Easy Cheap Effective Rugged Safe Research Articles

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.

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.

Detection of Per- and Polyfluoroalkyl Substances in High-Protein Food Products.

Per- and polyfluoroalkyl substances (PFAS) belong to the emerging class of persistent organohalogenated contaminants in the environment. We determined the levels of 10 PFAS in selected samples representing different food types, with a special focus on those rich in protein such as fish, meat and meat preparations, liver, eggs, and leguminous vegetables. Such determinations were based on the Quick Easy Cheap Effective Rugged Safe extraction procedure followed by micro-high-performance liquid chromatography-tandem mass spectrometry. The most frequently found was perfluorooctanoic acid, in 84% of the food samples. However, its maximum measured concentration was 0.50 ng g-1 , in a herring sample. The highest concentrations were for perfluorobutanoic acid (35 ng g-1 measured in a pork liver sample) and perfluorooctane sulfonate (12 ng g-1 measured in a herring sample). Because these compounds may bioaccumulate in human tissues by dietary intake, further research into their impact on human health is called for. Environ Toxicol Chem 2023;42:2589-2598. © 2023 SETAC.

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.

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.

Validation of the Multiresidue Method Analysis for Pesticides in Bee Honey by UPLC-MS/MS using the Method of Samples Preparation QuEChERS

In this paper we present the results of evaluating the suitability of the developed method for the simultaneous determination of 200 pesticide residues in bee honey using ultraperformance liquid chromatography - tandem mass spectrometry (UPLC-MS/MS). The main stages of extraction of pesticides from the matrix using QuEChERS (Quick Easy Cheap Effective Rugged Safe) sample preparation are described. Appropriate mobile phase composition was used to better identify analytes, internal standards were not applied. The studied list of pesticides is relevant for use in modern agriculture. The limit of quantification of the method (LOQ) for each of the analytes is 0.001 mg/kg, the relative standard deviation in the conditions of repeatability and reproducibility &lt; 20.0 %, the expanded measurement uncertainty is less than the limit of regulatory requirements &lt; 50.0 %. The calibration graph for each of the analytes had a coefficient R2 &gt; 0.99. The use of QuEChERS sample preparation methods allows to reduce labor intensity, time and reagents, increase the accuracy and precision of research in comparison with classical methods of sample preparation. The described method makes it possible to detect a wide range of pesticides and has a fairly high sensitivity

Impact of Photolysis and TiO2 on Pesticides Degradation in Wastewater

Pesticide residues are harmful to the environment and human and animal health even at low levels because of long-term bioaccumulation. In this study, photolysis was applied to treat three representative water samples: aqueous atrazine and dimethoate solutions as target pesticides, as well as wastewater and agriculture wastewater containing pesticide residue. It was performed using ultraviolet (UV) irradiation at two wavelengths (254 and 306 nm) with exposure times ranging from 2 to 12 h in the presence and absence of a photocatalyst to identify the optimal degradation conditions. Extraction and analyzation process were performed by the Quick Easy Cheap Effective Rugged Safe (QuEChERS) methods and gas chromatography–tandem mass spectrometry with triple quadrupole detector (GC–MSMS/TQD), respectively. Photodegradation increased with an increase in exposure time and the TiO2 catalyst was beneficial for degradation. Both selected irradiation wavelengths were effective, although the wavelength of λ = 306 nm was the most efficient.

A laboratory comparison of the interactions between three plastic mulch types and 38 active substances found in pesticides.

BackgroundIn semi-arid regions, the use of plastic mulch and pesticides in conventional agriculture is nearly ubiquitous. Although the sorption of pesticides on Low Density Polyethylene (LDPE) has been previously studied, no data are available for other plastics such as Pro-oxidant Additive Containing (PAC) plastics or “biodegradable” (Bio) plastics. The aim of this research was to measure the sorption pattern of active substances from pesticides on LDPE, PAC and Bio plastic mulches and to compare the decay of the active substances in the presence and absence of plastic debris.MethodsFor this purpose, 38 active substances from 17 insecticides, 15 fungicides and six herbicides commonly applied with plastic mulching in South-east Spain were incubated with a 3 × 3 cm2 piece of plastic mulch (LDPE, PAC and Bio). The incubation was done in a solution of 10% acetonitrile and 90% distilled water at 35 °C for 15 days in the dark. The Quick Easy Cheap Effective Rugged Safe approach was adapted to extract the pesticides.ResultsThe sorption behavior depended on both the pesticide and the plastic mulch type. On average, the sorption percentage was ~23% on LDPE and PAC and ~50% on Bio. The decay of active substances in the presence of plastic was ~30% lesser than the decay of active substances in solution alone. This study is the first attempt at assessing the behavior of a diversity of plastic mulches and pesticides to further define research needs.

