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

Quantitative analysis of erythromycin, its major metabolite and clarithromycin in chicken tissues and eggs via QuEChERS extraction coupled with ultrahigh-performance liquid chromatography-tandem mass spectrometry

A simple, rapid and novel method involving ultrahigh-performance liquid chromatography-electrospray ionization tandem triple quadrupole mass spectrometry (UHPLC-ESI–MS/MS) was developed to simultaneously detect erythromycin, its major metabolite and clarithromycin in chicken tissues (muscle, liver and kidney) and eggs (whole egg, albumen and yolk). Samples were extracted using acetonitrile–water (80:20, v/v), and a a Cleanert MAS-Q cartridge was used to perform quick, easy, cheap, effective, rugged, and safe (QuEChERS) purification. The average recoveries were 87.78–104.22 %, and the corresponding intraday and interday relative standard deviations were less than 7.10 %. The decision limits and detection capabilities of the chicken tissues and eggs were 2.15–105.21 μg/kg and 2.26–110.42 μg/kg, respectively. For chicken tissues and eggs, the limits of detection and limits of quantification were 0.5 μg/kg and 2.0 μg/kg, respectively. The proposed method was successfully employed to analyse real samples, demonstrating its applicability.

Quantitative determination of residue amounts of pesticide active ingredients used in grapes by LC-MS/MS and GC-MS/MS devices and evaluation of these pesticides in terms of public health.

The aim of this study was to quantitatively determine pesticide residues in grapes, one of the most produced and consumed fruits in Turkey and in the world. A total of 226 active ingredients were analyzed in 21 samples collected from Southeastern and Eastern Anatolia regions using QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction method and multiple residue analysis technique and LC-MS/MS and GC-MS/MS devices. In 11 out of 21 samples (52.4%), no active ingredient was detected, while at least one active ingredient was detected in 10 samples (47.6%). Thirteen different active substances (Ametoctradin, Azoxystrobin, Boscalid, Diphenoconazole, Dimethomorph, Fenhexamid, Fluopyram, Flutriafol, Metalaxyl- Metalaxyl-M, Metrafenone, Tebuconazole, Trifloxystrobin) were detected in the samples. The top 3 most detected active substances were Boscalid-Azoxystrobin and Fluopyram, respectively. The active ingredients were found between 0.015 and 0.499 mg kğ-1 values.

Development and validation of an analytical method based on QuEChERS followed by UHPLC–ToF-MS for the determination of tropane alkaloids in buckwheat (Fagopyrum esculentum L.) and buckwheat products

A method was developed for the determination of tropane alkaloids (TAs), including atropine, scopolamine, anisodamine and homatropine in buckwheat and related products. This work presents an optimised methodology based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction procedure followed by ultra-high performance liquid chromatography combined with time-of-flight mass spectrometry for the determination of TAs (atropine, scopolamine, anisodamine and homatropine) in buckwheat samples. The analytical methodology was successfully validated, demonstrating good linearity, low limit of quantification, repeatability (RSDr < 15%), inter-day precision (RSDR < 19%) and recovery (74–113%). Finally, 13 commercial samples of buckwheat were analysed and the results demonstrated that they were in compliance with the current European regulations regarding TAs.

Optimization of the QuEChERS Extraction of Mycotoxins in Maize Using Response Surface Methodology (RSM)

AbstractSeveral methods have been developed for the analysis and detection of mycotoxins in food; however, most do not make use of critical statistics and mathematical tools for precise optimization. This study developed, optimized, and validated a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction procedure for the extraction of multiple mycotoxins in maize and subsequent validation using liquid chromatography tandem mass spectrometry (LC–MS/MS). Central composite design (CCD) was used to optimize extraction conditions. Data analysis of full factorial screening experiments revealed that MeCN (%), FA (%), and extraction time significantly affected the mycotoxins recovery. Assessment of the statistical significance of the generated model using analysis of variance (ANOVA), coefficient tables, and surface plots showed the relative interactions of factors and the adequacy of the model. Thus, P values from the lack of fit (LOF) test ranged from 0.137– 0.467 and a composite desirability function of 0.91 was obtained. Using the optimum extraction conditions of 0.1% (v/v) FA in 80.2% MeCN for 74 min, 10 mycotoxins were effectively extracted with satisfactory recoveries (85–114%), coefficients of regression (R2 &gt; 0.98), coefficients of variation (CVs &lt; 15%), limit of quantifications (LOQs) (0.33–60.45 µg/kg), and other associated method validation parameters. The method validation was carried out according to Commission Implementing Regulation 2021/808 and Commission Regulation (EC) No 401/2006 of 23 February 2006. Application of this method to 20 maize samples collected from markets in Botswana showed detectable mycotoxins in 13 samples, with 2 exceeding the European Union (EU) maximum aflatoxin B1 (AFB1) limit, suggesting potential exposure to high levels of toxic mycotoxins in Botswana.

