Quick, Easy, Cheap, Effective, Rugged, Safe Research Articles

Development and validation of a green analytical method for determining fourteen bisphenols in bee pollen by ultra-high-performance liquid chromatography-tandem mass spectrometry

A new analytical method was developed and validated to determine fourteen bisphenols (A, B, C, E, F, M, P, S, Z, AF, AP, BP, FL, PH) in bee pollen using ultra-high-performance liquid chromatography-tandem mass spectrometry. Two different sample treatments were proposed and evaluated: one based on the QuEChERS (quick, easy, cheap, effective, rugged & safe) approach and the other utilizing microextraction with a supramolecular solvent (SUPRAS). In both cases, average analyte recovery ranged between 71 % and 114 %, and the matrix effect was between −45 % and +5 %, although it was not significant when using the QuEChERS-based method (<±20 %). The environmental impact of both sample treatments was assessed using different analytical metrics, with both procedures classified as environmentally friendly, though slightly better results were obtained for SUPRAS. The method was fully validated, showing that the QuEChERS approach had better overall performance, particularly regarding sensitivity and matrix effect. Consequently, the QuEChERS methodology was applied to determine bisphenols in thirty bee pollen samples from different Spanish regions. Residues of three bisphenols (M, P, and S) were detected, although only bisphenol S was quantified in several samples at low concentration levels (<7 μg kg−1), which is below the established specific migration limit (SML; 50 μg kg−1). However, regarding human health, the estimated daily intake, target hazard quotient, and hazard index assessed were higher than acceptable limits, suggesting a potential risk for human consumers.

Co-occurrence and exposure assessment of deoxynivalenol and fumonisins from maize and maize-based products in Indonesia

This study was conducted to investigate the co-occurrence of deoxynivalenol (DON) and fumonisins (FBs) in maize-based food products and their dietary exposure to the Indonesian population. A survey of 45 samples of maize and maize-based-food products collected from markets in Indonesia were analyzed using liquid chromatography-mass spectrometry after a Quick Easy Cheap Effective Rugged Safe (QuEChERS) extraction and clean-up process. Results revealed that 35.56% of maize food products were found to contain DON and FBs simultaneously. FBs frequently detected in 84.44% of samples and DON was found in 42.22% of the samples with mean positive levels ranging from 0.12 to 264.24 µg/kg (FBs) and 2.62 µg/kg to 122.28 µg/kg (DON). None of the quantifiable samples exceeded the maximum limits established by the European Commission (EC) and National regulation. The highest total means exposure to DON and FBs was found in infants and toddler attaining up to 0.025 and 0.087 µg/kg body weight (bw) per day while 95th percentile (P95) values were 3.8 and 4.4 times higher than the mean exposure. Both for DON and FBs, total mean and P95 exposures of the population did not exceed the provisional maximum tolerable daily intake (PMTDI) of 1 µg/kg bw/day for DON and 2 µg/kg bw/day for FBs, respectively. Therefore, the risk assessment indicates that there is no potential risk to health from DON and FBs through maize and maize-based food intake.

Quechers Extraction Followed by HPLC Estimation of Steroidal Glycoalkaloids viz, α-Chaconine and α-Solanine in Different Solanaceae Family Vegetable Varieties

Glycoalkaloids are the alkaloid derived chemical constituents naturally produced in various plants species especially Solanaceae family. These chemical constituents protect the plant against predators as well as pathogens. The consumption of high dose of glycoalkaloids was toxic to humans. This study was purposeful to evaluate steroidal glycoalkaloids viz., α-chaconine and α-solanine quantity in different Solanaceae family vegetable varieties. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) extraction using acetonitrile as extracting solvent was used for extracting steroidal glycoalkaloids in vegetable samples. In the optimized conditions, the standard chromatogram shows clear resolution of α-chaconine and α-solanine. The analytes were identified at 3.15 min for α-chaconine and 4.88 min for α-solanine. The optimized HPLC (High pressure liquid chromatography) method was validated. The method optimized using acetonitrile and 1.0 mM ammonium acetate buffer at pH 4.2 in 65:45 (v/v) as mobile phase at 0.6 mL/min, μBondapak C18 (10 μm, 4.6x250 mm) column as stationary phase and UV detection is selected at 218 nm. Findings suggest that this method was simple and convenient for the estimation of glycoalkaloids in vegetables. The glycoalkaloids was achieved under the acceptable levels of less than 200 mg/kg as prescribed by USFDA and German Federal Institute for Risk Assessment.

