by adjusting inlet temperature and transformation conditions to effectively convert metham sodium into its primary metabolite, methyl isothiocyanate. Furthermore, parameters such as the extraction solvent type, volume, and purifying agent were systematically optimized. The method achieved a limit of quantification (LOQ) of 0.05 mg/kg, with a linear range from 0.025 to 1.0 mg/L and determination coefficients (R²) from 0.9892 to 0.9999. Recovery rates ranged from 82 % to 102 %, with relative standard deviations (RSDs) between 0.3 % and 6.8 %. Inter-laboratory validation, in accordance with EU SANTE guidelines, confirmed the method's accuracy and reliability. Validation results passed Cochrane's and Grubbs' tests, with repeatability RSDs between 0.70 % and 5.28 % and reproducibility RSDs from 3.62 % to 21.89 %. This method provides a reliable and effective approach for determining metham sodium residues, and addresses a critical gap in current analytical techniques, offering significant contributions to residue monitoring and food safety regulations.

Assessment of Pesticide Residues in Fruits and Vegetables Grown in Abidjan, Ivory Coast

Introduction: The presence of pesticide residues in primary and derived agricultural products raises serious health problems for consumers. The aim of this study was to assess the level of pesticide residues in commonly consumed vegetables. Methods: Pesticide residues were extracted from market garden products (Solanum lycopersicum, Capsicum sp, Cucumis sativus and Lactuca sativa) by the QuEchERS method and analyzed by high performance liquid chromatography (HPLC-UV) technique. Results: These analyzes made it possible to detect 32 pesticide residues. All market garden products contained pesticide residues, 12.82% of which exceeded the maximum residue limits (MRLs). The pesticide families found were triazines (34.34%), urea derivatives (31.25%), organophosphorus residues (9.37%), organochlorines (9.37%), triazinones (9.37%) and carbamates (6.25%). Among the market garden products, only lettuce was contaminated by residues from all families with concentrations of pesticide residues exceeding their limits of quantification at the level of 5 molecules: Chlorpropham (0.016 mg/kg), Linuron (0.02 mg/kg), Chlorfenvinphos (0.026 mg/kg) Parathion-ethyl (0.014) and Metolachlor (0.013 mg/kg) which is an organochlorine pesticide. Organochlorines are among the prohibited pesticides. Among agrochemicals used, some were not approved. Conclusion: The results indicate the presence of pesticide residues in commonly consumed vegetables and highlight the urgent need to develop comprehensive intervention measures to reduce the potential health risk to consumers. The need for regular monitoring of pesticide residues and raising farmers' awareness of better pesticide safety practices are actions to be taken for the health of consumers.

Low background dual-ligand Cu-MOF nanoprobe for plant tissue imaging and fast screening as well as sensitive detection of glyphosate in environmental samples

The monitoring of glyphosate residue in environmental samples is critically important due to its high environmental risk. Here, we reported a low background dual-ligand and fast response copper-based metal organic framework (Cu-MOF) nanoprobe for imaging glyphosate in plant tissue, rapid screening of glyphosate-contaminated samples, and sensitive detection of glyphosate in environmental samples. The Cu-MOF nanoprobe was prepared with 2-Aminoisophthalic Acid (AIA) and trimesic acid (H3BTC) as ligands, and Cu2+ as a metal node. Thanking to both ligand-to-metal charge transfer (LMCT) and photoinduced electron transfer (PET) effects, the fluorescence of ligand AIA could be fully quenched in Cu-AIA/BTC probe. Upon the addition of glyphosate, it competed with the ligands in Cu-AIA/BTC probe, causing the collapse of MOF structure and the release of ligand AIA with obvious fluorescence recovery. This nanoprobe exhibited a desirable linear response for glyphosate in the concentration range of 0.1–80 μM, with a low detection limit of 33 nM, much lower than the maximum contaminant level (4.1 μM) set by the U.S. Environmental Protection Agency (EPA). Furthermore, it was also successfully applied for plant tissue imaging, fast screening of glyphosate-contaminated samples and monitoring of the degradation of glyphosate on tea leaves and in soil, indicating the broad application prospect of the nanoprobe.