Simultaneous Quantification of Two Neonicotinoids Using QuEChERS-LC-MS/MS in Moroccan Spearmint (Mentha Spicata.L): Qualimetry of the Method by Uncertainty Estimation Using Generalized Pivotal Quantities Approach and Monte Carlo Simulation.

Neonicotinoids (NEOs) are used for the phytosanitary treatment of Mentha Spicata.L crops, and this practice requires precise control of these harmful substances at very low concentrations. The objective of this study is to apply an approach allowing simultaneously validation and evaluation of measurement uncertainty based on total error methodology, in order to accurately quantify the presence of two NEOs in Mentha Spicata.L utilizing a Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS)-LC-MS/MS methodology. The quantification of imidacloprid and acetamiprid employing a QuEChERS extraction method, coupled with LC-MS/MS, ensuring the accuracy of the analytical method and managing the risks associated with its routine use.A complete and exhaustive validation approach based on the "β-content, γ-confidence" tolerance interval was used for the uncertainty assessment, using the generalized pivot quantity (GPQ) concept and Monte Carlo simulation, which avoids the need for additional data while achieving intermediate precision for each concentration level within predetermined acceptable limits. The validation procedure is based on the choice of a quadratic model for the two NEOs, allowing the validation of acetamiprid and imidacloprid by LC-MS/MS assay within the range of working concentration. The flexibility of the uncertainty profile intervals was demonstrated with a variation in β-content values (66.7, 80, and 90%) and risk values (10 and 5%), which remained within the acceptability limits of 20%, and the relative expanded uncertainty did not exceed 15 and 11%. A QuEChERS-LC-MS/MS method for the analysis of two NEOs has been successfully fully validated using the uncertainty profile strategy. Implementation of an overall validation strategy, which involves both the validation and uncertainty assessment known as the uncertainty profile, for the quantification of two important NEOs in Mentha Spicata.L using QuEChERS-LC-MS/MS. This qualimetric approach has been conducted by computing the measurement uncertainty of the method utilizing data from analytical validation under conditions of intermediate precision at each level of concentration without additional effort. After that we have demonstrated the flexibility of this strategy for the LC-MS/MS quantification of acetamiprid and imidacloprid, using a decision tool that enables the choice and modification of β-content and γ-confidence values.

Quantitative SERS detection of aflatoxin B1 in edible crude palm oil using QuEChERS combined with chemometrics

Aflatoxin B1 (AFB1) is a potent carcinogen whose presence in food threatens consumers. This study aimed to develop a rapid method for the quantitative detection of AFB1 in crude palm oil (CPO) using novel gold nanoparticles (AuNPs) and the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique, combined with chemometrics. The bootstrapping soft shrinkage-partial least squares (BOSS-PLS) algorithm yielded the most favorable results, with an Rc of 0.9929, RMSECV of 0.204 ng/g, and an RPD of 3.93. The results demonstrated that the developed method is highly accurate, sensitive, and specific for detecting AFB1 in CPO, with a low limit of detection (LOD) of 0.00092 ng/g. The results underscore the potential of employing a combination of AuNPs, QuEChERS extraction, and chemometrics for detecting AFB1 in CPO. The developed method can be employed to monitor and ensure the quality of CPO, thereby preventing the spread of AFB1 contamination in the food industry.

