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

Understanding the bioaccumulation of pharmaceutical active compounds by clams Ruditapes decussatus exposed to a UWWTP discharge

Twenty-four pharmaceutical active compounds (PhACs) were evaluated in the soft tissues of clams Ruditappes decussatus exposed along a 1.5-km dispersal gradient of the treated effluent from an urban wastewater treatment plant discharging in Ria Formosa, and compared with those in the marine waters and discharged effluents. The clams were exposed for 1 month, in June–July 2016, 2017 and 2018. PhACs were quantified by high performance liquid chromatography coupled to tandem mass spectrometry after the quick, easy, cheap, effective, rugged and safe (QuEChERS) method (clams) or solid-phase extraction (water samples). The most representative PhACs in the effluents and receiving waters (regardless of the tidal dilution effect) were diclofenac, carbamazepine and caffeine (on average ≤ 2 μg/L) and only caffeine exhibited significant inter-annual differences, with higher values in 2017. In turn, the most bioaccumulated PhACs in clams were caffeine (0.54–27 ng/g wet weight, significantly higher in 2016) and acetaminophen (0.37–3.7 ng/g wet weight, significant lower in 2016). A multivariate principal component analysis showed (i) PhAC bioaccumulation primarily depended on biotic factors (clams length and weight), (ii) PhAC physicochemical properties Log Kow, pKa and water solubility interplaying with water abiotic variables were more relevant for explaining data variability in water than the physical dilution/tidal mixing, (iii) this process, reflected by the salinity gradient, had a tertiary role in data variation, responsible for spatial discrimination of marine waters. This study provides a better understanding of PhACs bioaccumulation by clams Ruditapes decussatus in real environmental conditions, under the influence of urban treated effluent dispersal in Ria Formosa coastal lagoon, a major producer of bivalves, ultimately disentangling key factors of PhAC bioaccumulation.

Establishment of optimal QuEChERS conditions of various food matrices for rapid measurement of heterocyclic amines in various foods

The optimal conditions for QuEChERS (quick, easy, cheap, effective, rugged and safe) with superior performance were established to rapidly extract 21 heterocyclic amines (HAs) from 9 categories of food matrices including meat and poultry, eggs, soy beans and products, composite foods, fish and seafood, grains, beer, dairy foods, and coffee. The QuEChERS conditions and the developed ultra-high performance liquid chromatography-tandem mass spectrometry analysis conditions were then applied to the determination of HAs in popular food products sold in the Taiwan market. The conditions comply with the food chemical analysis specifications of Taiwan Food and Drug Administration. Coffee products and braised products that require a longer cooking time contained relatively high content of HAs (mainly Harman and Norharman), and their consumption is relatively high resulting in relatively high intake of HAs from these products. The dietary intake of HAs in plant-based protein food products should also be of concern.

Persistence evaluation of fluopyram + tebuconazole residues on mango and pomegranate and their risk assessment.

The persistence of combination formulation of fluopyram 200 + tebuconazole 200-400 SC was evaluated across different agro-climates in India for the management of fungal diseases in two commercially important fruit crops, mango and pomegranate. The residues were extracted using quick easy cheap effective rugged and safe (QuEChERS) method and quantification was done on liquid chromatography-tandem mass spectrometry (LC-MS/MS). The fungicide degradation followed 1st-order kinetics and the half-lives were 2.9-6.4days for mango, and 3.5-7.4days for pomegranate for both the fungicides. On the basis of Organisation for Economic Co-operation and Development (OECD) maximum residue limit (MRL) calculation, 1.0mgkg-1 MRL was obtained for fluopyram while for tebuconazole, it was 0.5mgkg-1 on mango, at the pre-harvest interval (PHI) of 5days. For pomegranate, the respective MRLs were 1.0mgkg-1 and 0.7mgkg-1 at PHI of 7days. The dietary risk assessment study indicated that % acceptable daily intake (% ADI) and % acute reference dose (% ARfD) were much lower than 100; thus, the application of fluopyram and tebuconazole on mango and pomegranate is unlikely to present public health concern.

