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

Residue levels of emamectin benzoate, imidacloprid and its major metabolites in cabbage from twelve regions in China and dietary risk assessment.

A modified quick, easy, cheap, effective, rugged and safe (QuEChERS) method combined with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established to investigate the residues of emamectin benzoate (EB), imidacloprid (IMI) and five IMI metabolites (IMI-olefin, IMI-urea, IMI-guanidine, 5-OH and 6-CNA) in cabbage. The average recoveries of the seven compounds in cabbage were 80%-102%, with relative standard deviations (RSDs) <8.0%. The limit of quantification (LOQ) for each compound was 0.01 mg kg -1 . Standardized residue tests were carried out in 12 areas of China under Good Agricultural Practice (GAP) conditions. A 10% EB-IMI microcapsule suspension was applied once with the high recommended dosage (18 g a.i. ha-1 ) on cabbage. The residues of EB (<0.01 mg kg-1 ), IMI (<0.016 mg kg-1 ) and the sum of IMI and its metabolites (<0.068 mg kg-1 ) in cabbage on the recommended preharvest interval (PHI) (7 d) were lower than the maximum residue limits (MRLs) in China. Based on residual data from fields, toxicology data, and Chinese dietary patterns, dietary risk assessments were conducted. Both the chronic risk quotients (25.2%-73.1%) and acute risk quotients (0.43%-1.57%) of EB and IMI were below 100%, indicating no unacceptable public health risk for different populations. This study provides guidance on the rational application of these insecticides in cabbage.

Fungicide Dissipation Kinetics and Dietary Exposure Risk Assessment in Squash Fruit and Leaf.

The dissipation behavior and dietary exposure risk assessment of four fungicides (dimethomorph, mandipropamid, myclobutanil, and metalaxyl) was performed in fruits and leaves of squash grown under greenhouse conditions. Squash fruit and leaf samples were randomly collected at 0, 3, 5, 7, and 14 days after the last pesticide application. Analysis was performed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was used for sample preparation. Recovery rates at two spiked levels (0.01 and 0.1 mg/kg) were found to be in the range of 76.4%-101.9% for the analyzed pesticides and their relative standard deviations were ≤4%. Pesticide half-lives were 2.1 and 4.9 days for dimethomorph, 4.6 and 8.1 days for mandipropamid, 4.7 and 8.2 days for myclobutanil, and 2.7 and 5 days for metalaxyl in squash fruit and leaf, respectively. Regarding the total surveyors, hazard quotient values for squash fruit and leaf were ≤1.03 × 10-3 and ≤2.39 × 10-3, respectively. These values in the case of true consumers were ≤3.14 × 10-3 and ≤3.91 × 10-1, respectively.

Residues and dietary risk assessment of fluazinam in root mustard after field experiments.

The residue levels of fluazinam in root mustard were investigated by using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique with ultra-performance liquid chromatography tandem mass spectrometry. Samples of leaf and root mustard were analyzed. The recoveries of fluazinam were 85.2-110.8% for leaf mustard with the coefficient of variation of 1.0-7.2%, and 88.8-93.3% for root mustard with the coefficient of variation of 1.9-12.4%. The suspension concentrate formulation of fluazinam was applied on root mustard at 262.5g a.i. ha-1 in accordance with good agricultural practice (GAP), respectively. After the final application, the root mustard samples were collected at 3, 7, and 14days. Fluazinam residues in root mustard were less than 0.01-0.493mgkg-1. The dietary risk of fluazinam was predicted by comparing intake amounts with the toxicological data, namely acceptable daily intake (ADI) and acute reference dose (ARfD). The risk quotient (RQ) was 72.2-74.3%, for ordinary consumers, which showed negligible risk. According to the maximum residue limit (MRL) and dietary risk assessment, it is suggested that the pre-harvest interval (PHI) of 3days; meanwhile, the MRL of 2mgkg-1 was suggested for fluazinam in root mustard, which indicates that the dietary risk of fluazinam 500g L-1 suspension concentrate (SC) with the recommended usage on root mustard is negligible. This study provided basic data on the use and safety of fluazinam in root mustard to help the Chinese government formulate a maximum residue level for fluazinam in root mustard.

