RESUMEN

Phoxim, extensively utilized in agriculture as an organothiophosphate insecticide, has the potential to cause neurotoxicity and pose human health hazards. In this study, an electrochemical enzyme biosensor based on Ti3C2 MXene/MoS2@AuNPs/AChE was constructed for the sensitive detection of phoxim. The two-dimensional multilayer structure of Ti3C2 MXene provides a robust framework for MoS2, leading to an expansion of the specific surface area and effectively preventing re-stacking of Ti3C2 MXene. Additionally, the synergistic effect of self-reduced grown AuNPs with MoS2 further improves the electrical conductivity of the composites, while the robust framework provides a favorable microenvironment for immobilization of enzyme molecules. Ti3C2 MXene/MoS2@AuNPs electrochemical enzyme sensor showed a significant response to phoxim in the range of 1 × 10-13 M to 1 × 10-7 M with a detection limit of 5.29 × 10-15 M. Moreover, the sensor demonstrated excellent repeatability, reproducibility, and stability, thereby showing its promising potential for real sample detection.

Asunto(s)

Técnicas Biosensibles , Técnicas Electroquímicas , Frutas , Oro , Nanopartículas del Metal , Nanocompuestos , Compuestos Organotiofosforados , Titanio , Oro/química , Técnicas Electroquímicas/instrumentación , Técnicas Electroquímicas/métodos , Nanocompuestos/química , Frutas/química , Nanopartículas del Metal/química , Técnicas Biosensibles/instrumentación , Compuestos Organotiofosforados/análisis , Titanio/química , Límite de Detección , Contaminación de Alimentos/análisis , Molibdeno/química , Insecticidas/análisis , Insecticidas/química , Residuos de Plaguicidas/análisis , Residuos de Plaguicidas/química

RESUMEN

A modified QuEChERS method was developed to determine multi-class pesticide and veterinary residues in aquatic products. Chitosan microspheres were conveniently synthesized and utilized as the cleanup adsorbent in the QuEChERS procedure, showcasing rapid filtration one-step pretreatment ability for the determination of drug multi-residues in aquatic products. Compared to conventional synthetic sorbents, chitosan microspheres not only have good purification performance, but also have renewable and degradable properties. This novel sorbent worked well in the simultaneous determination of 95 pesticides and veterinary drug residues in aquatic products after being combined with an improved one-step vortex oscillating cleanup method. We achieved recoveries ranging from 64.0% to 115.9% for target drugs in shrimp and fish matrix. The limits of detection and quantification were 0.5-1.0 and 1.0-2.0 µg kg-1, respectively. Notably, hydrocortisone was detected with considerable frequency and concentration in the tested samples, underscoring the necessity for stringent monitoring of this compound in aquatic products.

Asunto(s)

Quitosano , Peces , Microesferas , Espectrometría de Masas en Tándem , Drogas Veterinarias , Animales , Quitosano/química , Cromatografía Líquida de Alta Presión , Drogas Veterinarias/análisis , Drogas Veterinarias/aislamiento & purificación , Contaminación de Alimentos/análisis , Residuos de Medicamentos/análisis , Residuos de Medicamentos/aislamiento & purificación , Residuos de Medicamentos/química , Plaguicidas/aislamiento & purificación , Plaguicidas/análisis , Plaguicidas/química , Residuos de Plaguicidas/aislamiento & purificación , Residuos de Plaguicidas/análisis , Residuos de Plaguicidas/química , Adsorción , Extracción en Fase Sólida/métodos , Extracción en Fase Sólida/instrumentación , Contaminantes Químicos del Agua/aislamiento & purificación , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/análisis , Alimentos Marinos/análisis , Mariscos/análisis , Cromatografía Líquida con Espectrometría de Masas