Evaluation of the QuEChERS extraction approach for the analysis of active compounds of pharmaceuticals in olive tree portions

BackgroundA modified version of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method has been tested for quantifying six active compounds of pharmaceuticals (PhACs), i.e., two different antibiotics, two anti-inflammatories, one antifungal, and one anti-depressant, extracted from roots, leaves and stems, pulp, pits, and oil obtained from olive trees. The different matrices have been polluted with all contaminants at 25, 50, and 250 µg L−1 and the recoveries were determined by liquid chromatography tandem–mass spectrometry. The validation of the method has been carried out by determining linearity, recovery, precision, limits of detection (LODs), and limits of quantification (LOQs) values. A matrix-matched calibration for each matrix has been adopted in order to avoid the matrix effect at the aforementioned levels of fortification.ResultsThe recoveries of PhACs from the different matrices were always above 70% and the relative standard deviation (RSD) always ≤ 20%, conditions required for the validation of the method. The LOD and LOQ values were always lower than 25 µg L−1, i.e., always lower than the minimum concentration used in the experiment; therefore, the method can be validated at 25, 50, and 250 µg L−1.ConclusionsThis method can represent a valid alternative to the traditional extraction methods to quantify pharmaceuticals extracted also from fatty matrices.Graphical

Algerian Workers' Exposure to Mycotoxins-A Biomonitoring Study.

Mycotoxins, produced by fungi as secondary metabolites, have the potential to induce both short-term and long-term toxic consequences in animals and humans. The present study aimed to determine multi-mycotoxin levels in Algerian workers using urine as the target. A method based on a QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction procedure followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was optimized and validated for the determination of eleven mycotoxins in 96 urine samples. Different sorbents were tested to be used in the dispersive solid-phase extraction (d-SPE) cleanup step of QuEChERS. The final method was fit-for-purpose and showed good analytical performance in terms of specificity, linearity, and precision. All samples contained at least two mycotoxins, and toxin-2 (T-2) was the most common, being found in 92.7% of the samples, followed by zearalenone (ZEN) in 90.6% of positive samples, and ochratoxin A (OTA) in 86.4%. T-2 levels ranged from 0.3 μg/L to 36.3 μg/L, while OTA ranged from 0.3 μg/L to 3.5 μg/L, and ZEN ranged from 7.6 μg/L to 126.8 μg/L. This was the first mycotoxin biomonitoring study carried out in the Algerian population. The findings highlight the need for accurate data for better risk assessment and for the development of better regulation to manage mycotoxin contamination in this country.

Quantitative determination of polychlorinated biphenyls in chicken based on QuEChERS extraction and GC-MS/MS detection

Polychlorinated biphenyls (PCBs), a class of synthetic organic compounds consisting of chlorine atoms on two coupled biphenyl rings, have been declared class A carcinogens by the World Health Organization. Here, we report a new method for the determination of PCBs content in chicken. The method employs QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction, followed by gas chromatography and tandem mass spectrometry (GC-MS/MS) detection for the identification and quantification of seven indicative PCBs (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153, PCB180). The PCBs were extracted by acetone with an Association of Official Analytical Chemists (AOAC) extraction kit, followed by a clean-up step using primary secondary amine, octadecyl silica, florisil, and anhydrous magnesium sulfate. PCBs in the extracts were subsequently quantified by GC-MS/MS. The method was validated, and the correlation coefficients of the curves were found to be higher than 0.99. The limits of detection for the seven indicative PCBs ranged from 0.1 to 0.5 ng/g, and the limits of quantification were 0.3–1.5 ng/g. Satisfactory recovery rates ranged from 96% to 115%, with a maximum relative standard deviation of 9%. For simple pretreatment and accurate detection, this method is quick and efficient in detecting batches of seven indicative PCBs in chicken.

Quantification of PFAS in Oyster Tissue Using a Rapid QuEChERS Extraction Followed by UPLC-MS/MS Analysis

Per- and poly-fluoroalkyl substances (PFAS) are a large group of man-made chemicals that repel oil, stains, grease, and water and are fire resistant. PFAS are known to be persistent in the environment and bioaccumulate in human and animal tissue, soil, and water. To mitigate human exposure to these chemicals, PFAS analysis by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was used to monitor their presence in the environment. This study focused on analyzing oysters harvested from coastal New England for 14 PFAS. The validated method addressed in this study utilized a quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach using various sorbents and showed that the combination of primary secondary amine/graphitized carbon black (PSA/GCB) provided the most effective sample clean-up prior to analysis. The recoveries for the targeted analysis ranged from 61% to 116.3% with relative standard deviations from 2.4% to 13.3% at the 125.0 ng mL−1 analyte level. The method detection limits were from 0.33 ng g−1 to 6.75 ng g−1. In a targeted analysis of five unknown samples, two samples had a detectable level of the legacy compound, perfluorooctanesulfonic acid (PFOS).