Simultaneous Quantification of Chloramphenicol, Thiamphenicol, Florfenicol, and Florfenicol Amine in Animal and Aquaculture Products Using Liquid Chromatography-Tandem Mass Spectrometry.

The accumulation of antimicrobial residues in edible animal products and aquaculture products could pose health concerns to unsuspecting consumers. Hence, this study aimed to develop a validated method for simultaneous quantification of chloramphenicol (CAP), thiamphenicol (TAP), florfenicol (FF), and florfenicol amine (FFA) in beef, pork, chicken, shrimp, eel, and flatfish using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Primary-secondary amine (PSA) and MgSO4 were used for sample purification. The analytes were separated on a reversed-phase analytical column. The coefficients of determination for the linear matrix-matched calibration curves were ≥0.9941. Recovery rates ranged between 64.26 and 116.51% for the four analytes with relative standard deviations (RSDs) ≤ 18.05%. The calculated limits of detection (LODs) and limits of quantification (LOQs) were 0.005–3.1 and 0.02–10.4 μg/kg, respectively. The developed method was successfully applied for monitoring samples obtained from local markets in Seoul, Republic of Korea. The target residues were not detected in any tested matrix. The designed method was versatile, sensitive, and proved suitable for quantifying residues in animal-derived products.

High-Throughput Determination of Major Mycotoxins with Human Health Concerns in Urine by LC-Q TOF MS and Its Application to an Exposure Study.

Human biomonitoring constitutes a suitable tool to assess exposure to toxins overcoming the disadvantages of traditional methods. Urine constitutes an accessible biological matrix in biomonitoring studies. Mycotoxins are secondary metabolites produced naturally by filamentous fungi that produce a wide range of adverse health effects. Thus, the determination of urinary mycotoxin levels is a useful tool for assessing the individual exposure to these food contaminants. In this study, a suitable methodology has been developed to evaluate the presence of aflatoxin B2 (AFB2), aflatoxin (AFG2), ochratoxin A (OTA), ochratoxin B (OTB), zearalenone (ZEA), and α-zearalenol (α-ZOL) in urine samples as exposure biomarkers. For this purpose, different extraction procedures, namely, the Solid Phase Extraction (SPE); Dispersive Liquid–Liquid Microextraction (DLLME); and Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) methods were assessed, followed by Liquid Chromatography coupled to Quadrupole Time of Flight Mass Spectrometry with Electrospray Ionization (LC-ESI-QTOF-MS) determination. Then, the proposed methodology was applied to determine mycotoxin concentrations in 56 human urine samples from volunteers and to estimate the potential risk of exposure. The results obtained revealed that 55% of human urine samples analyzed resulted positive for at least one mycotoxin. Among all studied mycotoxins, only AFB2, AFG2, and OTB were detected with incidences of 32, 41, and 9%, respectively, and levels in the range from <LOQ to 69.42 µg/L. Risk assessment revealed a potential health risk, obtaining MoE values < 10,000. However, it should be highlighted that few samples were contaminated, and that more data about mycotoxin excretion rates and their BMDL10 values are needed for a more accurate risk assessment.

Spectroscopic quantifiication of preservatives in different food matrices using QuEChERS extraction and multivariate calibration with comparison against liquid chromatography

The application of QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction procedure has recently received significant attention, particularly for quantifying food additives in complex food matrices. A reliable analytical method based on QuEChERS extraction, UV spectroscopic measurement at 200–320 nm and partial least square regression PLS1 was outlined to determine two classes of preservatives in different processed food products. Examined additives were sodium benzoate SB, potassium sorbate PS, propylparaben PP, and methylparaben MP which showed highly overlapping UV spectra. The method indicated high detection of preservatives down to 1.1–2.4 mg/kg, recoveries between 97 and 102%, and RSD ≤ 7.0%. The efficient extraction of preservatives by QuEChERS from real matrices has improved the snentivity of spectral measurement and the detection of the analytical procedure. Methylparaben, MP, was detected in most samples with levels of 24.5, 74.3 and 393.7 mg/kg in liquid drinks, corn flakes, and soya sauce, respectively. The levels of preservatives were found to be within the regulated limits in all tested items. The outlined QuEChERS along with PLS1 calibration of spectroscopic data is proved to be a suitable alternative for liquid chromatography to monitor different types of preservatives in complex food matrices. The validity of the proposed method was checked against standard liquid chromatography.