RESUMEN

Spinetoram is one of the most extensively used insecticides globally and is a new spinosyn-based insecticide registered for direct treatment of Egyptian grapes. This work established and validated a developed method for determining spinetoram in grape berries and leaves using the QuEChERS coupled LC-MS/MS technique. The average recoveries ranged between 98.52-101.19% and 100.53-104.93%, with RSDs of 2.74-6.21% and 2.79-7.26% for grape berries and leaves, respectively. Spinetoram residues degraded in grape berries and leaves through a first-order kinetic, with an estimated half-life (t1/2) of 4.3 and 2.8 days in grape berries and leaves, respectively, and significant degradation (91.4-97.5%, respectively) after 14 days. Besides, the terminal residues of spinetoram detected in grape berries and leaves samples ranged between 0.017-0.077 mg‧kg-1 and 0.79-0.023 mg·kg-1, respectively, when applied two to three times at a single recommended rate, while it was varied between 0.026-0.44mg‧kg-1 and 0.79-0.023mg‧kg-1 when applied two to three times at a double recommended rate, respectively. A dietary risk assessment was conducted using scientific data from field trials, acceptable daily intake (ADI), and food consumption. It was determined that no noteworthy health hazards were connected to eating grape berries and leaves that had been treated with spinetoram since the risk quotients (RQs) were ≤ 0.4.

Asunto(s)

Insecticidas , Vitis , Vitis/química , Egipto , Medición de Riesgo , Insecticidas/análisis , Humanos , Estrobilurinas/análisis , Residuos de Plaguicidas/análisis , Frutas/química , Exposición Dietética/estadística & datos numéricos , Contaminación de Alimentos/análisis , Hojas de la Planta/química , Monitoreo del Ambiente , Macrólidos

RESUMEN

Consuming leafy vegetables with excessive thiophanate-methyl (TM) residue poses serious risks to human health. To realize rapidly and sensitively detecting TM in leafy vegetables, we developed a fluorescent probe based on zeolitic imidazolate framework-8-modified carbon dots using Hami melon as the green precursor (HM-CDs@ZIF-8). Meanwhile, the mechanism of HM-CDs@ZIF-8 for detecting TM was investigated and explained. The results of the performance tests showed that the prepared HM-CDs@ZIF-8 exhibited high sensitivity, excellent selectivity, robust anti-interference capability, reliable reproducibility and repeatability, and long-term stability. After optimization experiments, the fluorescence intensity of HM-CDs@ZIF-8 showed a strong linear correlation with the concentration of TM (0.00171-3.4239 mol/L) with a detection limit of 2.025 µmol/L. The HM-CDs@ZIF-8 was successfully applied to determine TM in spiked leafy vegetables with satisfactory recoveries of 96-105%. The relative standard deviations were in the range of 0.26-2.55%. The sensor has a promising application for detecting TM in leafy vegetables.

Asunto(s)

Carbono , Puntos Cuánticos , Tiofanato , Verduras , Verduras/química , Puntos Cuánticos/química , Carbono/química , Tiofanato/química , Tiofanato/análisis , Contaminación de Alimentos/análisis , Estructuras Metalorgánicas/química , Residuos de Plaguicidas/análisis , Residuos de Plaguicidas/química , Cucurbitaceae/química , Límite de Detección , Colorantes Fluorescentes/química , Espectrometría de Fluorescencia , Hojas de la Planta/química

RESUMEN

Drug residues that contaminate food and water represent a serious concern for human health. The major concerns regard the possible irrational use of these contaminants, since this might increase the amplitude of exposure. Multiple sources contribute to the overall exposure to contaminants, including agriculture, domestic use, personal, public and veterinary healthcare, increasing the possible origin of contamination. In this review, we focus on crop pesticides and veterinary drug residues because of their extensive use in modern agriculture and farming, which ensures food production and security for the ever-growing population around the world. We discuss crop pesticides and veterinary drug residues with respect to their worldwide distribution and impacts, with special attention on their harmful effects on human reproduction and embryo development, as well as their link to epigenetic alterations, leading to intergenerational and transgenerational diseases. Among the contaminants, the most commonly implicated in causing such disorders are organophosphates, glyphosate and antibiotics, with tetracyclines being the most frequently reported. This review highlights the importance of finding new management strategies for pesticides and veterinary drugs. Moreover, due to the still limited knowledge on inter- and transgenerational effects of these contaminants, we underlie the need to strengthen research in this field, so as to better clarify the specific effects of each contaminant and their long-term impact.