Final Residues, Dissipation Dynamics and Dietary Risk Assessment of Cupric Nonyl Phenolsulfonate in Citrus and Soil

ABSTRACT Field trials were conducted in two consecutive years to evaluate the terminal residue levels, dissipation trend of cupric nonyl phenolsulfonate in citrus and soil. Analyses were carried out using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) to determine the concentration of cupric nonyl phenolsulfonate in citrus and soil. The results showed a good linear relationship within the range of 0.01 to 5.0 mg·L−1 (R2 = 0.9999). Average recoveries were 77.70%-105.25% for cupric nonyl phenolsulfonate at the spiked levels of 0.01, 0.1,1, and 5 mg·kg−1, the relative standard deviations (RSDs) were 2.23–7.22%. Half-lives (t1/2) of cupric nonyl phenolsulfonate were 2.76–5.87 and 1.27–3.22 days in citrus and soil, respectively. The results showed that the final contents of cupric nonyl phenolsulfonate in citrus peel were the highest while that of citrus pulp were the lowest. As for soil, the final contents range from < 0.010 to 4.081 mg·kg−1. The dietary risk assessment of citrus was evaluated with risk quotients. The risk quotient values were found to be significantly < 100%, indicating that using recommended doses of cupric nonyl phenolsulfonate in citrus fruits poses risks to human health within acceptable risk levels. The results of this study contribute to the guidance of safe and reasonable use of cupric nonyl phenolsulfonate.

Simultaneous Determination of Pesticides in Lonicera japonica by QuEChERS Preparation and Gas Chromatography-Mass Spectrometry (GC-MS)

Lonicera japonica is a commonly used Chinese herbal medicine, but few studies have focused on its pesticide residues. In this study, a quick, easy, cheap, effective, rugged, safe (QuEChERS) pretreatment combined with gas chromatography-mass spectrometry (GC-MS) was established to determine 16 pesticides in L. japonica. Various factors including the type and volume of extraction solvent, times of ultrasound-assisted extraction, and type and weight of purifying agents were optimized. The established method showed good linearity with correlation coefficient (r) > 0.99 within the range of 0.01–5.0 mg·L−1, and average recoveries (AR) were 82.3%-102.5% at spiking levels of 0.01, 0.1, and 0.5 mg·kg−1 with relative standard deviations (RSD) of 0.43%-4.75%. Only bifenthrin and fenvalerate can be detected with maximum detected concentrations of 1.41 and 0.13 mg·kg−1. The results showed that the established method can be applied to detect pesticide residues in L. japonica with potential applications for other Chinese herbal medicines.

Optimization and validation of high-performance liquid chromatography using modified QuEChERS to determine anthelmintic drugs in mutton.

The aim of this study was to rapidly determine the presence of anthelmintic drugs in sheep meat using the optimized high-performance liquid chromatography-ultraviolet (HPLC-UV) method with modified QuEChERS (quick, easy, cheap, effective, rugged, safe) technology. Fifty fresh sheep meat samples from different slaughterhouses were collected. A double extraction procedure (QuEChERS/HPLC-UV technology) was used to extract the target analytes. A multilevel calibration curve from 1 to 1000 g/kg was used to establish instrument linearity for rafoxanide, albendazole, and closantel, whereas 0.1-100 μg/kg was used for ivermectin, levamisole, and oxyclozanide to find the lowest concentration, maximum residue limit (MRL), and occupied range for targeted analytes. The concentration levels were used to investigate the linearity, whereas several certified reference materials were applied to determine accuracy. The process was linear for all combinations, from the limit of quantification (LOQ) to the maximum concentration. The LOQ was established at 0.5μg/kg for ivermectin, levamisole, and oxyclozanide and 10μg/kg for rafoxanide, albendazole, and closantel. Recovery values were 70%-120%, and repeatability/reproducibility stated in relative standard deviation was obtained at less than 20%. QuEChERS method revealed that most meat samples contained anthelmintic drug residues, of which the majority exceeded the MRLs. Thus, the drugs should be used correctly in animals to avoid residues in food for human consumption.

Multi-residue monitoring and dietary risk assessment of 17 pesticides and 3 related metabolites in rice and rice flour from markets in China.