Impact of Matrix Species and Mass Spectrometry on Matrix Effects in Multi-Residue Pesticide Analysis Based on QuEChERS-LC-MS

With the popularity of multi-residue pesticide analysis based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) cleanup and liquid chromatography-mass spectrometry (LC-MS), matching optimal matrix-matched calibration protocols and LC-MS conditions to reduce matrix effects (MEs) has become a crucial task for analysts in their routines. However, dozens to hundreds of pesticide analytes in a single run generate increasingly multi-dimensional ME data, requiring appropriate tools to handle these data sets. Therefore, we established an ME analysis strategy by drawing on analytical thinking and tools from metabolomics analysis. Using this, matrix species-induced and mass spectrometry-induced systematic ME variations were distinguished, and pesticides contributed to the variations were scanned out. A simultaneous weakening of MEs on 24 pesticides in 32 different matrices was achieved using the time-of-flight-mass spectrometry (TOF-MS) scan under the information-dependent acquisition (IDA) mode of high-resolution mass spectrometry (HR-MS), compared to multiple reaction monitoring (MRM) scanning by tandem mass spectrometry (MS/MS). Bay leaf, ginger, rosemary, Amomum tsao-ko, Sichuan pepper, cilantro, Houttuynia cordata, and garlic sprout showed enhanced signal suppression in the MRM scan for 105 differential MRM transitions for 42 pesticides and in IDA mode for 33 pesticides, respectively. This study revealed the interference of matrix species and mass spectrometry on MEs and provided a novel strategy for ME analysis.

Analysis of polychlorinated biphenyls (PCBs) in dairy products by modified QuEChERS/GC-QqQ-MS/MS method: A risk assessment study.

Polychlorinated biphenyls (PCBs) are harmful chemicals that are persistent in the environment and can accumulate in the food chain. The purpose of the present research was to assess non-dioxin-like polychlorinated biphenyls (NDL-PCBs) in some dairy products (yogurt, doogh, and kashk) using modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique and gas chromatography-triple-quadrupole mass spectrometry (GC-QqQ-MS/MS) method and risk assessment study. The LOQs (limit of quantifications), LODs (limit of detections), recovery, and RSD for the PCB analytes were 0.180-0.360, 0.06-0.12 ng/g fat, 97.45-102.63%, and 6.33-8.86%, respectively. The results revealed that the mean concentrations of Ʃ6-NDL-PCBs in samples were 15.17 ± 3.44 ng/g fat, which was lower than the standard level established by European Union (EU, 40 ng/g fat). The maximum mean level was PCB 180 (9.98± 2.04 ng/g fat) and the minimum mean level of PCBs in samples was PCB 28 (0.09± 0.06 ng/g fat). Also, results showed that kashk samples had a maximum mean level of 6-NDL-PCBs (18.66 ± 2.42 ng/g fat) and doogh samples had a minimum mean level of 6-NDL-PCBs (12.21 ± 2.22 ng/g fat). The mean level of 6-NDL-PCBs in yogurt samples was 14.65 ± 2.02 ng/g fat. The heat map results showed the correlation between the spectral indices of 6-NDL-PCBs in different dairy products. According to the Monte Carlo method, risk assessment was done using calculating the Estimated Daily Intake (EDI) and Incremental Life Cancer Risk (ILCR). The EDI values of 6 NDL-PCBs based on the 95th percentile in yogurt, doogh, and kashk were 14.3, 1.49, and 0.5ng/kg.day, respectively. Considering that the contaminant level in the samples is lower than the EU limit, it can be concluded that dietary exposure to 6 NDL-PCBs may not pose a risk to the health of consumers.

Residue analysis and dietary risk assessment of thiamethoxam, flonicamid and their metabolites in cucumber under field conditions in China.