Determination of pesticide residues in rooibos (Aspalathus linearis) teas in South Africa

An efficient gas chromatography–mass spectrometry approach was used in this study to quantify 13 pesticide residues in rooibos teas purchased from registered retail outlets in South Africa between November 2019 and April 2020. A QuEChERS (Quick, easy, cheap, effective, rugged, and safe) procedure was used to extract pesticides using 7.5 mg of graphitized carbon black (GCB), 50 mg of primary secondary amine (PSA), and 150 mg of anhydrous MgSO4. In order to compensate for the matrix effect, matrix matched calibration curves ranging from 10 µg/kg–500 µg/kg were applied for accurate quantification. For validation purposes, accuracy tests were conducted using a blank tea sample spiked with pesticide standards at two different concentrations (10 and 100 μg/kg). Most of the analytes were recovered within acceptable recovery ranges (72–106%), with a relative standard deviation of less than 20%. The limits of quantification were low, all falling below 10 μg/kg which meets the maximum residue limits (MRLs). The validated method was used to analyze 100 tea samples, and among the pesticides analyzed, deltamethrin and lambda-cyhalothrin were detected in only one samples at a concentration (92.11 and 66.41 μg/kg, respectively) below the MRLs stipulated by the European Union. The level of pesticides that are commonly used in tea should be checked often.

Carbofuran residues in soil and consumption risks among farmers growing vegetables in Ubon Ratchathani Province, Thailand

&lt;abstract&gt; &lt;p&gt;Farmers in Khi Lek Subdistrict, Muang District, Ubon Ratchathani Province, Thailand have been known to persistently use pesticides, especially carbofuran, in their agricultural fields. This indeed poses a risk to farmers' health and ecosystem. However, there has been no report pointing out this problem. The purpose of this study was to determine carbofuran residues in soil in four villages in Khi Lek Subdistrict, Muang District, Ubon Ratchathani Province, Thailand, where pesticides were widely used for vegetables. The quick, easy, cheap, effective, rugged and safe (QuEChERS) method was used to extract the samples, which were then analyzed utilizing high-performance liquid chromatography with a mass spectrometry detector. The health risks of carbofuran exposure through soil ingestion among 485 farmers were investigated by using the hazard quotient (HQ). The concentration of carbofuran in 10 soil samples was less than 0.01 mg/kg. The overall average of the farmers' daily dose of carbofuran in Villages 5, 8, 9 and 10 ranged from 3.9×10&lt;sup&gt;-9&lt;/sup&gt; mg/kg-day to 5×10&lt;sup&gt;-9&lt;/sup&gt; mg/kg-day, and the hazard quotient (HQ) indicated an acceptable level for health risks. However, this study found that 98.97% of the farmers ate food and 97.53% drank water while farming. As a result of this, they may still be exposed to pesticides. Since the factors contributing to human health risks include the length of exposure, frequency of exposure, and farmer body weight, this study suggests that the government should be concerned because the current pattern of pesticide use still poses an immediate health risk to the farmers. While The farmers should be trained in safe pesticide usage while safe pesticide practice should also be promoted.&lt;/p&gt; &lt;/abstract&gt;

Analysis of pesticide residues in fruits and vegetables using gas chromatography-mass spectrometry: a case from West Omo and Bench-Sheko Zone, Southwest Ethiopia

