Imidacloprid Residues Research Articles

Simple high-temperature annealing affords commercial carbon cloth with enhanced electrochemical performance for highly sensitive detection of imidacloprid

Imidacloprid (IDP) residue in modern agricultural production seriously endangers human health and environmental safety. The establishment of a rapid and efficient method for the detection of IDP residue can effectively prevent its harm to human health. Herein, we demonstrate the carbon cloth (CC) prepared by a high-temperature annealing strategy possesses enhanced electrochemical performance, which could be directly used in electrochemical IDP sensing. Annealed carbon cloth (ACC) is endowed with higher defects, rougher surfaces, more functional groups, more hydrophilic surface, and increased ion-accessible surface area. Furthermore, the ACC electrode shows superior electrocatalytic reduction activity towards IDP, possessing a wide linear range of 5–100 μM, a low detection limit of 0.04 μM, and high sensitivity of 35.58 μA mM−1 cm−2. Meanwhile, this sensor can be applied for sensing IDP in grapes and apples with a good recovery of 96.8–104.1%. Compared with other modified electrodes, the ACC electrode has the advantages of no binder, no complicated modification, excellent detection effect, low cost, and easy large-scale production. Consequently, this work designs a self-supporting metal-free electrode with high electrochemical performance, providing a new idea for the development of environmentally friendly IDP sensors.

Residual determination of spirotetrament and imidacloprid in onion and tomato crop by mass spectrometery

ABSTRACT Persistence of spirotetramat and imidacloprid residues on tomato and onion after three applications of a combination formulation, spirotetramat 12% + imidacloprid 12%, @ 625 and 1250 mL ha−1 is reported. An easy and simple methodology was standardised for the extraction of residues in tomato, onion and soil followed by estimation and confirmation on LC-MS/MS using C18 column by keeping the positive mode of electrospray. The methodology was validated for selectivity, linearity, precision, repeatability, reproducibility and its limit of detection and quantification. The limit of quantification (LOQ) was worked out to be 0.05 mg kg−1. The results of recovery studies were consistent and more than 80% in all the matrices. No residues above LOQ were detected in tomato sample after 3rd day and after 7th day for onion samples.

Determination of insecticide residues in soils from Troia agricultural fields by the QuEChERS method

Extensive and misuse of pesticides can cause to toxicity to humans and pollution in the environment. The primary objective of this study was to determine insecticide load of agricultural soils of Troia, located in Troia National Park of Çanakkale Province (Türkiye) by the QuEChERS method. For method verification, blank soil samples were spiked at two levels of pesticides. The overall recovery was 84.8% with a relative standard deviation of 13.0% (n = 230), with the values within acceptable recovery (60-140%) and repeatability (≤20%) ranges set by SANTE. Forty-nine soil samples were collected in the study area in 2020. Thirty-six samples had insecticide residues at varying concentrations. Overall, 23 insecticide residues were detected at different frequencies. The most frequent pesticides were: chlorantraniliprole> imidacloprid> pyridaben> clothianidin> indoxacarb (in decreasing order). Mean concentration of insecticide residues in soils varied between 0.99-77.7 µg/kg. Imidacloprid residues were detected in all fields, except cabbage fields. The highest imidacloprid concentration (23.3 µg/kg) was detected in pepper fields. Imidacloprid was detected in 21 samples with a mean concentration of 6.20 µg/kg. Persistent insecticides with the long half-lives, such as chlorantraniliprole, imidacloprid, and clothianidin, were detected in almost all samples.

Rapid screening of imidacloprid residue in grains and medicinal herbs: A newly designed hapten and monoclonal antibody