Pesticide residues in rice have attracted widespread public attention in recent years. This research aimed to monitor the residues of 17 pesticides and their 3 metabolites in 120 samples of rice and rice flour collected from markets in China using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) pretreatment method combined with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The monitoring results showed that isoprothiolane, tricyclazole, fenoxanil, and tebuconazole were detected in the rice samples, with detection frequencies of 33.3%, 17.5%, 8.3%, and 2.5%, and concentrations ranging from 0.02 to 0.1 mg/kg (median = 0.04), 0.01 to 0.17 mg/kg (median = 0.14), 0.04 to 0.06 mg/kg (median = 0.05), and 0.01 to 0.02 mg/kg (median = 0.01), respectively. The residues of these four pesticides were all below their corresponding maximum residue levels (MRLs) set by China. Additionally, isoprothiolane, tricyclazole, fenoxanil, and tebuconazole were detected in rice flour samples, with detection frequencies of 74.2%, 55.0%, 5.0%, and 2.5%, and concentrations ranging from 0.01 to 0.1 mg/kg (median = 0.04), 0.01 to 0.04 mg/kg (median = 0.02), 0.01 to 0.06 mg/kg (median = 0.03), and 0.02 to 0.04 mg/kg (median = 0.03), respectively. Furthermore, the chronic dietary intake risk (HQc), the acute dietary intake risk (HQa), and cumulative dietary risk (HI) for all the detected pesticides were evaluated and found well below 100%, indicating that the dietary intake risks would not pose potential health risks.

Occurrence of Pesticides in Polished Rice Samples From Tanjung Karang and Sekinchan and the Health Risk among Consumers

Introduction: One of the key staple foods in many different countries, including Malaysia, is rice (Oryzae sativa L.). Pesticides are used to reduce weed growth and safeguard crops from insect attacks in order to boost paddy output. Objective: This research quantifies the concentration of pymetrozine, chlorantraniliprole, and difenoconazole, along with any potential health risks to consumers. Methods: Samples of polished rice from three rice milling factories in Tanjung Karang and Sekinchan were extracted using the QuEChERS (Quick Easy Cheap Effective Rugged Safe) technique. The amount of pesticide residue in polished rice was then measured using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). A health risk assessment was conducted utilizing the Hazard Quotient (HQ) and Lifetime Cancer Risk (LCR) to estimate the non-carcinogenic and carcinogenic health risks. Results: The mean concentration of pesticides in polished rice ranged from less than the detection limit (difenoconazole) to 1.122 µg/kg (pymetrozine). No rice samples above the Maximum Residue Limit (MRL) specified in the Food Act 1983 as implemented by Malaysia’s Food Regulations 1985. Pymetrozine, chlorantraniliprole, and difenoconazole in rice had respective MRLs of 50 µg/kg, 2000 µg/kg, and 100 µg/kg. For all age groups, no significant non-carcinogenic health risk was associated with consuming polished rice from the study area, where the HQ and Hazard Index (HI) were less than one. When LCR values were less than 10-6, carcinogenic health risks of consuming polished rice from the study area were at a clearly acceptable risk level. Conclusion: As no sample exceeded the MRL, the findings indicated that all rice samples collected from Tanjung Karang and Sekinchan were safe for consumption.

Determination of 45 Pesticides in Avocado Varieties by the QuEChERS Method and Gas Chromatography-Tandem Mass Spectrometry.

Gas chromatography (GC) tandem mass spectrometry (MS/MS) stands as a preeminent analytical instrument extensively employed for the surveillance of pesticide residues in food. Nevertheless, these methods are vulnerable to matrix effects (MEs), which can potentially affect accurate quantification depending on the specific combination of analyte and matrix. Among the various strategies to mitigate MEs, matrix-matched calibration represents the prevailing approach in pesticide residue applications due to its cost-effectiveness and straightforward implementation. In this study, a total of 45 representative pesticides were analyzed in three different varieties of avocado (i.e., Criollo, Hass, and Lorena) using the Quick-Easy-Cheap-Effective-Rugged-Safe (QuEChERS) method with ammonium formate and GC-MS/MS. For this purpose, 5 g of the avocado sample was extracted with 10 mL of acetonitrile, and then 2.5 g of ammonium formate was added to induce phase separation. Subsequently, the supernatant underwent a cleanup process via dispersive solid-phase extraction employing 150 mg of anhydrous MgSO4, 50 mg of primary-secondary amine, 50 mg of octadecylsilane, 10 mg of graphitized carbon black, and 60 mg of a zirconium oxide-based sorbent (Z-Sep+). The GC-MS/MS analysis was successfully performed in less than 25 min. Rigorous validation experiments were carried out to assess the performance of the method. The examination of a matrix-matched calibration curve for each variety of avocado revealed that the ME remained relatively consistent and less than 20% (considered as a soft ME) for most pesticide/variety combinations. Furthermore, the method´s limits of quantification were lower than 5 µg/kg for all three varieties. Finally, the recovery values for most pesticides fell within the acceptable range of 70-120%, with relative standard deviation values below 20%.