ABSTRACT Uncontrolled use of pesticides could result in contamination of air, water, food, and ecosystems. This study aimed to determine pesticide residues in fruits and vegetables collected from selected farmlands of southwest Ethiopia from the end of April 2019 until mid of May 2019. The samples were extracted using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and clean-up method. Quantitative analysis of four organophosphorus pesticides (OPPs) and seven organochlorine pesticides (OCPs) were conducted using gas chromatography-mass spectrometry. All the fruit and vegetable samples obtained from all sampling sites were contaminated with one or more pesticide residues. Chloroflurenol-methyl was the most predominantly detected OPPs residue in all crop samples obtained from different sampling sites, with a maximum concentration of 0.402 mg kg−1 in potato samples obtained from the Gurafarda site and a minimum value of 0.049 mg kg−1 in onion samples obtained from the South Bench site. Dibutyl chlorendate was the predominant OCPs in all samples, with the minimum value of 0.498 mg kg−1, which was detected in tomato samples collected from the Jamo site, and the maximum concentration of 1.003 mg kg−1 detected in pineapple samples obtained from the North Bench site. Dimethoate concentrations in tomato samples (0.045–0.084 mg kg−1) were above the maximum residue limits (MRLs) established by the European Union (EU) guidelines (0.01 mg kg−1) but were below the MRLs established by Codex Alimentarius Commission (CAC) guidelines (0.5 mg kg−1). Relatively high residue concentrations of dibutyl chlorendate and chloroflurenol-methyl were detected in all the samples obtained from all sampling sites. There is widespread use of pesticides for agriculture by the producers in the study area and there is a need for the regular monitoring of pesticide residues.

Multiresidue pesticide analysis in tomato using GC-MS/MS using modified QuEChERS method with titanium-coated graphite with CNT-ABS nanocomposite as dispersive solid-phase extraction materials

Abstract The presence of pesticide residues in food and vegetables is a growing concern for consumers. To monitor these residues reliably, a selective and sensitive multiresidue system has been developed and validated in tomato by gas chromatography–tandem mass spectrometry (GC-MS/MS). Titanium-coated graphite with carbon nanotube (CNT) in acrylonitrile–butadiene–styrene (ABS) used as reversed-dispersive solid-phase (extraction materials with modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method. Titanium-coated graphite with CNT-ABS is synthesized, characterized by X-ray diffraction and scanning electron microscopy. The clean-up performance of titanium-coated graphite with CNT-ABS was demonstrated to be better to primary secondary amine and graphitized carbon black cartridges. The processing of two multiple reaction monitoring transformations for each analyte is done using GC-MS/MS in electron impact mode. Satisfactory purification and recovery effects (74%–100%) of 35 pesticides were achieved in tomato matrices when using 5 mg of titanium-coated graphite ABS-CNT nanocomposite. It was observed that quinolphos and deltamethrin are present above the maximum residue limit. The technique proved to be reliable and sensitive in tomato samples for the routine testing of 35 pesticides.

Determination of Ethyl Carbamate in Commercial Sweetened Sugar Cane Spirit by ESI-MS/MS Using Modified QuEChERS and 18-Crown-6/Trifluoroacetic Acid Spiking Additives

A fast, sensitive, and selective direct injection electrospray tandem mass spectrometry (DI‑ESI‑MS/MS) method that is able to quantify ethyl carbamate in commercial sweetened sugar cane spirit is described. The preparation method uses a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) with potassium carbonate added to sweetened sugar cane spirit to separate the aqueous phase from the ethanol phase. The aqueous phase contains sucrose that suppresses electrospray ionization. Ethyl carbamate supernatant from the ethanol phase is transferred and enriched with 18-crown-6/trifluoroacetic acid additives. The additives sequester metal cations reducing the ionization of sodium and potassium, favoring the detection of ethyl carbamate as sole protonated cations. The method was successfully applied for the quantification of eleven real samples and certified sugar cane spirit demonstrating its applicability for quality control and regulatory analysis. The method showed reliable analytical parameters compared to conventional gas chromatography mass spectrometry (GC-MS) method commonly used for ethyl carbamate analysis. DI-ESI-MS/MS method requires just a fast step sample clean up and presents consistent values for the limit of detection (LOD 48.0 μg L−1) and limit of quantification (LOQ 160.0 μg L−1). Furthermore, the recoveries obtained were close to 100%, with relative standard deviations below 10% of sample certificates.