Thiamethoxam and flonicamid are two representative insecticides of neonicotinoids which are used to treat cucumber aphids, causing food safety and human health problems. A 60% thiamethoxam-flonicamid commercial mixture water dispersible granule (WDG) is being prepared for registering in China, so it is essential to investigate the residue levels of these neonicotinoids and their metabolites in cucumber and evaluate the dietary risks of these insecticides. We developed a modified quick, easy, cheap, effective, rugged and safe (QuEChERS) method combined with high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) for the simultaneous determination of thiamethoxam and its metabolite clothianidin, flonicamid and its metabolites 4-trifluoromethylnicotinic acid (TFNA), 4-trifluoromethilnicotinamide (TFNA-AM), 4-(trifluoromethyl) nicotinol glycine (TFNG) in cucumber. Method validation indicated good selectivity, linearity (r ≥ 0.9996), accuracy (recoveries of 80-101%), precision (relative standard deviations (RSD) ≤ 9.1%), sensitivity (limits of detection (LOD), 0.28-1.44 × 10-3mg/L; limits of quantification (LOQ), 0.01mg/kg) and minor matrix effect (ME) ( ≤|± 5%|). In the terminal residue trials under good agricultural practice (GAP) conditions, the residue levels of six analytes in cucumber samples were ˂0.01-0.215mg/kg after application trice with an interval of 7days based on pre-harvest interval (PHI) of 3days under the high recommended dosage of 54g active ingredient/ha (g a.i./ha). Relevant toxicological, residual chemistry parameters and dietary consumption of the residents were applied to assess the potential risk of dietary exposure. The chronic and acute dietary exposure assessment risk quotient (RQ) values were less than 1. The above results indicated that the potential dietary intake risk of this formulation was negligible to consumers.

Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee Pollen.

Pesticides can be found in beehives for several reasons, including contamination from surrounding crops or for their use by beekeepers, which poses a risk to bee ecosystems and consumers. Therefore, efficient and sensitive methods are needed for determining pesticide residues in bee products. In this study, a new analytical method has been developed and validated to determine seven acaricides (atrazine, chlorpyrifos, chlorfenvinphos, α-endosulfan, bromopropylate, coumaphos, and τ-fluvalinate) in bee pollen using gas chromatography coupled to mass spectrometry. After an optimization study, the best sample treatment was obtained when using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method employing an ethyl acetate and cyclohexane as the extractant mixture, and a mixture of salts for the clean-up step. A chromatographic analysis (<21 min) was performed in an Agilent DB-5MS column, and it was operated under programmed temperature conditions. The method was fully validated in terms of selectivity, limits of detection (0.2-3.1 µg kg-1) and quantification (0.6-9.7 µg kg-1), linearity, matrix effect (<20% in all cases), trueness (recoveries between 80% and 108%), and precision. Finally, the proposed method was applied to analyze commercial bee pollen samples, and some of the target pesticides (chlorfenvinphos, α-endosulfan, coumaphos, and τ-fluvalinate) were detected.

Concentration levels and risk assessment of organochlorine and organophosphate pesticide residue in selected cereals and legumes sold in Anambra State, south-eastern Nigeria

Abstract The levels of organochlorine and organophosphate pesticide residues in selected cereal crops (beans, cowpea, millet, maize, sorghum, and rice) purchased from major markets in Anambra, south-eastern Nigeria, were assessed and compared with established MRLs. The QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used for extraction and clean-up of pesticide residues. Thereafter detection and quantification were done using GC/MS. The result reveals that the analysed grain samples contained some organochlorine pesticides and organophosphates. The organochlorine was most dominant followed by the organophosphates. Organochlorine pesticide residues varied from 0.048 to 0.298 mg/kg in beans, BDL to 0.398 mg/kg in cowpea, 0.018–0.337 mg/kg in maize, 0.023–0.375 mg/kg in millet, 0.058–0.415 mg/kg in sorghum and 0.045–0.442 mg/kg in rice while organophosphate pesticide residue varied from BDL to 0.315 mg/kg in beans, BDL to 0.113 mg/kg in cowpea, BDL to 0.228 mg/kg in maize, BDL to 0.253 mg/kg in millet, BDL to 0.218 mg/kg in sorghum and BDL to 2.1 35 mg/kg in rice. Highest concentration of endosulphan II (0.442 mg/kg) was detected in rice, followed by aldrin (0.415 mg kg−1) in sorghum and endosulphan II (0.40 mg/kg) in sorghum. The pesticide toxicity index (PTI) was above one (1), whereas health index (HI) was less than one (1) and cancer risk were within USEPA reference guideline for crops indicating children will have greater health effect than adults. Hence, strict monitoring and control of pesticide residues in agricultural products is advocated.