Residue analysis and dietary risk assessment of abamectin in fresh corn, bitter melon, and Fritillaria.

To clarify the residue behavior and possible dietary risk of abamectin in fresh corn, bitter melon, and Fritillaria, a method was developed for the simultaneous determination of abamectin residues in fresh corn, bitter melon, and Fritillaria by QuEChERS (quick, easy, cheap, effective, rugged, safe) ultra-performance liquid chromatography-tandem mass spectrometry. The mean recovery of abamectin in fresh corn, bitter melon, and Fritillaria was 86.48%-107.80%, and the relative standard deviation was 2.07%-10.12%. The detection rates of abamectin residues in fresh corn, bitter melon, and Fritillaria were 62.50%, 87.50%, and 80.00%, respectively. The residues of abamectin in fresh corn, bitter melon, and Fritillaria were not more than 0.020, 0.019, and 0.087 mg/kg, respectively. Based on these results, dietary risk assessment showed that the risk content of abamectin residues in long- and short-term dietary exposure for Chinese consumers was 61.57% and 0.41%-1.11%, respectively, indicating that abamectin in fresh corn, bitter melon, and Fritillaria in the market would not pose a significant risk to consumers.

Multiresidue analysis and dietary intake risk assessment of 29 pesticides in banana from five provinces of southern China

The present study utilized a combined quick, easy, cheap, effective, rugged, safe (QuEChERS) method with ultra-performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS) to detect and quantify pesticide residues in both whole banana fruit and pulp samples collected from five provinces in southern China between June 2018 and December 2021. The analysis identified the occurrence of 29 widely used insecticides, fungicides, and herbicides on bananas, including organophosphates, organochlorines, pyrethroids, triazoles, etc. The limits of quantification for the pesticides analyzed in the banana matrix ranged from 1.0 to 5.0 μg/kg. Among the 501 samples collected, the detection rates of pesticides in whole fruit and pulp samples were 65.1 % and 40.9 %, respectively. Specifically, 20 kinds of pesticides were detected in whole fruit samples, while 16 were detected in pulp samples. Furthermore, imidacloprid was detected across various regions and years. The evaluation of risk of hazard quotient (HQ) to the identified pesticides in whole fruit and pulp samples revealed values ranging from 0.0016-0.0313 and 0.0002–0.0131, respectively. Overall, the results suggest that the detected pesticide residues in bananas are unlikely to pose an unacceptable health risk to consumers of different age groups in China.

Monitoring and method validation of organophosphorus/organochlorine pesticide residues in vegetables and fruits by gas chromatography.

In this study, an analytical method was developed and validated for the assessment of pesticide residues in commonly consumed vegetables and fruits. Fresh samples of apple, green peas, tomatoes, and cucumbers were processed and subjected to analysis using a modified QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction technique. Subsequently, quantification of pesticide residues was conducted utilizing gas chromatography (GC)-electron capture detector. Extraction and cleanup parameters were meticulously optimized, resulting in a modification of the original QuEChERS method. This modification aimed to reduce solvent consumption, making the study more environmentally friendly. The developed method was validated in terms of selectivity, specificity, linearity, precision, and accuracy by following the SANTE guidelines. Calibration curves showed good linearity (r > 0.99) within the test range. Precision was evaluated by intra- and inter-day experiments with an acceptable relative standard deviation (<20.0%). Recovery was assessed at the limit of quantification level and was observed to fall within the range of 70%-120%, with relative standard deviations below 5.45%. The validated method presented here can be applied to analyze pesticide residues in various other vegetables, fruits, and cereals. It is essential for ongoing monitoring of pesticide residues to ensure public safety.

AFB1 colorimetric aptamer sensor for the detection of AFB1 in ten different kinds of miscellaneous beans based on gold nanoparticles and smartphone imaging.