QuEChERS: A Microextraction Technique for Pesticide Residue Analysis in Food Commodities

Pesticide residues in food commodities has become a major cause of concern all-over the world. Analysis of pesticide residues from vegetable and fruit samples to ensure the safety of consumers is becoming increasingly important. The most important step of any analytical methodologies is sample preparation step because it determines the efficiency of any method. A good microextraction technique reduces the sample and solvent volume, maintaining the high performance, low-cost and improvement of the sampling steps such as extraction, concentration, isolation of analytes, and clean-up. Lots of analytical methods are developed to analysed multiple pesticide residues analysis and contaminantcontroloffoodproducts,feedstuff,andenvironmentalsamples. While in starting, the QuEChERS was introduced for pesticides residues analysis in fruits and vegetables, but over a period of time, it is gaining significant popularity in the analysis of wide spectrum of analytes. QuEChERS method provided high quality results in a fast, easy, an inexpensive approach. The method is very effective and gives recovery for most of the pesticides in the range of 80 -120 percent and the ruggedness of the method is evident from reproducibility, repeatability being within acceptable range in all the tested samples. Liquid-liquid partitioning using acetonitrile and purifying the extract using dispersive solid-phase extraction (d-SPE) is the key point of this method. The objective of this paper is to give an overview of the benefit of QuEChERS and the recent developments in the QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach for sample preparation.

Pesticide residues in green-house cucumber, cantaloupe, and melon samples from Iran: A risk assessment by Monte Carlo Simulation

This research aims to analyze 56 pesticide residues in 100 green-house cucumber and 150 cantaloupe and melon samples collected from markets in Iran by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction method based on analysis with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). In addition, non-carcinogenic and carcinogenic probabilistic health risk assessments were evaluated by Hazard Quotient (HQ), Hazard Index (HI), and Carcinogenic Risk (CR) based on the Monte Carlo Simulation (MCS) method. According to Iranian regulation, 18% of cucumber and 22% of cantaloupe and melon samples were contaminated by at least one pesticide. Arrange pesticides based on HQ ranking was diazinon > thiacloprid > imidacloprid tebuconazole for cucumbers and chlorpyrifos > thiacloprid > imidacloprid > metalaxyl for cantaloupes and melons. In addition, HI for adults was 0.067 in cucumber and 0.24 in cantaloupe and melon; and for children, 0.30 in cucumber and 0.60 in cantaloupe and melon. Arrange pesticides based on CR ranking was thiacloprid > imidacloprid > metalaxyl > chlorpyrifos > tebuconazole > diazinon. However, CR was more than 1.0E-6 value due to thiacloprid, so consumers were at considerable carcinogenic risk in these commodities.

Validation of Pesticides Multi-Residual Testing Method on Nutmeg by Using UPLC-MS/MS

The use of pesticides in nutmeg still leaves an accumulation of pesticide residues that can endanger human health and damage the ecological balance. In addition, nutmeg with high pesticide residue content will be rejected by nutmeg export destination countries. This research was conducted to validate the method of testing pesticide residues of carbaryl, carbofuran, acetate, and dimethoate on nutmeg. This pesticide residue test uses the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) optimization method and is analyzed using UPLC-MS/MS (Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry). This method meets the validation requirements according to SANTE/12682/2019. The limit of quantification (LOQ) of the analyte is below the Maximum Residue Limit (MRL) set by the European Union through Regulation (EC) No. 396/2005.

High-Resolution Mass Spectrometry Screening of Emerging Organophosphate Esters (OPEs) in Wild Fish: Occurrence, Species-Specific Difference, and Tissue-Specific Distribution.