Three different imidacloprid hapten structures were designed to conjugate with proteins (bovine serum albumin, BSA; ovalbumin, OVA; keyhole limpet hemocyanin, KLH) for screening the optimal immunogen and coating antigen. Among these, an unreported antigen (hapten 6-KLH) was selected as the optimal immunogen and coating antigen. In addition, an imidacloprid-specific and high titer monoclonal antibody (IMIB7C3) was obtained by using the above-selected immunogen. A sensitive ic-ELISA (indirect competitive enzyme-linked immunosorbent assay) with a half-maximal inhibitory concentration (IC50) of 1.3 ng mL−1 was established by using the IMIB7C3 antibody (only 1.2 ng per well) to detect the residues of imidacloprid in grains (wheat and maize) and different herbs (Notoginseng radix et rhizoma, Dioscoreae rhizoma, Lonicerae japonicae flos, Astragali radix, Jujubae fructus). The detection results of real samples by the developed immunoassay were confirmed by liquid chromatography-tandem mass spectrometry (LC–MS/MS), which proved the accuracy and reliability of the established ic-ELISA. These results indicate that the proposed ic-ELISA method is suitable for rapid and high-throughput detection of imidacloprid residues in agricultural products and medicinal herbs. Furthermore, a quantitative risk assessment was conducted for Lonicerae japonicae flos based on the detection results, which indicates an acceptable risk to human health after the intake of Lonicerae japonicae flos polluted by imidacloprid.

Detection and Concentration of Neonicotinoids and Other Pesticides in Honey from Honey Bee Colonies Located in Regions That Differ in Agricultural Practices: Implications for Human and Bee Health.

This is a preliminary study conducted to analyze the presence and concentration of pesticides in honey obtained from honey bee colonies located in two regions with managed ecosystems that differ in the intensity and technification of agricultural practices. Fourteen pesticides at variable concentrations were detected in 63% of the samples analyzed. The pesticides most frequently found at higher concentrations were insecticides (neonicotinoids, followed by organophosphates), herbicides, and fungicides. The number, frequency, and concentration of pesticides were higher in samples collected from hives located where intensive and highly-technified agriculture is practiced. Forty-three percent of the samples from that zone had residues of imidacloprid, compared with only 13% of the samples from the less-technified zone. Furthermore, 87.5% of those samples had imidacloprid concentrations that were above sublethal doses for honey bees (>0.25 ng/g) but that are not considered hazardous to human health by the European Commission. The results of this study suggest that honey can be used as a bioindicator of environmental contamination by pesticides, which highlights the need to continue monitoring contaminants in this product to determine the risks of pesticide impacts on pollinator health, on ecosystems, and on their potential implications to human health and other non-target organisms.

Study of Imidacloprid, Azoxystrobin and Difenoconazole Residues and their Biochemical effects on Cucumber

Study of Imidacloprid, Azoxystrobin and Difenoconazole Residues and their Biochemical effects on Cucumber

Physiological Responses of the Firefly Pyrocoelia analis (Coleoptera: Lampyridae) to an Environmental Residue From Chemical Pesticide Imidacloprid.

Imidacloprid, a neonicotinoid insecticide, is widely applied to control insect pests across a broad spectrum. Though the impact of residues from this chemical pesticide on non-target organisms in the field has been reported, it was not well characterized across a wide range of ecosystems, especially for some species considered as environmental indicators that live in forests. The effects of sublethal dose of imidacloprid on firefly, Pyrocoelia analis, were analyzed physiologically and biochemically in this study to better understand the impact of chemical pesticide application on environmental indicators such as fireflies. After imidacloprid treatment, the midgut tissues of the larva presented an abnormal morphology featured as atrophy of fat body cells, shrinking cells, and the destruction of a midgut structure. The activities of antioxidant enzymes, superoxide dismutase, catalase, and peroxidase were noticeably increased during early exposure to sublethal imidacloprid and then decreased at later stages. The malondialdehyde content significantly increased after 12 h of exposure to imidacloprid compared with the control. Similarly, the enzyme activities of polyphenol oxidase and acetylcholinesterase were increased after the imidacloprid treatment and then decreased at the later stage. In summary, a sublethal dose of imidacloprid caused destructive change in the tissue structure, and this damage was followed by an excessive reactive oxygen species that could not be eliminated by antioxidant enzymes. Our results indicated that the residues of imidacloprid might cause severe toxicity to non-target insects in the environment even far away from the agro-ecosystem where the chemicals were applied.