Optimization of the QuEChERS extraction method to determine Polycyclic Aromatic Hydrocarbons (PAHs) in powder aerosol particles collected by cyclone

Conventional methods for collecting and extracting aerosol particles are challenging in accurately characterizing particle-bound polycyclic aromatic hydrocarbons (PAHs) contamination and conducting cellular exposure studies. Therefore, developing direct aerosol sample collection and simple pretreatment analytical methods is necessary. This study describes the optimization of the QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction method for the determination of PAHs in powder-form environmental standard materials (SRM1944) and proves it is also effective for analyzing PAHs in powder aerosol particle samples collected by cyclone. In this study, we used an I-optimal design response surface method combined with a desirability function to investigate the extraction effect of PAHs under different combinations of QuEChERS extraction factors, including extraction solvent, salt, and clean-up reagent. The optimized conditions of the method were determined using the 2-factor interaction (2FI) model combined with boundary conditions, resulting in acetonitrile/dichloromethane (7:1, v/v), Na2SO4/NaCl (1:1, w/w), and primary and secondary amine (PSA) as extraction solvents, extraction salts, and clean-up reagent, respectively. The optimized method showed good recoveries of PAHs reaching 76%–118% and 85%–121% for SRM1944 and standard solution. The results for cyclone-collected ambient powder aerosol particles extracted by the optimized QuEChERS illustrated that this improved procedure has good PAHs extraction efficiency as the traditional Soxhlet method, while reducing hazardous organic solvents usage, experimental cost (per mg sample) by 97% and sample pretreatment time. Overall, this combination of “powder aerosol particle collection and modified QuEChERS extraction” provides new insight on aerosol sample collection, extraction, and in vitro/in vivo exposure studies.

Development of the QuEChERS Extraction Method for the Determination of Polychlorinated Biphenyls (Aroclor 1254) in Soil Samples by Using GC-MS

Polychlorinated biphenyls (PCBs) have been found in soil, which has typically been the result of industrial pollution in the past two decades. Although they are banned, PCBs can still be found in soils and other environmental media. For this reason, it is critical to develop an analytical method that can reliably identify and monitor their sources. This study describes a gas chromatography with mass spectrometry (GC-MS) technique, which was used to detect PCBs in soil samples by using a fast extraction method. Using the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, PCBs were more effectively extracted from soil. Different related parameters, such as time of shaking and centrifuging, type of solvent, and clean-up adsorbents, were compared and optimized. As the extraction solvent, acetonitrile/water produced the best results, and as the dispersive solid-phase extraction sorbent, diatomaceous earth produced the best results. Procedures allowed recovery values between 95.3% and 103.2%. A limit of detection of 1.9 µg/kg was determined with relative standard deviations (n = 3) of 2.1–4.0% for intra-day assays and 3.6–5.8% for inter-day assays. It was demonstrated that the method was simple, sensitive, efficient, and environmentally friendly when applied to soil samples. To our knowledge, an integrated approach based on QuEChERS for the determination of Aroclor 1254 in soil has not been published before. It is believed that this approach will eliminate the significant challenge of sample extraction in GC-MS processing, which was considered to be a procedural challenge in previous analyses.

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.

Analysis of organophosphorus pesticide residues in selected vegetables purchased from Narsingdi district of Bangladesh using QuEChERS Extraction

Pesticide residues in different crops, including food grains and vegetables are burning issues in Bangladesh. Therefore, the present study was conducted to analyze organophosphorus pesticide residues in three popular vegetables (cauliflower, hyacinth bean and yard long bean) collected from five local markets of Narsingdi district of Bangladesh. The collected vegetable samples were extracted and cleaned up using Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction technique and analyzed by Gas Chromatography (GC) equipped with Flame Thermionic Detector (FTD). A total of 45 vegetable samples were analyzed. Among the 15 analyzed samples of hyacinth bean, three samples (20 % of the total samples) contained pesticide residues above the EU-MRL and the remaining samples did not contain any detectable residues of the selected organophosphorus pesticides. In case of cauliflower, out of 15 analyzed samples, two samples (13% of the total number of samples) contained pesticide residues above the EU-MRL. In case of yard long bean, of the 15 analyzed samples, four samples (27% of the total number of samples) contained pesticide residues above the EU-MRLs. This study reveals the present status of pesticide residue contamination in the selected vegetables. Asian Australas. J. Biosci. Biotechnol. 2022, 7 (3), 114-121