There is a dearth of information regarding the pollution status of emerging organophosphate esters (OPEs) in wild fish. Here, we optimized and validated a quick, easy, cheap, effective, rugged, and safe (QuEChERS) pretreatment method, which was further applied for target, suspect, and nontarget screening of OPEs in n = 48 samples of wild fishes from Taihu Lake (eastern China). This integrated technique allows us to fully identify 20 OPEs, and 9 out of them are emerging OPEs detected in wild fish for the first time. Importantly, some of the emerging OPEs, i.e., tris(2,4-di-tert-butylphenyl) phosphate (TDtBPP), 4-tert-butylphenyl diphenyl phosphate (BPDP), and 2-isopropylphenyl diphenyl phosphate (IPDP), exhibited greater or at least comparable contamination levels as compared to traditional ones. There were no statistically significant interspecies (n = 6) differences regarding OPE concentrations. However, we observed significant differences on OPE concentrations among different tissues of silver carp (Hypophthalmichthys molitrix), for which the intestine has the highest OPE mean concentration (46.5 ng/g wet weight (ww)), followed by the liver (20.1 ng/g ww) ≈ brain (20.0 ng/g ww) > gill (14.8 ng/g ww) > muscle (11.4 ng/g ww). An interesting exception is IPDP, which presents an unexpectedly high concentration in the brain (0.510 ng/g ww). Collectively, this study expands our understanding of OPE contamination in wild fish and clearly shows that emerging TDtBPP, IPDP, and BPDP could play an equally important role as traditional OPEs in contribution of OPE pollution in wild fish samples.

QuEChERS sample preparation integrated to dispersive liquid-liquid microextraction based on solidified floating organic droplet for spectrometric determination of sudan dyes: A synergistic approach

In this project, a synergistic approach has been proposed where a quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation technique was developed for the extraction of sudan III and sudan IV dyes in different spices prior to its dispersive liquid-liquid microextraction based on solidified floating organic droplet (DLLME-SFO). Initially, the sample was extracted by QuEChERS method and then preconcentrated through DLLME-SFO followed by spectrophotometric detection. All the experimental parameters i.e., volume of extraction solvent, pH, acetonitrile to water ratio, temperature, centrifugation rate and time, and sample volume were optimized. Limit of detection (LOD) calculated for sudan III and sudan IV were 0.42 and 0.35 mg/L, respectively. Excellent recoveries were obtained in the range of 98.29–99.88%. After validation through standard addition methodology, the developed QuEChERS@DLLME-SFO method was successfully applied to determine sudan (III-IV) dyes in real spices samples. Integration of QuEChERS and DLLME-SFO was found to be a suitable substitute to eliminate the usage of costly primary secondary amines and other sorbents. The synergistic approach of QuEChERS and DLLME-SFO with the aid of UV/visible spectrophotometry makes it prompt, cost effective technique with excellent analytical figures of merit.

Analysis of human serum and urine for tentative identification of potentially carcinogenic pesticide-associated N-nitroso compounds using high-resolution mass spectrometry

Human serum and urine samples were analyzed for a suite of nitrosatable pesticides and potentially carcinogenic pesticide-associated N–nitroso (PANN) compounds. Formation of PANN compounds may occur in vivo after consumption of food or water containing trace amounts of nitrosatable pesticide residues and nitrate. Using a modified version of the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method, nine nitrosatable pesticides and byproducts were extracted from serum and urine from 64 individuals from two different sample populations in Atlantic Canada: (i) Prince Edward Island, a region where nitrate and trace amounts of nitrosatable pesticides have been detected in groundwater; and (ii) Halifax, Nova Scotia, a non-agricultural urban area. Samples were then analyzed using ultra-high pressure liquid chromatography (UHPLC) coupled with high-resolution accurate mass (HRAM) single-stage orbitrap mass spectrometry (MS), which allows for semi-targeted analysis and tentative identification of a virtually limitless number of exposure biomarkers. Two nitrosatable target analytes, ethylenethiourea (ETU) and 3,5,6-trichloro-2-pyridinol (TCPy) were found in serum, while atrazine (ATR) and ETU were detected in urine. Five and six PANN compounds were tentatively identified in serum and urine, respectively. The two PANN compounds that were most frequently tentatively identified in serum were N-nitroso dimethoate (N-DIM) and N-nitroso omethoate (N-OME) with detection frequencies of 78% and 95%, respectively. This is the first biomonitoring study of its kind to investigate PANN compounds in human serum and urine.