Asunto(s)

Desarrollo Embrionario , Fertilidad , Plaguicidas , Drogas Veterinarias , Humanos , Desarrollo Embrionario/efectos de los fármacos , Fertilidad/efectos de los fármacos , Exposición Dietética/efectos adversos , Animales , Residuos de Medicamentos/análisis , Epigénesis Genética/efectos de los fármacos , Residuos de Plaguicidas/análisis

RESUMEN

BACKGROUND: Although pesticides play an integral role in food security and preventing public health from vector-borne diseases, inappropriate handling and continual use of restricted organochlorine pesticides pose short- and long-term adverse effects and become public health concerns in the African region. This study aimed to determine the combined level of protective equipment use, management of empty pesticide containers, and leftover pesticide residues in the African region. METHODS: The preferred reporting items for systematic reviews and the meta-analysis protocol were used to carry out this study. The Scopus, PubMed, Web of Science, Google Scholar, DOAJ, and National Repository databases were searched for articles published between November 12, 2023, and January 2, 2024. The meta-analysis data were visualized using a forest plot. A random-effects model was applied when heterogeneity existed in pooled studies. Subgroup analysis of the data was performed based on the location where the study was conducted and the publication year. Meta-regression and sensitivity analysis were performed to evaluate the robustness of the pooled prevalence of studies. Publication bias was assessed using a funnel plot. The authors used the Joanna Briggs Institute Critical Assessment tool to determine the quality of the studies. RESULTS: In this review, 2174 articles were identified from the included electronic databases, 24 of which were included in the present study. The study revealed that the combined mean prevalence of wearing a mask, glove, boot/safety shoes, overall wear, and head cover accounted for 18% (95% CI: 11.9 to 26.1%, p < 0.001), 18% (95% CI: 11.7 to 26.9%, p < 0.001), 23% (95% CI: 15.7 to 33.3%, p < 0.001), 26% (95% CI: 16.2 to 38.7%, p < 0.001), and 14% (95% CI: 8.90 to 22.0%, p < 0.001), respectively. The prevalence of pesticides stored in the living room and pesticide containers used for different purposes was 51% and 26%, respectively. CONCLUSIONS: Poor pesticide safety practices were identified. A substantial proportion of the respondents reported storing pesticide residues in their living rooms, and the reuse of pesticide empty containers. Regional institutions should lead the designing of safety strategies to reduce the public health risks of pesticide exposure.

Asunto(s)

Plaguicidas , Salud Pública , Humanos , África , Residuos de Plaguicidas/análisis

RESUMEN

The application of agrochemicals in citrus fruits is widely used to improve the quality of crops, increase production yields, and prolong post-harvest life. However, these substances are potentially toxic for humans and the ecosystem due to their widespread use, high stability, and bioaccumulation. Conventional techniques for determining pesticide residues in citrus fruits are chromatographic methods coupled with different detectors. However, in recent years, the need for analytical strategies that are less polluting for the environment has encouraged the appearance of new alternatives, such as sensors and biosensors, which allow selective and sensitive detection of pesticide residues in real time. A comprehensive overview of the analytical platforms used to determine pesticide residues in citrus fruits and citrus-derived products is presented herein. The review focuses on the evolution of these methods since 2015, their limitations, and possible future perspectives for improving pesticide residue determination and reducing environmental contamination.

Asunto(s)

Citrus , Frutas , Residuos de Plaguicidas , Citrus/química , Residuos de Plaguicidas/análisis , Frutas/química

RESUMEN

The use of pesticides in viticulture may play a crucial role in ensuring the health and quality of grapes. This review analyzes the most common pesticides used, illustrating their classification and toxicity, and their variations throughout the winemaking process. Fungicides are generally harmless or mildly toxic, whereas insecticides are classified as either highly or moderately hazardous. Potential alternatives to synthetic pesticides in wine production are also reviewed, thereby including biopesticides and biological agents. Analytical methods for detecting and quantifying pesticide residues in wine are then described, including liquid chromatography and gas chromatography coupled with mass spectrometry. This review also discusses the impact of the winemaking process on pesticide content. Pesticides with strong hydrophobicity were more likely to accumulate in solid byproducts, whereas hydrophilic pesticides were distributed more in the liquid phase. Grape's skin contains lipids, so hydrophobic pesticides adsorb strongly on grape surfaces and the clarification has been shown to be effective in the reduction of hydrophobic compounds. Therefore, the final wine could have more quantities of hydrophilic pesticides. Alcoholic fermentation has been shown to be crucial in pesticide dissipation. However, pesticide residues in wine have been shown an antagonistic effect on yeasts, affecting the safety and quality of wine products. Therefore, proteomic and genomic analyses of yeast growth are reviewed to understand the effects of pesticides on yeast during fermentation. The last section describes new effective methods used in removing pesticides from grapes and wine, thereby improving product quality and reducing harmful effects.