Effect of Chinese steamed bun and bread processing on pesticide residues in wheat flour

The changes of five pesticides including imidacloprid, triadimefon, fenitrothion, chlorpyrifos-methyl, and chlorpyrifos in wheat flour during Chinese steamed bun and bread processing were systematically investigated. The pesticide residues were determined by high performance liquid chromatography coupled with diode array detector. Dough mixing step in both Chinese steamed bun and bread processing reduced the concentration of five pesticide residues significantly by 33 to 46%. It was mainly attributed to the increase of moisture content in mixed dough during this step. The reduction of pesticides in fermenting step varied from 2 to 22% in Chinese steamed bun and bread processing. Resting step in both Chinese steamed bun and bread processing has little effect on the pesticide residues with the reduction from 2 to 8%. The five pesticides have different behaviours in steaming step of Chinese steamed bun processing and in baking step of bread processing. During the steaming step, only the concentrations of triadimefon and imidacloprid residues in crust were increased by 52 and 1%, the others in crust and in crumb of Chinese steamed bun were decreased by 4 to 38%. After the baking step, the concentrations of triadimefon and imidacloprid residues in crust, and the triadimefon residue in crumb of bread were increased by 65, 83, and 14%, respectively, the others were all reduced. The processing factors (PFs) for triadimefon and imidacloprid in crust in the steaming and baking steps, for triadimefon in crumb in the baking steps were greater than 1, and the others were all less than 1. Overall, this study provides important references for monitoring pesticide residues in the processing of wheat flour products. The PFs obtained could be helpful for the risk assessment of pesticides in wheat flour products.

Effect of decontamination and processing on insecticide residues in grape (Muscat Hamburg).

Field and laboratory experiments were conducted to study the effect of simple decontamination methods and processing on imidacloprid, dimethoate, and emamectin benzoate residues in grapes and their processed products by liquid chromatography-mass spectrometry. Among the decontamination methods evaluated, washing with NaCl (2%) solution was effective for reducing imidacloprid (77.55%), dimethoate (83.27%), and emamectin benzoate (77.28%) residues in mature grapes. No metabolites (omethoate and 6-chloronicotinic acid) were detected in both decontamination and processing studies. The grapes were processed into various products, including fresh juice, squash, and raisin, following the standard effective steps for each product. Washing with NaCl (2%) solution for decontamination was included as an additional step in the standard protocol and resulted in substantial removal of surface residues of the selected insecticides. The processing factor calculated was less than one for all the products.

Residue and Risk Assessment of Imidacloprid and Chlorantraniliprole in Open Field and Greenhouse Celery

The residue levels and risk assessment of imidacloprid (IMI) and chlorantraniliprole (CAP) in celery grown under open field and greenhouse cultivation were investigated. Both pesticides were used through foliar application and soil drench application at the recommended dose (RD) and 10-fold recommended dose (10RD). The half-lives of IMI and CAP in celery were 1.9 to 5.8 days and 4.3 to 6.5 days after foliar application, respectively, and the dietary risk quotients of IMI and CAP were 14.8 to 18.3% and 1.0 to 1.2%, respectively. For soil drench application, the half-lives of IMI and CAP in soil were 17.5 to 28.5 days and 15.1 to 23.7 days, respectively. Celery plants were able to absorb both insecticides from the soil. The highest concentrations of IMI in celery plants were 0.12 to 0.24 mg kg-1 (RD) and 0.34 to 0.39 mg kg-1 (10RD), and those for CAP were 0.0081 to 0.015 mg kg-1 (RD) and 0.028 to 0.057 mg kg-1 (10RD). Based on the highest residues of IMI and CAP in celery, the dietary risk quotients of IMI and CAP were 15.0% (RD) to 15.6% (10RD) and 1.0% (RD and 10RD) after soil drench application, respectively. The observed bioconcentration factors were 1.38 to 2.11 (IMI) and 0.35 to 0.48 (CAP), indicating that celery accumulated IMI more easily than CAP. The foliar and soil applications of IMI and CAP in celery at the RD and 10RD do not pose a safety risk to consumers.