Influence of pH, Total Acidity and Technological Processes of Preparation of babenda “leafy vegetables and cereal sauce” on Pesticide Residues

The uncontrolled use of pesticides on leafy vegetables has been frequently reported in recent years. The aim of this study was to evaluate the influence of pH, total acidity and various technological processes for the preparation of on pesticide residues contained in leafy vegetable. The babenda is a Burkinabe dish consisting mainly of Hibiscus sabdariffa, Amaranthus hybridus and Cleome gynandra coarsely cut from steamed rice. The Quick, Easy Cheap Effective Rugged Safe Method (QuEChERS) and Gas Chromatography with Microelectron Capture Detector (GC-μECD) were used. Six pesticides were detected in 180 samples of leafy vegetables and cereal sauce (babenda) collected in 5 cities of Burkina Faso. Results showed that 56% of the samples contained residues among which 41.66% contained concentrations above the LMR and 25% contained multiple pesticides. There were found a correlation between pH and dieldrin content. Compared with the diuron with an average value of 0.0625-0.0969 mg.kg-1, there is no correlation between this molecule and the pH (5.86) whose acidity varies between 0.04 - 0.10. The pH has an influence on the cypermethrin and the diuron. However acidity has an effect on the degradation of Lamda-cyhalothrines, 2, 4 DDT, dieldrin, heptachlor. For treatments of 150°C and 300°C, organochlorine pesticides are little or no degradation. There is a considerable reduction as the temperature increases. Only lindane, heptachlor, aldrin, alpa-endosulfan and 2, 4 DDT which have undergone total destruction from 250 and 300°C. Significant reductions were observed in all treatments applied. Future research needs to focus on the integration of food safety parameters into actual applied research at the level of producers.

Estimation of Pesticide Residues in Selected Products of Plant Origin from Poland with the Use of the HPLC-MS/MS Technique

The purpose of this work was to compare the content of pesticide residues (250) in unprocessed plant products from farms situated in the eastern part of Poland. The content of pesticide residues in the analysed samples was assayed with the use of the QuEChERS (Quick Easy Cheap Effective Rugged Safe) method combined with HPLC-MS/MS (high performance liquid chromatography with tandem mass spectrometry) analysis. The analyses revealed that among 160 analysed samples, pesticide residues were detected in 83 samples (approximately 52%), while in 77 samples (approximately 48%), no presence of those substances was noted. In all the samples in which the presence of the sought compounds was identified, their levels did not exceed the Maximum Residue Levels (MRL). The most often identified ones were azoxystrobin—detected in 36 samples (22.5%), linuron—assayed in 33 samples (20.6%), chlorpyrifos and carbendazim—each detected in 13 samples (8.1%), metalaxyl and metalaxyl M—in 11 samples (6.9%), and acetamiprid—in 7 samples (4.4%).

Dietary exposure of the Qatari population to food mycotoxins and reflections on the regulation limits.

The article estimates the exposure of the population of Qatar to aflatoxins, fumonisins and ochratoxins, measured in food samples collected from the markets of Doha. The mycotoxin extractions were performed using the "Quick Easy Cheap Effective Rugged Safe" Method (QuEChERS) and the extract measured with LC-MS/MS. High contamination with aflatoxins was detected in Nuts and Spices (e.g. 534.15 ng/g and 371.6 ng/g respectively). The estimated daily intake (EDI) level was estimated using statistical data on average Qatari population. Additionally, the probability to exceed TDI was calculated for fumonisins and ochratoxins. The results indicate high exposure to aflatoxins (with alarming values of margin of exposure, i.e. MoE). The article points to the necessity of a regular assessment and reevaluation of the concentration limits allowed in food products accounting for statistics on the population (i.e. food consumption), economic growth of the country, and monitoring of mycotoxin contamination of food as much as technological, financial and human resources of a country allows.