Development and validation of a modified QuEChERS method for extracting polychlorinated biphenyls and organochlorine pesticides from marine mammal blubber

The monitoring of legacy persistent organic pollutants (POPs) in blubber of key sentinel marine mammal species has been conducted using established techniques for decades. Although these methods for polychlorinated biphenyl (PCB) and organochlorine (OC) pesticide determination provide accurate and reproducible results, they possess some drawbacks in terms of cost, time, and a need for large volumes of toxic solvents. QuEChERS (quick, easy, cheap, effective, rugged, and safe) extractions may help address these issues, but have not been applied to marine mammal blubber/adipose. As such, our aim was to develop, validate, and apply a QuEChERS method for the extraction of PCB and OC contaminants in marine mammal blubber. First, we tested multiple solid-phase extraction and clean-up steps to find the approach that provided the cleanest extracts along with consistent and acceptable analyte recovery, accuracy, and precision. QuEChERS extractions followed by two enhanced matrix removal-lipid (EMR-lipid), one primary-secondary amine (PSA), and one silica gel clean-up showed the highest matrix removal and acceptable recoveries of spiked internal (62–97%) and external standards (61–94%). Solvent usage was reduced by ∼393% and extraction time was reduced by ∼25% (from 16 to 12 h). Next, the method was validated using standard reference material (SRM) NIST 1945. Recovery experiments on SRM (n = 5) showed acceptable recovery for 76% and 77% of PCBs and OC pesticides, respectively, and high precision for 73% and 69% of PCBs and OCs, respectively. Finally, the method was used on a set of southeast Greenland killer whales (n = 13), with previously published PCB and OC data. Bland-Altman plots indicated good agreement between QuEChERS and current-use methods for ΣPCBs and some OCs with no significant constant or proportional bias. These results demonstrate that this QuEChERS extraction method represents an effective, lower cost alternative to current-use extractions for PCBs and OCs in blubber, and likely other high-lipid samples.

QuEChERS-based extraction and two-dimensional liquid chromatography-high resolution mass spectrometry for the determination of long chain chlorinated paraffins in sediments

In this study, a method was established for the analysis of long-chain chlorinated paraffins (LCCPs) in sediment based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and two-dimensional liquid chromatography-Orbitrap high resolution mass spectrometry (2DLCOrbitrap HRMS). Compared with other reported methods, this method greatly reduces sample preparation time (2 h) and solvent consumption. The QuEChERS extraction method presented satisfactory recoveries, 90.5–95.2, 84.7–86.6, and 81.4–83.4% of 5, 50, and 200 ng/g LCCPs with 49% Cl spiked into sediments. Meanwhile, no matrix effects were found in the LCCPs analysis after online purification by the 2DLC system. With the current commercial LCCP standards and a mixture of three chlorinated paraffins (CPs) industrial products, a suspect screening strategy was established and accurate identification of LCCPs (including vLCCPs, which carbon chain length greater than 20) under the plight that the reference standards for vLCCPs are currently unavailable. A total of 21 C18–20-LCCP and 22 vLCCP congeners were identified in sediment samples collected from Dongting Lake, China. The total concentrations of LCCPs in six sediment samples ranged from 1.69 to 18.0 ng/g (median 6.66 ng/g) and was dominated by C18 groups (mean, 28.8%), C19 groups (mean, 19.1%) and C21 groups (mean, 16.9%). Taken together, the successful application of this method to analyze sediment samples shows great potential for the analysis of LCCPs in environmental samples in future studies.