Asunto(s)

Fermentación , Plaguicidas , Vitis , Vino , Vino/análisis , Plaguicidas/química , Plaguicidas/análisis , Vitis/química , Residuos de Plaguicidas/análisis , Residuos de Plaguicidas/química , Manipulación de Alimentos/métodos , Contaminación de Alimentos/análisis

RESUMEN

To investigate the safety of Indocalamu Iatifolius McClur leaves sold in the market, a study was conducted using Indocalamu Iatifolius McClur leaves randomly collected from an online store and a large supermarket. Acute toxicity experiments were performed on mice, and their body weight was monitored for 14 days after administration. After the observation period, blood samples were collected for biochemical analysis, and organ pathology was examined. Then, the content of copper (Cu), lead (Pb), cadmium (Cd), mercury (Hg), arsenic (As), and the residues of nine organochlorine pesticides in Indocalamu Iatifolius McClur leaves were measured according to the National Food Safety Standard (GB/T5009-2003) and the pesticide residue determination methods in the 2020 edition of the Chinese Pharmacopoeia. The results showed that the mice in the Indocalamu Iatifolius McClur leaves (online store) group experienced mortality and severe liver and lung damage. The levels of lead, cadmium, mercury, arsenic, and the nine organochlorine pesticides met the relevant standards and regulations. However, the copper content in the Indocalamu Iatifolius McClur leaves (online store) group was nearly 80 times higher than that in the supermarket group. Mice in the Indocalamu Iatifolius McClur leaves (supermarket) group remained healthy without any abnormalities, and the levels of harmful metals and organochlorine pesticides complied with the standards and regulations. The study suggests the need for regulatory policies and safety standards for the sale of Indocalamu Iatifolius McClur leaves.

Asunto(s)

Hidrocarburos Clorados , Residuos de Plaguicidas , Hojas de la Planta , Animales , Hojas de la Planta/química , Ratones , Hidrocarburos Clorados/toxicidad , Hidrocarburos Clorados/sangre , Hidrocarburos Clorados/análisis , Residuos de Plaguicidas/toxicidad , Residuos de Plaguicidas/análisis , Masculino , Metales Pesados/toxicidad , Metales Pesados/análisis , Femenino , Pruebas de Toxicidad Aguda

RESUMEN

Food safety is an important issue to protect humane health and improve the life quality. Hence, analysis of the possible contaminants in food samples is essential. A rapid and efficient vortexed-assisted dispersive µ-solid-phase extraction coupled with gas chromatography-mass spectrometry was proposed for simultaneous separation/preconcentration and determination of five commonly used organophosphorus pesticides. Reduced graphene oxide decorated NiCo2(OH)6 nanoflowers as a novel nanostructure was synthetized and introduced for separation of the target pesticides from the wheat flour, rice flour, and baby food cereal samples. The characterization of the nanoflowers was accomplished by SEM-EDX, XRD, and FT-IR techniques. The main factors including pH, the amount of nanoflower, the volume of sample solution, salt concentration (ionic strength), desorption conditions (i.e. desorption solvent type and volume, and desorption time) on the pesticides extraction efficiencies were inquired using matrixed match method. Applying the optimum conditions, the linearity of 0.100-500.000 µg kg-1, LODs and LOQs in the range of 0.03-0.04 µg kg-1 and 0.1 µg kg-1 for the studied food samples were obtained. The repeatability (intra-day precision (n = 5)) of ≤ 2.0 % and reproducibility (inter-day precision, days = 5, n = 3) of ≤3.1 % and were appraise at three concentration levels (10, 50 and 100 µg kg-1 of each analyte). High relative recoveries of 90.0-99.3 % ascertained high potential of the presented method for complex matrix analysis.