Fast and easy liquid chromatography–mass spectrometry method for evaluation of postharvest fruit safety by determination of mycotoxins: Fumitremorgin C and verruculogen

Fumitremorgin C and verruculogen are mycotoxins produced by heat-resistant Neosartorya fischeri. Easy and fast monitoring of their production by selective and sensitive analytical methods is crucial for ensuring postharvest quality of fruit, food safety, and thus human health and well-being. A six-minute liquid chromatography tandem mass spectrometry method (LC/MS/MS) was developed for quantification of fumitremorgin C and verruculogen in potato dextrose broth (PDB), strawberry juice, strawberry fruit, and soil. Mycotoxins were extracted from all media with the QuEChERS (Quick Easy Cheap Effective Rugged Safe) method. The lower limit of quantification (LLOQ) of the method for both mycotoxins was 1μgL−1 for PDB and strawberry juice and 1μgkg−1 for strawberry fruit and soil. Collision-induced dissociation of protonated fumitremorgin C and verruculogen ions was also examined by high-resolution mass spectrometry to assist researchers in non-targeted screening for mycotoxins and in identification of these two toxins. The developed LC/MS/MS method was applied to examine mycotoxin production by 45 environmental Neosartorya strains: 5 well-known strains, included in the study as reference strains, and 40 strains that were newly isolated and identified by us.

Risk Assessment of Florists Exposed to Pesticide Residues through Handling of Flowers and Preparing Bouquets.

Flowers are frequently treated with pesticides and, as a result, florists handling daily a large number of flowers can be exposed to pesticide residues. A study was conducted among twenty volunteer florists located in Namur Province and in the Brussels Capital Region of Belgium in order to assess their potential dermal exposure to dislodgeable pesticide residues transferred from flowers to hands. Two pairs of cotton gloves were worn during two consecutive half days while handling flowers and preparing bouquets (from min 2 h to max 3 h/day). The residual pesticide deposits on the glove samples were extracted with a multi-residue Quick Easy Cheap Effective Rugged Safe (QuEChERS) method and analyzed by a combination of gas and liquid chromatography tandem mass spectrometry (GC-MS/MS and LC-MS/MS) by an accredited laboratory. A total of 111 active substances (mainly insecticides and fungicides) were detected, with an average of 37 active substances per sample and a total concentration per glove sample of 22.22 mg/kg. Several predictive levels of contamination were considered to assess the risk. The potential dermal exposures (PDE) of florists were estimated at the average, for different percentiles, and at the maximum concentration of residues in samples. At the PDE P90 and at the PDEMAX (or worst case) values, three and five active substances respectively exceed the Acceptable Operator Exposure Level (AOEL), indicating risk situations. For the systemic exposure (SE), one active substance (clofentezine) exceeds the AOEL at the P90 predictive level. In the worst case, SEMAX (at the maximum concentrations), four active substances (clofentezine, famoxadone, methiocarb, and pyridaben) exceed their respective AOEL values. Among the 14 most frequently detected active substances, two have SEMAX values exceeding the AOEL. Exposure could be particularly critical for clofentezine with an SEMAX value four times higher than the AOEL (393%). The exposure of florists appeared to be an example of a unique professional situation in which workers are exposed regularly to both a very high number of toxic chemicals and rather high concentration levels. Therefore the priority should be to raise the level of awareness among the florists who must change their habits and practices if they want to minimize their exposure.

Pesticide Residues on Three Cut Flower Species and Potential Exposure of Florists in Belgium.

In order to assess the prevalence of pesticide contamination and the risk of florists’ exposure when handling cut flowers, sampling and analysis of 90 bouquets of the most commonly sold cut flowers in Belgium (50 bouquets of roses; 20 of gerberas, and 20 of chrysanthemums) were carried out. The bouquets were collected from 50 florists located in the seven largest cities of Belgium (Antwerp, Brussels, Charleroi, Ghent, Leuven, Liege, and Namur) and from five supermarkets located in the different regions. To have a better understanding of the route of exposure and professional practices a questionnaire was also addressed to a group of 25 florists who volunteered to take part in the survey. All florists were interviewed individually when collecting the questionnaire. The residual pesticide deposit values on cut flowers were determined in an accredited laboratory using a multi-residue (QuEChERS Quick Easy Cheap Effective Rugged Safe) method and a combination of gas chromatography (GC) and liquid chormatograhphy (LC) analysis. A total of 107 active substances were detected from all samples; i.e., an average of about 10 active substances per bouquet. The most severely contaminated bouquet accumulated a total concentration of residues up to 97 mg/kg. Results show that roses are the most contaminated cut flowers; with an average of 14 substances detected per sample and a total concentration per rose sample of 26 mg/kg. Some active substances present an acute toxicity (acephate, methiocarb, monocrotophos, methomyl, deltamethrin, etc.) and exposure can generate a direct effect on the nervous system of florists. Nevertheless, fungicides (dodemorph, propamocarb, and procymidone) were the most frequently detected in samples and had the highest maximum concentrations out of all the active substances analysed. Dodemorph was the most frequently detected substance with the highest maximum concentration (41.9 mg/kg) measured in the rose samples. It appears from the survey that, despite being exposed to high deposits of residues, florists usually do not protect themselves from contact with residues even if they spend several hours handling cut flowers and preparing bouquets (from 2 to 6 h/day, depending on the time of year and/or selling periods) daily. Bad habits (eating, drinking, or smoking at work) and absence of personal protective equipment of most florists also increase the risk of contact with pesticide residues.