Concentration evaluation and risk assessment of pesticide residues in selected vegetables sold in major markets of Port Harcourt South-South Nigeria

Abstract Concentration levels and health risk assessment of residues of organochlorine and organophosphate pesticides in four commonly vegetables (Cucumber, carrot, cabbage, and eggplant) collected from major markets of Port Harcourt city, South-south Nigeria were assessed. The collected samples were analysed using QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction method by gas chromatography coupled with Electron Capture Detector (ECD). Pesticide concentrations were compared with UK/EU maximum residual limits (MRLs). Health risk estimates were analysed using estimated daily intake (EDI), hazard quotient (HQ), and hazard ratio (HR) for children (16.7 kg) and adults (60 kg) weight groups. The results of this study showed that 80% of the vegetable samples contained detectable pesticide residues, of which 70% had residues that exceeded MRLs while 20% had residues below detectable levels. The highest concentrations of HCH residues are present in cabbage with a concentration of 0.25 ± 0.15 mg/kg for α-HCH while the least are present in eggplant with concentration of 0.038 ± 0.025 mg/kg in lindane. Pirimophos-methyl was detected in cucumber at 0.017 mg/kg while parathion and isofenfos was detected only in eggplants at concentration of 0.042 mg/kg and 0.022 mg/kg respectively. Concentrations of parathion, chlorpyrifos, and pirimophos-methyl residues were lower than MRLs in all the detected vegetable samples analysed. Non-carcinogenic health risk estimates for the children consumer groups showed that mevinfos, p, pʹ DDD, aldrin, and heptachlor epoxide detected in eggplant, carrot, and cabbage had HQ &gt; 1. While for adults, only p, pʹ DDD and heptachlor epoxide revealed non-carcinogenic effect in cabbage. Risk was highest for child consumers. However, most of the pesticide residues were less than 1 for the HQs value which is indicative of insignificant health risk. Human risk estimations for the carcinogenic health effect for the studied vegetables showed that lindane and delta HCH could pose carcinogenic health risks to adult, while aldrin, dieldrin, heptachlor, α HCH, β HCH, delta HCH, and heptachlor epoxide could pose carcinogenic health risks to children. The HRI values in some of the detected residues indicate that the cancer benchmark concentrations exceeded the EDI for the respective organochlorine pesticide in the vegetable samples, thus raising serious concerns of possible carcinogenicity. Non carcinogenic and carcinogenic risk assessment of organochlorine pesticide residues in the studied vegetable indicates health threat. Hence, strict monitoring and control of pesticide residues in agricultural products is being suggested, to protect consumers, especially the children who are vulnerable to the adverse effects of pesticides.

Quantification of 363 Pesticides in Leafy Vegetables (Dill, Rocket and Parsley) in the Turkey Market by Using QuEChERS with LC-MS/MS and GC-MS/MS

Contamination of agricultural products with pesticide residues is a growing concern due to their adverse health effects and increasing worldwide usage of pesticides. In 2021 a total of 200 samples of green leafy vegetables, including 80 dill, 80 rocket and 40 parsley, purchased from greengrocer shops, markets and bazaars in Corum Province, Turkey, were monitored for pesticide residues. In green leafy vegetables, 363 pesticides were analyzed using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation, followed by liquid chromatography coupled to mass spectrometry (LC-MS/MS) for 311 residues and gas chromatography coupled to mass spectrometry (GC-MS/MS) for 52 residues. The method was in-house validated at two fortification levels, and satisfactory recoveries and precisions were achieved for all residues. No quantifiable residues were found in 35% of the samples, whereas 43 residues belonging to 24 different chemical classes were detected in 130 green leafy vegetables. Among the green leafy vegetables, the highest occurrence frequency was recorded in the rocket, followed by dill and parsley. In 46% of the green leafy vegetables, the residue levels exceeded European Union Maximum Residue Levels (EU MRLs). The most frequently detected pesticides were pendimethalin (22.5%), diuron (38.7%) and pymetrozine (52.5%) in dill, rocket and parsley, respectively.