Dissipation and risk assessment of Solomon (300 OD), a combination product of beta-cyfluthrin and imidacloprid in lemon and onion samples

ABSTRACT Supervised field trials were conducted to study dissipation of combination product of beta-cyfluthrin and imidacloprid (Solomon) in various samples of lemon and onion. The pesticides were extracted and analysed using QuEChERS (with some modifications) based methods after validation of the method. Linearity, accuracy and precision data showed that the results were in the acceptable range as per SANTE 2019. The results of dissipation revealed that the initial accumulation of beta-cyfluthrin was 0.6 and 1.1 mg kg−1 in lemon and 0.24 and 0.97 mg kg−1 in onion samples at standard and double dose respectively. The residues of imidacloprid were 2.61 and 4 mg kg−1 in lemon and 0.36 and 0.53 in onion at two doses. The residues of beta-cyfluthrin followed first order dissipation in both the crops at standard dose and showed biphasic dissipation in double dose in both lemon and onion samples. Imidacloprid followed first-order dissipation in lemon in both the doses. Half-life of beta-cyfluthrin ranged from 3.6 to 23.2 days in lemon samples and that of imidacloprid was 15.1 and 21.5 days in two different doses. In onion the half-life ranged from 2.1 to 4.0 for beta-cyfluthrin and 2.8 to 5.2 days for imidacloprid in different doses. Theoretical maximum residue concentration (TMRC) was always less than maximum permissible intake (MPI) in all the samples suggesting that the use of combination product is safe.

Monitoring and dietary risk assessment of pesticide residues in brinjal, capsicum, tomato, and cucurbits grown in Northern and Western regions of India

The present study monitored pesticide residues in 2319 samples of fruiting vegetables namely, tomato (416), capsicum (363), brinjal (448), and cucurbits (1092) grown in the Northern and Western regions of India. The samples were extracted using QuEChERS method and analyzed for the residues of 155 multi–class pesticides by gas chromatography–mass spectrometry and/or liquid chromatography–tandem mass spectrometry. The residues of 56 pesticides were detected in vegetables with the highest percentage of positive samples in capsicum (69.7%) followed by brinjal (36.6%), cucurbits (34%), and tomato (30.3%). Residues of acetamiprid, profenofos, imidacloprid, metalaxyl, chlorpyrifos, and tebuconazole were most frequently detected. Dietary risk due to pesticide residues was evaluated using food consumption data, acceptable daily intake (ADI), and safety indices such as hazard quotient (HQ) and hazard index (HI) considering lower bound (LB) and upper bound (UB) scenarios in adults and children. The HQs and HIs did not exceed unit value (HQ, HI < 1) for both adults and children, indicating that the level of pesticide residues in these fruiting vegetables does not pose any appreciable risk to the consumers.

Residue, Dissipation Pattern, and Dietary Risk Assessment of Imidacloprid in Chinese Chives

The demand for Chinese chives is growing as they are also rich in vitamins, fiber, and sulfur nutrients. Chinese chives should be sprayed with imidacloprid to control pests and diseases to safeguard their yield and to meet the demands of East Asian consumers for Chinese chives. Overspraying of imidacloprid can lead to residues in Chinese chives, posing a severe risk to human health. To reduce the harmful effects of imidacloprid residues on humans, we investigated the imidacloprid dissipation pattern and the final residue on Chinese chives using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Good linearity (R2= 0.9988), accuracy (expressed as recovery % of 78.34–91.17%), precision [expressed as relative SDs (RSDs) of 0.48–6.43%], and sensitivity [a limit of quantification (LOQ) ≤ 8.07 × 104 mg/kg] were achieved. The dissipation dynamics were consistent with the first-order kinetics, with a half-life of 2.92 days. The final residual levels on Chinese chives were 0.00923–0.166 mg/kg, which is lower than the maximum residue limits (MRLs) of 1 mg/kg for imidacloprid on Chinese chives. A risk assessment index of <1 indicates that Chinese chives are safe for consumption.

The Estimation of Lipid Peroxidation and Osmotic Fragility of Human Red Blood Cell Induced by Pesticides Residues Detected in Some Vegetables Crops