Measurement of pyrethroids and their environmental degradation products in fresh fruits and vegetables using a modification of the quick easy cheap effective rugged safe (QuEChERS) method

Pyrethroid insecticides are used extensively in agriculture, and they, as well as their environmental degradates, may remain as residues on foods such as fruits and vegetables. Since pyrethroid degradates can be identical to the urinary markers used in human biomonitoring, it is important to understand the contribution of these degradates when studying sources of human pyrethroid exposure.We modified the widely used Quick Easy Cheap Effective Rugged Safe (QuEChERS) method to measure several current-use pyrethroids (cis/trans-permethrin, cypermethrin, deltamethrin, esfenvalerate, bifenthrin, cyfluthrin, and cyhalothrin) and their environmental degradation products (3-PBA, cis/trans-DCCA, 4-F-3-PBA, DBCA, and MPA) in selected fresh fruits and vegetables. Using fortified samples, we determined extraction efficiencies from: tomatoes, oranges (whole, peeled, and rind), grapes, apples, bananas (peeled and rind only), onions, lettuce, green peppers, carrots and broccoli. For a subset of these food items (apples, grapes, tomatoes, lettuce and banana peel), we also established limits of detection (MDLs) and quantitation (MQLs).Each sample was homogenized (1kg) then spiked with the target pyrethroids and their degradation products. Sub-samples (15g) were extracted with acetonitrile, then salted out and partitioned with NaCl and MgSO4. The extract was divided and further cleaned using solid phase extraction (SPE) cartridges containing either graphitized non-porous carbon (pyrethroids) or C18 (degradation products). Sample analysis was via liquid chromatography/tandem mass spectrometry (LC-MS/MS).Considering the mean recoveries each of the 14 analytes in all 13 matrices: 42% of the recoveries were ≥90%, 70% were ≥80%, and 90% were ≥70%. All MDL's were less than 100ng/kg, except 3-PBA (132ng/kg, tomato), MPA (129ng/kg, tomato), and trans-permethrin (141ng/kg, banana peel).We then applied the method to non-spiked samples (subset of 5 for which the MDLs/MQLs had been determined) collected weekly for four weeks from local supermarkets. At least one pyrethroid was present in measureable concentrations in all matrices except banana peels. In contrast, the only degradation products detected were cis/trans-DCCA, in one lettuce sample.

Organophosphorus insecticides in honey, pollen and bees (Apis mellifera L.) and their potential hazard to bee colonies in Egypt

There is no clear single factor to date that explains colony loss in bees, but one factor proposed is the wide-spread application of agrochemicals. Concentrations of 14 organophosphorous insecticides (OPs) in honey bees (Apis mellifera) and hive matrices (honey and pollen) were measured to assess their hazard to honey bees. Samples were collected during spring and summer of 2013, from 5 provinces in the middle delta of Egypt. LC/MS–MS was used to identify and quantify individual OPs by use of a modified Quick Easy Cheap Effective Rugged Safe (QuEChERS) method. Pesticides were detected more frequently in samples collected during summer. Pollen contained the greatest concentrations of OPs. Profenofos, chlorpyrifos, malation and diazinon were the most frequently detected OPs. In contrast, ethoprop, phorate, coumaphos and chlorpyrifos-oxon were not detected. A toxic units approach, with lethality as the endpoint was used in an additive model to assess the cumulative potential for adverse effects posed by OPs. Hazard quotients (HQs) in honey and pollen ranged from 0.01–0.05 during spring and from 0.02–0.08 during summer, respectively. HQs based on lethality due to direct exposure of adult worker bees to OPs during spring and summer ranged from 0.04 to 0.1 for best and worst case respectively. It is concluded that direct exposure and/or dietary exposure to OPs in honey and pollen pose little threat due to lethality of bees in Egypt.