A simple, rapid, low-cost, sensitive, intuitive, visual, label-free, colorimetric smartphone-assisted assay was developed for the measurement of aflatoxin B1 in miscellaneous beans. Ten different kinds of miscellaneous beans were treated and measured by modified QuEChERS(Quick、Easy、Cheap、Effective、Rugged、Safe) method with aflatoxin B1 nucleic acid aptamer as a recognition element and gold nanoparticles as indicators. Several factors influencing its sensitivity were investigated, including consumes and NaCl concentrations, as well as incubation time and specificity. The results showed a good linear relationship between concentrations of 0.2-8.0ng/g under optimal conditions. With a detection limit of 0.08ng/g, the linear regression equation was Y=0.024X+0.4615 (R=0.9989). Sensor specificity is good. The content of aflatoxin B1 in bean samples was determined successfully. The recovery of aflatoxin B1 ranged from 87.18% to 110.24%. The whole thing took 15min. This smartphone-assisted colorimetric aptamer sensor can be used to detect aflatoxin B1 in beans.

A green QuEChERS syringe filter based micro-solid phase extraction using hydrophobic natural deep eutectic solvent as immobilized sorbent for simultaneous analysis of five anti-diabetic drugs by HPLC-UV

BackgroundHere, it has been discussed about creating a specific and sustainable analytical technique for monitoring anti-diabetic drugs in order to accurately determine the dosage in patients and reduce side effects, remove them from wastewater (as emerging contaminants), and ultimately abate pharmaceutical pollutants in the environment. ResultsIn this research, a green and reproducible Quick Easy Cheap Effective Rugged Safe (QuEChERS) method based on syringe filter based micro-solid phase extraction (SF-μSPE) coupled with HPLC-UV using a green sorbent was developed and optimized for the extraction of five anti-diabetic drugs from wastewater, serum, and plasma real samples. A novel green sorbent composed of a liquid mixture of thymol: menthol ([Thy]:[Men], 1:1) hydrophobic natural deep eutectic solvent (HNADES) and curcumin (Cur) immobilized into the non-toxic and biodegradable polyvinyl alcohol (PVA) electrospun nanofibers’ mat was synthesized simply via cheap equipment. Cur was added to enhance the hydrophobicity and functionality of the sorbent. The immobilization process was performed by soaking the mat in the liquid mixture for a specific duration. The correct synthesis and experimental molar ratio of the HNADES components were confirmed by ATR-FTIR and NMR (1H and 13C) spectroscopy. The prepared green sorbent (Cur-HNADES/PVA) was characterized using ATR-FTIR, FE-SEM, EDX/EDX mapping analysis, and water contact angle (WCA) measurement, and it exhibited satisfactory adsorption capacity for the target analytes. SignificanceUnder optimal conditions (pH = 6.0, adsorption cycle = 3, sample volume = 5.0 mL, desorption cycle = 1, type and volume of elution = 80:20 %v/v MeOH/ACN and 500.0 μL), the method was validated in terms of specificity, linear dynamic ranges (LDRs = 0.1–2000.0 μg L−1 and 0.1–1800.0 μg L−1), limits of detection (LODs = 0.03–0.09 μg L−1), and precision (within-day RSDs% = 0.32–1.45% and between-day RSDs% = 0.59–2.03%). Evaluation of the greenness aspects of the proposed method was accomplished using the Green Analytical Procedure Index (GAPI) and Analytical GREEnness (AGREE) approaches. It is noteworthy that the conducted research represents the first report of the synthesis and application of this novel and green sorbent for the determination of anti-diabetic drugs in the mentioned real samples.

Quantitative analysis of lycorine dietary exposure in commercial foods and the Amaryllidaceae family

Lycorine, a prominent alkaloid found in the Amaryllidaceae plant family, is known for its therapeutic properties and potential applications. However, excessive lycorine consumption can cause food poisoning and other detrimental health effects. This study focuses on the quantitative measurement of lycorine levels in commercially available foods and an evaluation of dietary exposure. With regard to this, considerable research has not been conducted to date. For the analysis of lycorine, a Quick, Easy, Cheap, Effective, Rugged, Safe (QuEChERS) technique, and a liquid chromatography-tandem mass spectrometry method were developed, validated, and applied to 56 commercial food samples and 5 Amaryllidaceae plants. The calculated dietary exposure ranged from 0.0 to 3.77 × 10−4 and 0.39–4.72 µg/kg bw/day in lycorine detected foods and Amaryllidaceae plants, respectively (Allium cepa, Allium hookeri, Allium monanthum, Perilla leaves, and Amaryllidaceae plants). Foods in the Amaryllidaceae family were more likely to contain lycorine, with onion identified as a primary food source contributing to lycorine exposure. These findings help to accurately determine the lycorine content in foods, identify potential benefits and risks associated with the consumption of lycorine-containing foods, and may support the need for further research to establish appropriate guidelines for the consumption of these foods.