A Comparison between a Two-Dimensional Liquid Chromatography System and a Traditional QuEChERS-LC Method with Regard to Matrix Removal and Matrix Effects in Pesticide Analysis Using Time-of-Flight Mass Spectrometry.

In this study, a fully automated two-dimensional liquid chromatography (2D-LC) system was used for the investigation of the clean-up effect and was compared with a traditional Quick Easy Cheap Effective Rugged and Safe (QuEChERS) liquid chromatography (LC) method. The focus of those investigations was on negative electrospray ionization (ESI) mode. For that purpose, matrix fingerprinting profiles were created. The results allowed a comparison of both methods regarding the estimation of the number and the polarity of detected compounds. Moreover, the results of the present study were compared with the results generated in positive ESI mode (presented in a previous study). Furthermore, the two methods were compared with regard to matrix effects (ME) of 321 analytes in positive ESI mode and 96 analytes in negative ESI mode. In general, fewer compounds could be detected when 2D-LC and/or the negative ESI mode was used. Especially, very polar compounds with m/z values >1000 could be separated and could not be detected anymore when 2D-LC was applied. Furthermore, the best results were obtained for most analytes when 2D-LC was used, although the extent of ME seemed to be higher with 2D-LC.

Rapid determination of multi-antibiotic residues in honey based on modified QuEChERS method coupled with UPLC–MS/MS

Antibiotic residues in honey cause public health problems. To analyze multi-antibiotic residues in honey, a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction method coupled with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed for simultaneous quantification of 70 antibiotic residues in honey. Matrix-matched calibrations indicated the correlation coefficients were higher than 0.998. The recovery was in a range of 70.5%-119.8% with intra-day relative standard deviation (RSD) of ≤ 10.0% and inter-day RSD of ≤ 13.9%. The limits of detection ranged between 0.050 μg/kg and 1.02 μg/kg. Limits of quantification was 0.17 μg/kg to 3.40 μg/kg. The matrix effects were negligible in 71.4% of compounds and moderately in 24.3% of compounds. Methacycline, oxytetracycline, tetracycline and its metabolite 4-tetracycline residues were detected in the tested samples. Validation parameters were acceptable and were in line with the Codex guidelines. This method was effective for detecting multi-antibiotic residues in honey.

Monitoring of pesticide residues in vegetables collected from retail markets of Dhaka district of Bangladesh using QuEChERS Extraction and Gas Chromatography

The present study was aimed to detect and quantify major organophosphorus pesticide residues in cauliflower and cucumber collected from different retail markets of Dhaka city, Bangladesh. In this study, a total of 50 vegetable samples (30 samples of cauliflower and 20 samples of cucumber) were analyzed using Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) extraction technique and Gas Chromatography coupled with Flame Thermionic Detector (GC-FTD). Among the 30 analyzed samples of cauliflower, 5 samples (16.7% of the total number of samples) contained residues of chlorpyrifos, quinalphos, acephate and dimethoate, where 4 samples contained multiple pesticide residues. All the contaminated samples of cauliflower contained residues above the EU-MRL. On the other hand, among the 20 analyzed samples of cucumber, only 2 samples (10% of the total number of samples) contained residues of quinalphos and chlorpyrifos at a level being below the EU-MRL. This study reflects the overall scenario of pesticide residues remain in cauliflower and cucumber purchased from different local markets of Dhaka city, which will help the consumer to be aware of their health and safety. The findings derived from this study reveals the public health concern due to the potential of pesticide toxicity in vegetables for the consumers. Therefore, continuous monitoring on the use of pesticides in vegetables should be strengthened. Asian Australas. J. Food Saf. Secur. 2021, 5 (2), 63-70