Efficacy of processing treatments on cypermethrin residues in okra (Abelmoschus esculentus)

Purpose – This paper aims to study the effect of different processing treatments to reduce cypermethrin residues in okra and judge the consumer preferences of the applied unit operations. Deliberate use of pesticides on vegetables has been frequently reported in recent past. Association of pesticides with multiple health odds in human beings necessitates its removal from diet. Design/methodology/approach – Cypermethrin residues were analysed using Quick Easy Cheap Effective Rugged Safe method and quantified using gas chromatography. Consumer acceptability was judged using a 9-point Hedonic scale. Findings – Significant reductions were observed in all treatments applied. Percentage reduction observed with different pre-treatments ranged from 36 per cent (tap water) to 89 per cent (acetic acid and potassium permanganate). All cooking methods, except microwave cooking, were found effective, as the per cent reduction varied from 91 to 98 per cent. Maximum reductions were observed with pressure cooking. However, on the basis of organoleptic scores, washing was the most preferred pre-treatment, followed by sodium bicarbonate. Least score was obtained by samples treated with potassium permanganate. Among the cooking methods, all samples were acceptable, except pressure cooking. Taking into consideration both factors, i.e. residue reduction and consumer acceptability, sodium bicarbonate, sodium chloride and frying were found to be the best household treatments. Originality/value – Present study pioneered and tried to establish links between the efficacies of laboratory to the consumer level, thereby judging its utility. Further research must focus on taking this parameter of food safety to real applied research at the consumer level.

Development and validation of an LC–MS/MS/MS method for the quantification of fluoroquinolones in several matrices from treated turkeys

The study presents a sensitive and reliable confirmatory method for the extraction, identification, quantification of five fluoroquinolones (FQ) namely enrofloxacin, ciprofloxacin, difloxacin, sarafloxacin and flumequine, in plasma, liver, kidney, muscle, skin + fat, lung and intestinal content from turkeys.For the extraction and matrix clean-up of FQ residues from all biological matrices, the Quick Easy Cheap Effective Rugged Safe (QuEChERS) methodology was adopted; only for plasma samples acetonitrile was used.The analyses were performed by liquid chromatography with mass spectrometry detection (LC–MS). LC separation was performed on a C18 Kinetex column (100 × 2.1 mm, 2.6 μm, Phenomenex, CA, USA) with gradient elution using ammonium acetate solution (10 mM, pH 2.5) and methanol containing 0.1% formic acid. Mass spectrometric identification was done using an LTQ XL ion trap (Thermo Fisher Scientific, CA, USA), with a heated electrospray ionization probe, in positive ion mode.The method was validated according to the European Legislation (decision 2002/657/EC) and EMA guideline (EMA/CVMP/VICH/463202/2009); selectivity, linearity response, trueness (in terms of recovery), precision (within-day repeatability and within-laboratory reproducibility), limit of detection, limit of quantification, decision limits, detection capability, absolute recovery and robustness were evaluated using turkey blank matrices. All data were within the required limits established for confirmatory methods except for flumequine which presented a recovery value slightly higher than 110% in muscle and intestinal content. For all FQs, all the extraction rates were greater than 70% and limits of quantification ranged from 1.2 μg kg−1 to 118.8 μg kg−1.This fast and robust method was suitable for the identification and quantification of FQ residues in tissues, plasma and intestinal content as confirmed by data obtained from incurred samples of turkeys treated at farm for therapeutic purposes.

Comparative Study of the Methodology Used in the Extraction of Isoflavones from Legumes Applying a Modified QuEChERS Approach

Isoflavones are phytochemicals of great interest because of their association with a large variety of positive effects on human health. The major sources of isoflavones in the diet are plants of the Leguminosae family, especially soybeans, although many other legumes more widely consumed in the Mediterranean diet have also been reported to contain these compounds. In previous work we extracted isoflavones from samples using a modified QuEChERS (Quick Easy Cheap Effective Rugged Safe) methodology. To compare different methods for placing the sample and the solvent in contact to optimise the extraction of isoflavones from legumes (chickpeas, lentils and white beans) using a modified QuEChERS methodology. Five different approaches to sample agitation were tested: vortex agitation, thermostatted stirring agitation and thermostatted tray shaking, and a thermostatted ultrasound bath and an ultrasound probe. To evaluate the different methodologies a modified QuEChERS approach was used as the extraction method. The separation and quantification of isoflavones was carried out using liquid chromatography-triple quadrupole/mass spectrometry (LC-MS/MS). The best methods were found upon using a thermostatted shaking tray for the extraction of chickpeas and white beans and the ultrasound probe for lentil samples. These methods were chosen based on the highest amount of analytes obtained as well as the best recovery values. Determination of isoflavones in foods may be affected by the different methods used to place the sample and the solvent in contact in the extraction step. The main advantages of the proposed extraction procedures are their simplicity, speed, reliability and low cost.