Background: Many studies have reported the contamination by pesticides in a variety of matrices, such as food, water and soil, which despite their use, health risk of pesticides residues on food and in drinking water for the general population has been raised. The aim of this study is to quantify the pesticides residues of Abamectin and Imidacloprid in some vegetable samples; to study the in vitro effects of the both pesticides on the lipid peroxidation and hemolytic activity and finally, based on the mathematical models we estimate the values equivalent to the concentrations of pesticide residues detected in the vegetable samples. Methods: The extraction of pesticide residues from vegetable samples we use the FaPEx kits. Agilent Technologies 1260 infinity high performance liquid chromatography having UV/visible detector was used for the identification and quantification of pesticides residues. The results of this study proved the presence of pesticide residues in vegetable tested with higher values comparing with their corresponding MRLs. Result: The mean of the quantity of Abamectin detected in the vegetables samples ranged from 1.93 to 4.11 mg/kg for the green pepper (Capsicum annuum spp) and courgette (Cucurbita pepo), respectively. In addition, the Imidacloprid is just detected in the cucumber (Cucumis sativus) samples and the mean value of quantity is 24.09 mg/kg and corresponding MRL is 0.05 mg/kg. The in vitro study of the effects of the both pesticides on lipid peroxidation and hemolytic activity demonstrate significant effects of the different concentrations of the both pesticides on the both activities. The estimation by mathematical models of malondialdehyde quantity and hemolytic activity equivalent to the concentrations of the pesticides residues detected in vegetables samples proved the non-toxicity effects of these residues.

Degradation of Imidacloprid Residue in Cabbage (Brassica oleracea) Using Advanced Oxidation Processes and Its Analyzing by Spectrophotometer and HPLC

Imidacloprid is a synthetic pesticide used to kill and control insects by cabbage farmers. Consuming cabbage contaminated with imidacloprid can cause health problems such as chronic kidney, reproductive disorders and cancer. The parameters for degradation of imidacloprid residue in cabbage were processing time (5, 10, 15, 20, and 25 min), water volume (50, 100, 150, and 200 mL), and sample mass (25, 50, 75, and 100 g). Degradation of imidacloprid residue in cabbage using Advanced Oxidation Processes (AOPs) methods such as ozonolysis, sonolysis, and sonozolysis were compared. Methods of ozonolysis, sonolysis, and sonozolysis have performed using an ozonicator (ozone dose: 400 mg h-1), sonicator (35 kHz), and a combination of both. Using spectrophotometers UV-Vis and High-Performance Liquid Chromatography (HPLC) measurements showed a decrease in imidacloprid concentration after degradation. The degradation percentage of the imidacloprid residue with ozonolysis was higher than that of sonolysis and sonozolysis. The percentage of imidacloprid degradation by ozonolysis in 50 g cabbage at 100 mL of water increased to 82.53% for 15 min. The HPLC chromatogram showed no new peaks that formed after degradation. The imidacloprid residue’s degradation kinetics were then investigated. For all AOPs methods, the kinetic analysis demonstrated that imidacloprid degradation fit within a first-order kinetic model. The kinetic data showed that ozonolysis degraded imidacloprid with a half-life (t1/2) of 15.22 min, shorter than sonolysis and sonozolysis.

Validation of LC-MS/MS method for simultaneous determination of chlorpyrifos, deltamethrin, imidacloprid and some of their metabolites in maize silage

In this study, a validation of a multi-residue analysis method was performed for the simultaneous analysis of chlorpyrifos (CHL), deltamethrin (DEL) and Imidacloprid (IMI) residues and some of their metabolites in maize silage, by LC MS/MS. Extraction was conducted with acetonitrile acidified with 1% acetic acid. To avoid the matrix effect, a matrix matched calibration was used. The method was validated according to the SANTE/12682/2019 Guidelines. Selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), trueness (recovery %) and precision (intra-day and inter-day) parameters were evaluated in line with the SANTE document. The linearities of all compounds were quite confident (R2≥ 0.98) and no interference was observed. The LOD and LOQ values were between 2.76 µg kg−1 to 53.61 µg kg−1 and 9.19 µg kg−1 to 178.71 µg kg−1, respectively. The recovery, repeatability RDSr and reproducibility RDSR values of compounds were calculated between 93.7–109.2%, 1–15%, and 1–13%, respectively. Consequently, results obtained with the evaluation of all parameters were found to be compatible with the SANTE validation criteria, so the method was reliable, effective and easy to use for the detection of insecticides and metabolites in maize silage with LC MS/MS.