Dissipation, Processing Factors and Dietary Exposure Assessment of Myclobutanil in Tomato.

Myclobutanil residue poses a potential threat to consumers' health. This work aims to investigate the degradation behavior, residue levels, processing factors (PFs) and dietary risk of myclobutanil in tomato. Myclobutanil was analyzed using a modified quick, easy, cheap, effective, rugged, safe (QuEChERS) method combined with ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS), and average recoveries ranged from 82% to 102% with relative standard deviations RSDs ≤ 9.1%. After spraying myclobutanil miscible oil under field conditions, the initial concentration of myclobutanil was 0.055 mg/kg, and its dissipation followed the first-order kinetics equation with a half-life of 2.88 days. Myclobutanil was mainly present in the tomato skin, and its concentration was about four times that in the whole tomato. The initial concentration of myclobutanil in raw tomato was 0.100 mg/kg. After washing, peeling, homogenization, simmering and canning, the residual level of myclobutanil decreased to 0.067 mg/kg, 0.023 mg/kg, 0.013 mg/kg, 0.044 mg/kg and 0.041 mg/kg, respectively. Although the procedure of simmering led to an increase in myclobutanil concentration, the PFs were all less than 1 in the whole process, showing that the processing procedure significantly decreased the residual level of myclobutanil canned tomato paste in comparison with the raw agricultural commodity. Washing, peeling, and homogenization played critical roles in reducing pesticide residues. The residues of myclobutanil during the processing of tomato pose low dietary exposure risks to consumers in China, which were acceptable. However, the acute and chronic risk quotient for children revealed that it was necessary to monitor the dietary exposure of pesticide residues for children closely.

Evaluation of the potential migration of acaricides from stamped beeswax to honey simulating beehive conditions: A pilot study

There is an issue concerning the migration of pesticides from stamped beeswax to other bee products, mainly, honey. This implies that honey and other beehive-based products could be contaminated, which would represent a potential risk to consumers and food safety. To determine the degree to which acaricides can be transferred from the stamped beeswax to the honey, a pilot experiment was designed consisting of placing beeswax that contained acaricides (endogenous content, τ-fluvalinate, chlorfenvinphos, and coumaphos; spiked samples, coumaphos) in contact with multifloral honey in an incubator. Temperature and shaking conditions were settled simulating beehive conditions. The isolation of the analytes from beeswax involved the use of a QuEChERS (quick, easy, cheap, effective, rugged & safe) method, and honey was analyzed through a solvent extraction procedure. Acaricides were determined in the resulting extracts by gas chromatography with mass spectrometry detection. Coumaphos was the only acaricide transferred into honey in beeswaxes with endogenous acaricide content; meanwhile, results of the experiments with spiked beeswax samples showed that the initial concentration present in the contaminated beeswax significantly influences the transfer to honey, as it was observed that in the spiked beeswax sheets with high levels of coumaphos, the migration from beeswax to honey arose.

Dissipation, residue distribution, and risk assessment of ethiprole and its metabolites in rice under various open field conditions.

Ethiprole has been registered to control planthoppers in rice fields for many years in Asia. However, its dissipation and residues in rice under natural field conditions and health hazards are largely unclear. Herein, a modified QuEChERS and high-performance liquid chromatography-tandem mass spectrometry method was established to detect ethiprole and its metabolites, ethiprole amide and ethiprole sulfone, in brown rice, rice husks, and rice straw. The field experiments were implemented in 12 representative provinces of China under Good Agricultural Practices to study the fate and terminal residues of ethiprole and its metabolites in rice. Finally, the dietary risk of ethiprole was evaluated. The average recoveries of these analytes in all matrices were 86.4%-99.0% with a repeatability of 0.575%-9.38%. The limits of quantification for each compound were 0.01 mg kg-1 . Dissipation of ethiprole followed the single first-order, first + first-order, and first-order multi-compartment kinetic models with a half-life of 2.68-8.99 days in rice husks. The dissipation half-life of ethiprole combining all metabolites was 5.20-16.2 days in rice husks. The terminal residues of ethiprole and its metabolites at preharvest intervals of 21 days were < 0.011, 0.25, and 0.20 mg kg-1 in brown rice, rice husks, and rice straw, respectively. Ethiprole amide was undetectable in all matrices, and the risk quotient of ethiprole was far less than 100%. Ethiprole rapidly converted to ethiprole sulfone in rice, and ethiprole and ethiprole sulfone mainly remained in rice husks and straws. The dietary risk of ethiprole was acceptable for Chinese consumers. This article is protected by copyright. All rights reserved.