Asunto(s)

Grano Comestible , Harina , Grafito , Compuestos Organofosforados , Oryza , Extracción en Fase Sólida , Grafito/química , Oryza/química , Harina/análisis , Compuestos Organofosforados/análisis , Compuestos Organofosforados/aislamiento & purificación , Compuestos Organofosforados/química , Grano Comestible/química , Extracción en Fase Sólida/métodos , Alimentos Infantiles/análisis , Cromatografía de Gases y Espectrometría de Masas/métodos , Límite de Detección , Contaminación de Alimentos/análisis , Triticum/química , Plaguicidas/análisis , Plaguicidas/aislamiento & purificación , Plaguicidas/química , Nanoestructuras/química , Microextracción en Fase Sólida/métodos , Níquel/química , Residuos de Plaguicidas/análisis , Residuos de Plaguicidas/aislamiento & purificación , Reproducibilidad de los Resultados

RESUMEN

Thiacloprid, a hazardous neonicotinoid insecticide, prevalent in daily agricultural practices, raises concerns due to the harmful effects of its residues on food items, and on unintended organisms poses a significant threat to human health. Introduced in 1990, Thiacloprid have gained popularity for its perceived effectiveness and reduced risks to non-target animals. However, emerging research in recent years reports significant toxic effects of Thiacloprid on non-target species, spanning neurotoxicity, immunotoxicity, hepatotoxicity, nephrotoxicity, and reproductive issues. Mammalian studies, particularly involving rodents, reveal cognitive impairment, hippocampal damage, and hepatic abnormalities upon Thiacloprid exposure. Reproductive toxicity and DNA damage are imminent concerns, disrupting gestational epigenetic reprogramming and suggesting persistent effects on future generations. Genotoxic effects, Embryotoxic, and observed reproductive toxicity accentuate the need for caution in the utilization of Thiacloprid. This review highlights reported toxic effects produced by Thiacloprid in recent years, challenging the initial belief in its lower toxicity for vertebrates.

Asunto(s)

Insecticidas , Neonicotinoides , Residuos de Plaguicidas , Tiazinas , Neonicotinoides/toxicidad , Humanos , Animales , Tiazinas/toxicidad , Insecticidas/toxicidad , Residuos de Plaguicidas/toxicidad , Residuos de Plaguicidas/análisis , Piridinas/toxicidad

RESUMEN

Residues of pesticides in milk may pose a threat to human health. This study aimed to develop a liquid-phase microextraction (LPME) method using hexafluoroisopropanol (HFIP)-based supramolecular solvent (SUPRAS) for the simultaneous extraction and purification of four pesticides (boscalid, novaluron, cypermethrin and bifenthrin) in milk. Pesticides were extracted using SUPRAS prepared with nonanol and HFIP, and the extraction efficiency was analyzed. Results showed satisfactory recoveries ranging from 80.8%-111.0%, with relative standard deviations (RSDs) of <6.4%. Additionally, satisfactory linearities were observed, with correlation coefficients >0.9952. The limits of quantification (LOQs) were in the range of 1.8 µg·L-1-14.0 µg·L-1. The established method demonstrated high extraction efficiency with a short operation time (15 mins) and low solvent consumption (2.7 mL). The HFIP-based SUPRAS LPME method offers a convenient and efficient approach for the extraction of pesticides from milk, presenting a promising alternative to conventional techniques.

Asunto(s)

Contaminación de Alimentos , Microextracción en Fase Líquida , Leche , Solventes , Microextracción en Fase Líquida/métodos , Leche/química , Animales , Solventes/química , Contaminación de Alimentos/análisis , Residuos de Plaguicidas/aislamiento & purificación , Residuos de Plaguicidas/química , Residuos de Plaguicidas/análisis , Hexanoles/química , Bovinos , Plaguicidas/aislamiento & purificación , Plaguicidas/química , Plaguicidas/análisis , Hidrocarburos Fluorados , Propanoles

RESUMEN

Buprofezin (BUP) is an insect growth regulator widely used in agriculture to control hemipteran pests, particularly the melon aphid, Aphis gossypii, due to its efficiency and low toxicity. Although approved by the Chinese government, its maximum residue limit (MRL) in food is strictly regulated, and conventional techniques for detecting BUP have several limitations. Our study reports successful BUP detection using a supramolecular fluorescent probe DP@ALB, constructed with chalcone-based fluorescent dye DP and albumin as the host. The probe offers advantages such as low cost, visual signal output with high fluorescence color variation, rapid response, and high sensitivity. Additionally, portable test strips enable convenient on-site BUP detection and simplifying field monitoring of spiked real samples. The study achieves precise qualitative and quantitative BUP analysis in grape fruit, groundwater, and soil with satisfactory recoveries. Further, the biological applicability of sensor for the in vitro detection of BUP in L929 living cells was demonstrated. This research breakthrough overcomes the limitations of traditional analytical methods, offering an efficient and reliable approach for food and environmental monitoring and pesticide residue detection.