Analysis of pesticide residues in vegetables purchased from local markets of Mymensingh district of Bangladesh based on QuEChERS Extraction and Gas Chromatography

The study was conducted to analyze organophosphorus pesticide residues in two common vegetables (cauliflower and eggplant) collected from five local markets of Mymensingh district of Bangladesh. The collected samples were carried to the Pesticide Analytical Laboratory, Entomology Division of Bangladesh Agricultural Research Institute (BARI), Gazipur on the same sampling day. The collected samples were analyzed using Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction technique and Gas Chromatography (GC) coupled with Flame Thermionic Detector (FTD). In total, 60 vegetable samples were analyzed in this study. Out of 30 analyzed samples of cauliflower, 5 samples (17% of the total number of samples) contained residues of dimethoate, chlorpyrifos and quinalphos, where 3 samples contained residues above the maximum residue limits (MRLs). Among the 30 analyzed samples of eggplant, 5 samples (17% of the total number of samples) contained residues of chlorpyrifos, quinalphos, and dimethoate, where only one sample contained residues above MRL. This study reflects the actual scenario of pesticide residues remain in cauliflower and eggplant collected from local markets of Mymensingh district, which will help the consumer to be aware of their health and safety. Thus, continuous monitoring of pesticide residues in vegetables should be strengthened. Asian Australas. J. Food Saf. Secur. 2022, 6 (1), 10-17

Miniaturized QuEChERS extraction method for the detection of multi-residue pesticides in bat muscle tissue

Habitat loss and fragmentation are among the greatest threats to biodiversity and ecosystem stability, with physiological implications on wild fauna. Bats (Microchiroptera) are small mammals with a wide variety of eating habits, and the well-being of these animals is disturbed by exposure to pesticides. This study aimed to develop a miniaturized QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction method for the detection of multi-residue pesticides in bat muscle tissue using gas chromatography coupled with mass spectrometry (GC–MS). A total of 48 pesticides were tested in 250 mg of bat muscle tissue. The developed analytical method was applied to 148 bats collected from two different areas in Minas Gerais State, Southeast Region of Brazil. The method presented good sensitivity and allowed the determination of residues of 48 pesticides in bat muscle using GC–MS. The miniaturized extraction method makes the analysis feasible even when the sample volume is limited. However, no pesticide residues were detected in bats from the two areas investigated.

Novel QuEChERS-ultra-performance liquid chromatography–atmospheric-pressure chemical ionization tandem mass spectrometry method for the simultaneous determination of vitamin D and vitamin K in vitamin-fortified nanoemulsions

Nanoemulsion is a new vehicle for food fortification. In this study, a simple and reliable method for the simultaneous analysis of vitamins D2, D3, K1, and K2 in vitamin-fortified nanoemulsions was developed using QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction and ultra-high performance liquid chromatography–atmospheric-pressure chemical ionization tandem mass spectrometry techniques. Response surface methodology was employed to optimize the extraction parameters. The method was validated for the vitamins in terms of LOD (0.03–0.25 μg/L), LOQ (0.10–0.77 μg/L), intra-day (≤4.50%), inter-day precisions (≤6.43%), and accuracy (98.5%–108.0%). The recoveries of the vitamin-fortified nanoemulsion and yogurt were in the ranges of 104.0%–109.2% and 73.3%–85.2%, respectively. The solvent consumption and analysis time were reduced by 5.6 and 3.3 folds, respectively, rendering it superior to the traditional extraction methods established by the Association of Official Analytical Chemists and the Ministry of Food and Drug Safety.

Analysis of polychlorinated biphenyls in cream and ice cream using modified QuEChERS extraction and GC‐QqQ‐MS/MS method: A risk assessment study

The concentrations of six non–dioxin‐like polychlorinated biphenyls (NDL‐PCBs) were measured using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) by gas chromatography (GC) coupled with triple‐quadrupole (QqQ) tandem mass spectrometry (MS/MS) method in cream and ice cream offered in Tehran (Iran). The results showed the limits of detection, limit of quantification and recovery for the PCB analytes in the ranges 0.04–0.16, 0.132–0.482 ng/g fat, 5.2–9.2 and 95.5–107.2%, respectively. The results showed the mean concentration of total 6NDL‐PCBs in cream (21.634 ± 2.18 ng/g fat) was higher than that in the ice cream (12.317 ± 1.524 ng/g fat) samples. The estimated daily intake (EDI) was lower than the tolerable daily intake (TDI &lt; 10 ng/kg BW/day). Ultimately, the probabilistic model with Monte Carlo simulation (MCS) revealed the incremental lifetime cancer risk levels (95th) of PCB compounds in ice cream (adults = 1.62E−6 and children = 4.37E−6) and cream (adults = 9.65E−7 and children = 7.57E−6) were lower than the level of acceptable risk (10−4).