Risk Assessment of Pesticide Residues by GC-MSMS and UPLC-MSMS in Edible Vegetables.

In recent years, there has been a significant increase related to pesticide residues in foods, which may increase the risks to the consumer of these foods with the different quality and concentrations of pesticide residues. Pesticides are used for controlling pests that reduce yields. On the other hand, it has become a major public health concern due to its toxic properties. Thus, the objective of the current study employed the application of Quick Easy Cheap Effective Rugged Safe (QuEChERS) method, in combination with gas and liquid chromatography-tandem mass spectrometric detection (GCMSMS, LCMSMS) in order to determine 137 pesticide residues (63 insecticides, 41 acaricides, 40 herbicide, 55 fungicide, nematicide, growth regulator, Chitin synthesis inhibitors, and Juvenile hormone mimics), in 801 vegetables such as 139 tomatoes, 185 peppers, 217 squash, 94 eggplants, and 166 cucumbers from different locations in Hail and Riyadh cities. The results showed that the majority of pesticide residues were detected for each of the following pesticides: acetaimpride, metalaxyl, imidaclopride, bifenthrin, pyridaben, difenoconazole, and azoxystrobien, which were repeated in the samples studied 39, 21, 11, 10, 8, 7, and 5, respectively. In addition, results observed that the tomato was the most contaminated with pesticide residues; it was contaminated with 19 compounds and was followed by pepper, cucumber, and squash, and the last commodity in the contaminated ranking was eggplant. The highest calculated estimated daily intakes (EDIs) were recorded for tomatoes which were estimated between 0.013 to 0.516 mg/kg of body weight per day (bw/day) while the lowest EDIs value was between 0.000002 to 0.0005 mg/kg of bw/day for cucumber. Results indicated that the EDIs values were lower than the acceptable daily intake (ADI) values. Results observed that the most of pesticide residues exposure in food consumption in Saudi Arabia were lower than ADIs. In addition, the highest value for health risk index (HRI) was recorded with Ethion residue in tomato, but in sweet pepper, the highest value for HRI was 127.5 in the form of fipronil residue. On the other hand, results found that the highest values of HRI were 1.54, 1.61, and 0.047 for difenoconazole, bifenthrin, and pyridaben residues in squash, eggplant, and cucumber.

Analysis of Residues of Pesticides in Tomato Processed Foods

The tomato (Solanum lycopersicon L.) crop has great economic relevance, being one of the most processed agricultural products worldwide. Some pesticides are chemically stable and can remain in food even after processing. In this context, the objective of this work was to analyze food products derived from tomatoes (extract, sauce and ketchup), regarding the levels of pesticide residues. Fifteen samples were acquired from Vale do Jaguaribe, Ceará, Brazil. Six pesticides (bifenthrin, chlorothalonil, chlorpyrifos, cyfluthrin, pyriproxyfen, trifluralin) authorized by Agência Nacional de Vigilância Sanitária (Anvisa) for tomato cultivation were selected for the study. QuEChERS (quick, easy, cheap, effective, rugged, safe) extraction and gas chromatography coupled to mass spectrometry (GC-MS) were used in method validation, according to the recommendations of SANTE 11312/2021 guidelines. Statistical analyzes of linearity show that the six pesticides studied were classified as heterocesdastic. Limits of detection (LOD) and quantification (LOQ) values (0.01-0.03 and 0.03-0.10 mg kg-1, respectively) were below the established maximum residue limits (MRLs) for tomatoes. Accuracy and precision (78-121 and 2.3-16.7%, respectively) were satisfactory. The results indicated that among the 15 analyzed samples, one active ingredient was detected (0.05 mg kg-1) in a tomato sauce sample, lower than MRLs (Anvisa 0.15 mg kg-1 and FAO 0.3 mg kg-1). The results show the relevance of monitoring pesticide residues in tomato-derived products and the validation of new methodologies for food control.