Asunto(s)

Técnicas Biosensibles , Contaminación de Alimentos , Teléfono Inteligente , Tiadiazinas , Técnicas Biosensibles/instrumentación , Técnicas Biosensibles/métodos , Contaminación de Alimentos/análisis , Tiadiazinas/química , Tiadiazinas/análisis , Residuos de Plaguicidas/análisis , Vitis/química , Colorantes Fluorescentes/química , Insecticidas/análisis , Animales , Límite de Detección , Frutas/química

RESUMEN

The use of pesticides has increased with the development of agriculture. However, due to the trace content and the matrix's inherent complexity in environmental water, development of rapid and sensitive detection method present significant challenges in the analysis of pesticide residues. The study synthesized magnetic graphene oxide (MGO) by combining superparamagnetic nanoparticles with the easy modification of graphene oxide (GO). Covalent organic frameworks (COFs) were then modified to have a large specific surface area. Finally, magnetic graphene oxide-based covalent organic frameworks, namely MGO-COFs, were obtained with a spherical structure and used as magnetic solid-phase extraction materials, which was successfully used to determine the seven pesticide residues in environmental samples in conjunction with high performance liquid chromatography. The method has a wide linear range for the tested pesticides, with satisfactory correlation coefficients (R ≥ 0.099) and low detection limits (0.3-1.21 µg L-1). The correlation coefficients for all seven pesticides were high (R2 ≥ 0.9996). The spiked recoveries, exhibiting a range of 91.3 to 109 %, demonstrated that the developed MGO-COF-MSPE-HPLC-UV method is simple, efficient, and suitable for the analysis and detection of seven pesticide residues in environmental water.

Asunto(s)

Grafito , Límite de Detección , Estructuras Metalorgánicas , Residuos de Plaguicidas , Extracción en Fase Sólida , Contaminantes Químicos del Agua , Grafito/química , Residuos de Plaguicidas/análisis , Residuos de Plaguicidas/aislamiento & purificación , Extracción en Fase Sólida/métodos , Contaminantes Químicos del Agua/análisis , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/aislamiento & purificación , Cromatografía Líquida de Alta Presión/métodos , Estructuras Metalorgánicas/química , Nanopartículas de Magnetita/química

RESUMEN

Quantitative detection of pesticide residues in food and environmental samples using an improved lateral flow immunoassay (LFIA) is of considerable importance for real-time analysis. This paper proposes a highly sensitive LFIA platform based on a hierarchical magneto-colorimetric compact. This compact serves as both the target magnetic enrichment substrate and a photosensitive label. Initially, a large porous dendritic silica template is prepared and doped with superparamagnetic ferric oxide nanoparticles (Fe3O4 NPs) and colloidal gold nanoparticles (AuNPs) at high densities within its vertical channels. The sequential assembly of central-radial channels allow for the three-dimensional integration of these two components, enabling independent control of their discrete functions without mutual interference. Following alkyl organosilicon encapsulation and silica sealing, the composite spheres are then applied in LFIA to detect chlorothalonil residues. Fe3O4 NPs enhance the binding efficiency to target analytes, while AuNPs amplify the signal, leveraging their high loading densities and robust optical properties. The developed LFIA platform exhibited a detection limit of 0.34 ng/mL for chlorothalonil and a linear range of 0.0085-824 ng/mL. The recoveries varied between 85.1 % and 103.1 %, and the relative standard deviations were 1.25%-8.84 %. This LFIA approach demonstrates high sensitivity, specificity, reproducibility and flexible detection modes, making it highly suitable for the on-site monitoring of pesticide residues.