Residue analysis of selected organophosphorus and organochlorine pesticides in commercial tomato fruits by gas chromatography mass spectrometry

In this study, analysis of some selected organophosphorus and organochlorine pesticides was carried out in tomato samples collected from the markets of Mettu town, Ilu Aba Bora Zone, Oromia, Ethiopia. The quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was used for the extraction of collected samples using acetonitrile with 1% acetic acid, anhydrous magnesium sulfate, and anhydrous sodium acetate, followed by dispersive solid-phase extraction (d-SPE). Chromatographic separation and quantitative determination of the pesticides were performed by gas chromatography equipped with a mass spectrometer. The calibration curves for each analyte constructed in tomato samples were linear in the concentration range of 2–200 μg/kg with R2 > 0.99 and the LODs and LOQs of the method were in the range of 0.01–0.04 μg/kg and 0.04–0.13 μg/kg, respectively. The recovery and precision study results were within acceptable standard guidelines. Of the fourteen pesticides tested, chlordane, hexachlorobenzene, 4, 4'-DDE, 4, 4'-DDD, 4, 4'- DDT, and profenofos were detected at 0.15, 0.09, 0.17, 0.032, 1.24 and 0.062 μg/kg, respectively. Despite the concentrations of the detected pesticides being lower than the maximum residue limit recommended by FAO/WHO, the presence of these toxic chemicals in tomatoes indicates product contamination and requires extensive further investigation with the inclusion of other pesticides.

Accurate Determination of Pesticide Residues in Milk by Sonication-QuEChERS Extraction and LC-LTQ/Orbitrap Mass Spectrometry

A modified, quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction procedure combined with sonication and Ultra-High Performance Liquid Chromatography–Orbitrap-Mass Spectrometry (UHPLC–Orbitrap-MS) was developed as a sensitive and reliable methodology for the determination of multiclass pesticides in full-fat milk. Different amounts of EMR-lipid sorbent were assayed for the cleanup step in order to achieve both acceptably high recoveries and low co-extractives in the final extracts. Accurate mass measurements of the analyte’s pseudo-molecular ions and tandem MS fragmentation were used to quantify and identify the target pesticides. Analytical performance characteristics of the method, such as linearity, recovery, precision, the limit of detection (LOD) and quantification (LOQ), matrix effects (ME), and expanded uncertainty, have been determined for method validation fulfilling all criteria for its use as a validated routine method. The method was successfully applied to real samples (by local farms and commercial), revealing the presence of carbendazim in one milk sample at a concentration level below the maximum residue limits.

Simultaneous Rapid Determination of Seven Alternaria Toxins in Tuberous Crops during Storage Using QuEChERS Coupled with Ultrahigh-Performance Liquid Chromatography-Tandem Mass Spectrometry

Robust and sensitive ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was applied for the detection of seven Alternaria toxins (ATs) in tuberous crops. The influence of tuber conditions (fresh, germinated, and moldy) during storage on the concentration of the seven ATs is also investigated. ATs were extracted with acetonitrile under acidic conditions and purified with a C18 adsorbent. ATs were scanned with electrospray ionization (positive/negative ion) dynamic switching and detected in MRM mode. Calibration curve analysis results reveal good linear relationships in all toxin concentration ranges (R2 > 0.99). The limit of detection and limit of quantification were 0.25-0.70 and 0.83-2.31 μg/kg, respectively. The average recoveries of the seven ATs were 83.2-104% with intra-/inter-day precision at 3.52-6.55% and 4.02-7.26%, respectively. The developed method provided adequate selectivity, sensitivity, and precision in detecting the seven ATs at trace levels, and dispensed with standard addition or matrix-matched calibration to compensate for matrix effects. ATs in the fresh, germinated, and moldy samples of tuberous crops in storage (taro, potato, sweet potato, yam, cassava) were analyzed with this method, and the concentrations were 2.01-14.51 μg/kg and significantly increased with storage duration. ALS was detected in most samples, whereas no quantities of ALT and ATX-I were detected. AME was often detected in combination with AOH in sweet potatoes. TeA and Ten were mostly detected in taro, potato, and yam. The established method could be used for the simultaneous detection and quantification of multicomponent toxins in elaborate matrices.

Graphene-Type Materials for the Dispersive Solid-Phase Extraction Step in the QuEChERS Method for the Extraction of Brominated Flame Retardants from Capsicum Cultivars.

A new application of graphene-type materials as an alternative cleanup sorbent in a quick, easy, cheap, effective, rugged, and safe (QuEChERS) procedure combined with GC-ECD/GC-MS/GC-MS/MS detection was successfully used for the simultaneous analysis of 12 brominated flame retardants in Capsicum cultivar samples. The chemical, structural, and morphological properties of the graphene-type materials were evaluated. The materials exhibited good adsorption capability of matrix interferents without compromising the extraction efficiency of target analytes when compared with other cleanups using commercial sorbents. Under optimal conditions, excellent recoveries were obtained, ranging from 90 to 108% with relative standard deviations of <14%. The developed method showed good linearity with a correlation coefficient above 0.9927, and the limits of quantification were in the range of 0.35-0.82 μg/kg. The developed QuEChERS procedure using reduced graphite oxide (rGO) combined with GC/MS was successfully applied in 20 samples, and the pentabromotoluene residues were quantified in two samples.