Highly selective fluorescence probe for imidacloprid measurement based on fluorescence resonance energy transfer

Herein, a fluorescent probe was investigated for the detection of imidacloprid based on the fluorescence resonance energy transfer (FRET) between two carbon-based quantum dots, namely graphene- and carbon quantum dots (GQDs/C-dots). In an HAc-NaAc buffer solution at pH = 5.0, an effective FRET occurred between the GQDs and C-dots, significantly enhancing the C-dot fluorescence. When imidacloprid was added to the FRET system, the fluorescence intensity of the C-dots was quenched in a linear imidacloprid concentration-dependent manner, which allowed for the establishment of a new method for the determination of imidacloprid by GQD/C-dot FRET. Under optimised experimental conditions, the linear range of imidacloprid was 5–4000 × 10−9 mol L−1, with a correlation coefficient r and a detection limit of 0.998 and 8.23 × 10−10 mol L−1, respectively. This method was applied to the detection of imidacloprid residues in real samples, and a satisfactory recovery rate of standard additions was found between 93.0% and 105.6%.

Dissipation and dietary risk assessment of imidacloprid and spiromesifen in brassica and fruiting vegetables following good agricultural practices

Field trials were conducted to study dissipation of imidacloprid and spiromesifen from vegetable and to carry out risk assessment. Method validation parameters were within the acceptable range with limit of quantitation (LOQ) of 0.05 mg kg−1 for both the pesticides. Two foliar sprays of imidacloprid (Confidor 17.8 SL) @ 20 and 40 g ai ha−1and spiromesifen (Oberon 22.9 SL) @ 96 and 192 g ai ha−1 were applied at an interval of 10 days. The residues of imidacloprid were below LOQ (0.05 mg kg−1) after 1 day in fruiting vegetables and on 5 to 7 days in other vegetables. Residues of spiromesifen reached below LOQ (0.05 mg kg−1) on 10 to 20 days. Halflife ranged from 1.4 to 3.9 for imidacloprid and 2.3 to 6.7 days for spiromesifen. Hazard Quotient (HQ) was <1, suggesting that it is safe to use imidacloprid and spiromesifen in/on vegetable crops.

Safety of foods sold in street fairs: analysis of pesticide residues in lettuce (Lactuca sativa L.)

Pesticides are chemical contaminants that can be found in food. Those with the greatest residual representation include insecticides, fungicides, and herbicides. The objective of this study was to analyze the presence of pesticide residues in lettuce (Lactuca sativa L.) sold at street fairs. This was a quantitative, cross-sectional study, carried out in street fairs in Chapecó, state of Santa Catarina, with producers of fresh vegetables, and consumers, and also analyzed pesticide residues in lettuce from conventional and organic cultivation. Data were collected using a semistructured questionnaire, administered to all producers, and a sample of consumers. Pesticide residues were analyzed in lettuce as it is the most purchased food by consumers. Pesticides surveyed included azoxystrobin, deltamethrin, imidacloprid, and glyphosate, as they are the most frequently applied on farms, and in cultivation of vegetables. Of the 67 vendors active in the seven street fairs, 30 were vegetable and fruit producers, and of these, 17 were conventional producers and 13 were organic farmers. The analysis of pesticide residues in lettuce from conventional production showed residues of azoxystrobin and imidacloprid, but below the maximum residue limits allowed by Anvisa. In samples of organic lettuce, residues of the analyzed pesticides were not detected. From the analysis of residues in lettuce, it is inferred that the food is safe in terms of the pesticides analyzed and that municipal public policies should prioritize systematic monitoring to ensure food safety and encourage the production of organic food.

A Fast, Sensitive and Validated Analytical Method for Quantitation of Imidacloprid Pesticide Residual in Mangifera indica Matrix by LC-Tandem Mass Spectrometry (LC-ESI-MS/MS)

An accurate and precise analytical method was performed for the quantitation of imidacloprid pesticide residue in the matrix of Mangifera indica (alphonso), specific species of Indian mango of Valsad District, Gujarat. The validation of the analytical technique was carried out using UPLC-ESI-MS/MS and was done in accordance with the regulatory recommendations. The projected technique is based on QuEChERS Method with a mixture of diluents used followed by clean up with the PSA. Three concentration levels (0.50, 2.55 and 5.10 μg/kg) were used to validate the approach and the outcomes ranged between 70 to 120%, with relative standard deviations (% RSD) of ≤ 20%. The detection and quantification limits were derived at the concentration of 0.010 and 0.50 μg/kg, respectively with a significant %ME of 9.90%. The quantitation of imidacloprid pesticide residue in the mango matrix can be done at a lower quantification level by UPLC-ESI-MS/MS.