Asunto(s)

Oro , Nitrilos , Residuos de Plaguicidas , Inmunoensayo/métodos , Residuos de Plaguicidas/análisis , Oro/química , Nitrilos/química , Límite de Detección , Nanopartículas Magnéticas de Óxido de Hierro/química , Nanopartículas del Metal/química , Nanopartículas de Magnetita/química

RESUMEN

Cucumber (Cucumis sativus L.) is the world's most widely consumed salad vegetable, and it is frequently treated with pesticides to prevent pest and disease outbreaks. Pesticide residues in food commodities impede trade and pose a major health risk. Prior to residue estimation, the QuEChERS approach was validated utilising criteria such as limit of detection, limit of quantitation, linearity, accuracy, and precision. The residues of carbendazim, cypermethrin, ethion, profenofos, quinalphos, and triazophos were examined using a Gas Chromatograph equipped with an Electron Capture Detector or a Flame Photometric Detector and a high-performance liquid chromatography coupled to a photo diode array. The initial deposits of carbendazim, cypermethrin, ethion, profenofos, quinalphos, and triazophos at the prescribed dose were 1.235, 0.407, 0.817, 0.960, 0.628, and 0.985 mg/kg, respectively, with a pre-harvest interval of 5.58-11.30 days. According to the consumer risk evaluation data, the Hazard Quotient is less than one, and the Theoretical Maximum Dietary Intake is less than the Maximum Permissible Intake and Maximum Residue Limit, both of which are considered safe for human consumption at the authorised dose.

Asunto(s)

Cucumis sativus , Contaminación de Alimentos , Organotiofosfatos , Residuos de Plaguicidas , Cucumis sativus/química , Residuos de Plaguicidas/análisis , Contaminación de Alimentos/análisis , Medición de Riesgo , Organotiofosfatos/análisis , Triazoles/análisis , Carbamatos/análisis , Piretrinas/análisis , Plaguicidas/análisis , Humanos , Exposición Dietética/estadística & datos numéricos , Monitoreo del Ambiente/métodos , Bencimidazoles , Compuestos Organotiofosforados

RESUMEN

A general strategy for qualitative screening and quantitative analysis of 403 pesticides in various fruits and vegetables was developed using ultrahigh-performance liquid chromatography (UHPLC) in conjunction with a Thermo Q Exactive Focus high-resolution mass spectrometer, relying on an executable compound database comprised of the exacted mass of precursor ions, retention times, and fragment ions. Taking advantage of the powerful separation capacity of UHPLC, an Orbitrap analyzer with high sensitivity in full scan mode and elevated mass resolution of product ions in the MS/MS mode, eight pairs of isomers and fifty-seven groups of isobaric compounds were selectively identified. The method was then systematically assessed and validated for eight fruits and vegetables, in terms of screening detection limit (SDL), matrix effects, recovery, and precision over 400 pesticides. The results showed that the SDLs of 68.0-84.4% for the pesticides were less than or equal to 10 µg kg-1 in the representative matrices, recoveries in the range of 60-120% accounting for 48.6-84.4% of all the targets at three lower fortified levels of 5, 20, and 50 µg kg-1 with a precision of less than 20% while the range of overall average recoveries for the majority of the pesticides were from 82.4% to 105.1% in the as-selected matrices with RSDs between 3.9% and 7.7%. Using this method, screening data from a survey of pesticide residues in 68 practical samples across 32 different matrix types provides scientific data for the inspection and supervision of pesticide residue safety of fruits and vegetables.

Asunto(s)

Frutas , Residuos de Plaguicidas , Verduras , Verduras/química , Frutas/química , Cromatografía Líquida de Alta Presión/métodos , Residuos de Plaguicidas/análisis , Espectrometría de Masas en Tándem/métodos , Contaminación de Alimentos/análisis , Límite de Detección , Reproducibilidad de los Resultados

RESUMEN

The presence of pesticide residues in waterbed sediments poses a significant concern for aquatic ecosystems' health. This study examined pesticide contamination in sediments of 38 water bodies, embedded in agricultural-dominated regions, across eight European countries. Three indicators were targeted: occurrence, type, and concentrations of multiple pesticide residues in sediments. 196 pesticide residues (including degradation products) were tested in the sediment samples. The analytical results showed that only one sample was 'pesticide-free', three samples contained a single pesticide residue, and the remaining 34 samples contained mixtures of residues. Overall, 99 different residues were found in the sediments, with a maximum of 48 in a single sample. Twenty-seven out of the 99 detected residues were not approved for agricultural use at the time of sampling. The numbers of detected residues and pesticide levels varied among countries. AMPA, glyphosate and DDTs were the most common residues in sediment samples with frequencies of 76, 61, and 52%, respectively. The sediments from the Czech Republic had the highest pesticide concentrations, with total pesticide concentrations ranging between 600 and 1200 µg kg-1. The lowest total pesticide concentrations were found in Slovenia, Switzerland, Croatia, and Denmark, ranging between 80 and 120 µg kg-1. Sediments presented a mix of non-persistent and persistent compounds. Twelve of the detected pesticides are very persistent/stable in sediments, raising concerns about the long-term impacts of pesticides. Our study on the distribution of pesticide residues in European sediments provides valuable insights into the extent of pesticide contamination and possible risks of pesticides to water bodies' health. It also underlines the need for monitoring, research, and policy efforts to mitigate the impacts of pesticides, and to evaluate potential risks of re-use of dredged sediments.