Dissipation kinetics, risk assessment, and waiting period of spiromesifen on chili fruits using gas chromatography-electron capture detector.

A supervised field trial was designed in Rajasthan Agricultural Research Institute, Durgapura, Jaipur, Rajasthan, to assess the dissipation and persistence of spiromesifen in chili fruits. Spiromesifen (22.9% suspension concentrate) was sprayed two times at an interval of 10 days at the recommended dose (96 g. a.i. ha-1 ) and double the recommended dose (192 g. a.i. ha-1 ) with four replications. Sampling was done according to the planned interval of days after the second spray. Extraction and cleanup were performed using the modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method and the spiromesifen residue was analyzed by GC-electron capture detector and confirmation performed using GC-MS. The average initial deposit of spiromesifen was 1.207 mg kg-1 and 1.948 mg kg-1 at the recommended and double the recommended dose, respectively. The half-life values of spiromesifen ranged between 2.7 and 3.2 days at the recommended and double the recommended dose. The safe waiting period was calculated for the respective doses and it was concluded that an average of 7 days is safe for picking. The FSSAI (Food Safety and Standards Authority of India) have set the maximum residue limit of 0.1 mg kg-1 for spiromesifen in green chili. The theoretical maximum residue contribution value of spiromesifen was lower than the maximum permissible intake at both the applications on the 0th day. Hence, there will be no adverse effects on human health after consumption of green chilies.

Screening and quantification of pesticide residues in ciders by liquid chromatography-high resolution mass spectrometry

The present study aimed to apply a multi-residue method for the screening and quantification of pesticide residues in ciders, low alcoholic beverages made by fermentation of apple juice. Twenty bottled craft cider samples purchased from the Czech market were analysed for pesticide residues. The residues of pesticides were extracted from samples using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure in combination with additional solid-phase extraction (SPE) sample clean-up to achieve the lowest detection limit possible. In this study, targeted screening of pesticide residues in the samples was performed with the Q-Orbitrap mass spectrometry instrument. We identified 18 pesticides in cider samples analysed by screening method using an accurate-mass database of about 500 pesticide compounds, including their retention times, empirical formulas, and characteristic fragments. Additionally, liquid chromatography with high-resolution tandem mass spectrometer (LC-HRMS/MS) was used for re-analysis of positive findings of pesticides in samples and allowed to quantify compounds of interest at 0.2 µg L–1 concentration level. The monitoring scheme was applied to the set of craft ciders, and the results revealed the presence of pesticide residues in most of the samples at trace levels ranging from 0.5 to 5 µg L–1 and rarely at a level higher than 10 µg L–1.

Pesticide Residues and Effect of Household Processing in Commonly Consumed Vegetables in Jimma Zone, Southwest Ethiopia.

The long-term and indiscriminate use of pesticides has resulted in serious health effects. Aside from that, developing countries do not have any monitoring systems in place to prevent the consumption of high levels of pesticides in foods. Therefore, this study aimed to determine pesticide residues and the effect of processing in commonly consumed vegetables in the southwestern part of Ethiopia. In total, 12 samples of 1 kg of each type of vegetable were collected from selected markets. Moreover, as a solution to pesticide residue problems in vegetables, the effect of different processing methods such as washing, peeling, boiling, and their cumulative effect was studied. In the analytical procedure, the modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction with florisil as a cleanup sorbent was used and the identification of pesticides was done by using gas chromatography with an electron capture detector (GC-ECD). The parent p,p'-DDT was detected at a concentration of 0.015 mg/kg in potato samples from the Serbo market and a concentration of 0.516, 0.232, 0.174, and 1.512 mg/kg in Merkato, Kochi, Serbo, and Shebe onion samples, respectively. P`p-DDT is detected at a high concentration compared to its metabolites (p,p'-DDE and p,p'-DDD), which is an indication of recent use. DDT and its metabolites, other organochlorines (lindane, γ-chlordane, dimethachlor, and heptachlor), and pyrethroids (cypermethrin and deltamethrin) exceeded the recommended limits by FAO and WHO in multiple samples of potato, onion, and cabbage. The processing result showed that washing, boiling, and the combination of the two revealed a 100% reduction in o,p'-DDT, and p,p'-DDT pesticides detected in cabbage. In conclusion, multiple residues were detected in the three vegetables studied, indicating that pesticides were applied intensively. Pesticide levels were reduced by home processing procedures, which is important for consumer safety.