Asunto(s)

Monitoreo del Ambiente , Sedimentos Geológicos , Residuos de Plaguicidas , Contaminantes Químicos del Agua , Sedimentos Geológicos/análisis , Sedimentos Geológicos/química , Residuos de Plaguicidas/análisis , Europa (Continente) , Contaminantes Químicos del Agua/análisis

RESUMEN

In this paper, we present analytical methodologies for the determination of the thiazolidine fungicide flutianil (trade name GATTEN) and its primary metabolite OC56635 in hemp cannabis matrices. A total of nine crop matrices were tested: whole seed, fiber, flower buds, hemp hearts, hemp seed oil, hemp meal, hemp flour, ethanol extracted CBD resin (CBD-E), and supercritical CO2 extracted CBD resin (CBD-C). Processing of the CBD-E and CBD-C crop fractions was carried out in-house using methods detailed herein. Field sample analysis utilized sequential extractions, stacked solid phase extraction (SPE) column cleanups, and evaporation to prepare the samples for LC-MS/MS quantitation. Method validations for each fraction were carried out using untreated hemp matrices over a minimum of three levels, with lowest levels of method validation (LLMV) of 0.010 µg/g for all fractions except the CBD resins, for which LLMV was 0.020 µg/g. Flutianil-treated samples from nine field sites were collected from several crop production regions and analyzed to determine the distribution of incurred flutianil and OC56635 residues within the different hemp matrices. This data was generated in support of nationwide registration with the United States Environmental Protection Agency (USEPA).

Asunto(s)

Cannabis , Fungicidas Industriales , Espectrometría de Masas en Tándem , Cannabis/química , Espectrometría de Masas en Tándem/métodos , Fungicidas Industriales/análisis , Fungicidas Industriales/química , Residuos de Plaguicidas/análisis , Cromatografía Líquida de Alta Presión/métodos , Extracción en Fase Sólida/métodos , Contaminación de Alimentos/análisis , Semillas/química , Cromatografía Líquida con Espectrometría de Masas

RESUMEN

Grapes are among the most popular fruits globally, and insecticides are commonly used on grape farms. Sulfoxaflor, a novel sulfoximine insecticide that works against various insect pests, is extensively used in Egypt. Our field trials assessed the dynamics and final residues of sulfoxaflor in grapes and grape leaves grown in Egyptian environments with different application rates, including worst-case scenarios. A QuEChERS-based method with LC-MS/MS was used to analyze residues of sulfoxaflor in grapes and grape leaves. The limit of quantification (LOQ) was validated at 0.01 mg‧kg-1. Sulfoxaflor residues are degraded in grapes and grape leaves according to a first-order kinetic model, with an estimated half-life (t1/2) of 7.04 and 7.7 days, respectively, and considerable degradation (74.68 and 72.16%, respectively) after 14 days. The final residues in grapes and grape leaves were below the Codex or EU maximum residue limit (MRL) (2 mg‧kg-1) after 3 days of the recommended and high application rates. The findings showed that grapes and leaves treated with sulfoxaflor at the recommended rate are safe for humans 3 days after two or three consecutive treatments with intervals of 14 days. The current study should pave the way for implementing safe and appropriate sulfoxaflor use in grapes and grape leaves in Egypt.

Asunto(s)

Compuestos de Azufre , Vitis , Vitis/química , Egipto , Medición de Riesgo , Compuestos de Azufre/análisis , Piridinas/análisis , Residuos de Plaguicidas/análisis , Insecticidas/análisis , Humanos