Assessment of pesticide residues in vegetables selected from different Egyptian governorates

This study aimed to assess the levels of contamination by pesticide residues in several types of vegetables collected from different regions in Egypt. A total of 100 samples of vegetables (pepper, tomato, cucumber, and strawberry) were collected from markets in five cities (Al-Obour, Al-Salheia El-Gadida, Giza, Zagazig, and Fayed) and analyzed for the presence of 42 different pesticide residues. The Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was used to extract the target pesticides, which were then quantified using Gas Chromatography-Mass Spectrometry (GC-MS/MS) and Liquid Chromatography-Mass Spectrometry (LC-MS/MS) techniques. The results showed that 72% of the vegetable samples contained detectable levels of pesticide residues, with 21% exceeding the European Union Maximum Residue Levels (EU-MRLs) and 51% containing residues below the MRLs. The detected residues were primarily insecticides (56.4%) and fungicides (43.6%), with tomato and strawberry samples showing the highest frequency of both types of pesticides. Tomato also had the highest absolute intake from consumption (2.89 g/kg BW/day), followed by strawberries, peppers, and cucumbers (0.47, 0.159, and 0.096 g/kg BW/day, respectively). A hazard index (HI) was used to assess the dietary risk posed by the pesticide residues, with tomato having the highest contribution value. These findings highlight the need for Integrated Pest Management (IPM) programs to reduce the excessive use of pesticides, particularly in relation to raw food commodities. Action is required to minimize the unacceptable risks identified in this study.

QuEChERS-Based Approach to the Extraction of Five Calcium Channel Blockers from Plasma Determined by UPLC-MS/MS.

Here, a QuEChERS (quick, easy, cheap, effective, rugged, and safe) pretreatment method was combined with UPLC-MS/MS to facilitate the rapid and reliable simultaneous detection of five calcium channel blockers (CCBs) in human plasma. For this approach, samples were treated with 1 mL of acetonitrile, 350 mg of magnesium sulfate, and 70 mg of PSA adsorbent prior to centrifugation. Supernatants then underwent gradient elution for 8 min with an Agilent C18 column using an acetonitrile-water solution supplemented with 5 mmol⋅L-1 of ammonium acetate. This technique exhibited a good linear response in the 1-800 ng⋅mL-1 range for the analyzed drugs, with an R2≥ 0.9921, an accuracy of 87.54-113.05%, a matrix effect (ME) of 91.21-116.39%, a precision of 0.19-11.64%, and stability of no more than 10.05%. This time-saving QuEChERS reagent-based pretreatment technique thus allowed for the simultaneous and accurate detection of five CCBs in human plasma samples, providing a promising new basis for therapeutic drug monitoring in patients with hypertension.

Terminal residue of fungicides in agro-products from north China: Assessment of human exposure potential

The excessive and unreasonable use of fungicides can inevitably lead to increased residues in food and ultimately cause harm to human health. To detect the residues of 8 fungicides in agro-products from 2018 to 2021 in Hebei province China, the method with modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) by Ultra performance liquid chromatography coupled to tandem mass spectroscopy (UPLC-MS/MS) was developed. The analytical methods were validated with respect to matrix effect, recovery, calibration curves, limit of detection (LOD), and limit of quantification (LOQ). With the developed method, 78 samples collected from 13 vegetable categories were analyzed. The number of samples analyzed at concentrations above the LOQ (1.13 μg/kg to 7.70 μg/kg) was ranging from 5 to 18. The detection rate of metalaxyl, mepanipyrim and triazolone are the lowest among the tested fungicides, and the tebuconazole is the highest. In all 13 vegetable categories, the largest types of fungicides were detected in celery samples. The risk quotient (RQ) of difenoconazole was the highest and the RQ of dimethomorph was the lowest. The RQs of fungicide in vegetables were all less than 100 %. In this study, we have revealed that the residues of eight fungicides shown a low risk to human health.