Two-dimensional metal-organic framework nanosheets coated solid-phase microextraction Arrow coupled with UPLC-Q-ToF-MS for the determination of three veterinary residues in milk and pork.

This study presents a method utilizing solid-phase microextraction Arrow (SPME Arrow) combined with ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) for the selective detection of three veterinary drugs-thiabendazole, sulfamethazine, and clenbuterol-in milk and pork. Two-dimensional metal-organic framework nanosheets (2D-MOFs) were employed as coating materials for the SPME Arrow. Three types of 2D-MOFs (Ni, Mn, and Co based) were synthesized and characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, and a physical adsorption analyzer. The 2D-MOF coatings were fabricated using the electrospinning technique, with polyacrylonitrile (PAN) serving as the binder. Comparative analysis of the three 2D-MOF coatings revealed that 2D-Ni-MOF was the optimal coating material for the SPME Arrow. Optimization of the coating preparation conditions and SPME procedures included determining the optimal mass ratio of 2D-Ni-MOF to PAN, electrospinning time, and extraction and desorption parameters. Equilibrium extraction was achieved within 60 min, and desorption was completed within 30 min. Subsequently, the 2D-Ni-MOF-SPME Arrow-UPLC-Q-TOF-MS method was established and validated under optimal conditions, demonstrating high precision with inter-day precision ranging from 3.8 % to 9.5 % and intra-day precision ranging from 5.1 % to 11.5 %. The reusability study indicated that the extraction performance of the new SPME Arrow remained consistent after 90 adsorption-desorption cycles. The method exhibited linearity in milk and pork over the ranges of 0.002-5 µg L-1 and 0.01-5 µg L-1, respectively. The detection limits in milk and pork were 0.001-0.004 µg L-1 and 0.003-0.007 µg L-1, respectively. This method demonstrated excellent applicability for determining residues of the three veterinary drugs in milk and pork.

Veterinary Drug Residues in Food Products of Animal Origin and Their Public Health Consequences: A Review.

Veterinary medications used for disease treatment and prevention may remain in animal-origin foods, such as milk, eggs, honey and meat, which could pose a risk to the public's health. These drugs come from different groups of drugs, mostly with antibiotic, anti-parasitic or anti-inflammatory actions, in a range of food matrices including milk, meat or egg. This review is intended to provide the reader with a general insight about the current status of veterinary drug residues in food products of animal origin, detection methods and their public health consequences. The discovery of antimicrobials has led to the development of antibiotics for treating and preventing cattle illnesses and encouraging growth. However, the rise of drug resistance has led to increased antibiotic consumption and resistance among microbes in the animal habitat. This resistance can be passed to humans directly or indirectly through food consumption and direct or indirect interaction. Improper and illegal use, inadequate withdrawal periods and environmental contamination from veterinary drugs are reported to be the major causes for the formation of residue in food products of animal origin. The use of veterinary products above or below the advised level may also result in short- or long-term public health issues, such as the creation of resistant strains of micro-organisms, toxicity, allergy, mutagenesis, teratogenicity and carcinogenetic effects. To ensure consumer safety, veterinary drug residues in food must be under control.

High throughput detection of veterinary drug residues in chicken and eggs.

Co-extraction of multiple types of target substances is the key to achieve high throughput detection. In this work, PDA@MOF-808/PAN NFsM was prepared by co-modified polyacrylonitrile nanofiber membrane (PAN NFsM) with polydopamine (PDA) and metal-organic framework-808 (MOF-808), and its potential as a solid-phase extraction (SPE) adsorbent was investigated by using the most typical nine veterinary drug residues in eggs and chicken as model target substances. The results show that PDA@MOF-808/PAN NFsM could effectively co-extract all the target substances (adsorption efficiency ranged from 81.46 % to 96.78 %), and had good capability of sample matrix purification (matrix effect was lower than -15.26 %), so a new SPE method has been established. Combined with UPLC-MS/MS, the detection limits were 0.3 to 3.1 µg/kg, the recoveries were between 71.02 % and 106.48 %, and the relative standard deviations were lower than 12.03 %, indicating that the method has considerable good sensitivity, accuracy and precision.

Core-satellite-structured magnetic nanozyme enables the ultrasensitive colorimetric detection of multiple drug residues on lateral flow immunoassay.

BACKGROUND: Excessive use of veterinary drugs causes severely environmental pollution and agricultural pollution, and poses great threat to human health. A simple method for the rapid, highly sensitive, and on-site monitoring of veterinary drug residues in complex samples remains lacking. RESULTS: In this study, we propose a catalytically enhanced colorimetric lateral flow immunoassay (LFA) based on a novel core-satellite-structured magnetic nanozyme (Fe-Au@Pt) that can simultaneously and quantitatively detect three common veterinary drugs, namely, gentamicin (GM), streptomycin (STR), and clenbuterol (CLE), within a short testing time (<30 min). The Fe-Au@Pt nanozyme was simply prepared through the self-assembly of numerous Au@Pt nanoparticles on a large Fe3O4 core via electrostatic adhesion, which exhibited the advantages of high peroxidase-like activity, strong magnetic responsiveness, and multiple catalytic sites. Under the dual-signal amplification effect of magnetic enrichment and catalytic enhancement, the proposed nanozyme-LFA allowed the multiplex detection of STR, CLE, and GM with detection limits of 10.1, 6.3, and 1.1 pg/mL, respectively. SIGNIFICANCE: The developed Fe-Au@Pt-LFA achieves direct, simultaneous, and accurate detection of three target drugs in food samples (honey, milk, and pork). The proposed assay shows great potential for application in the real-time monitoring of small-molecule pollutants in complex environment.

[Determination of five veterinary drug residues in milk by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry based on modified chitosan membrane purification].

Milk is an important consumer product with high nutritional value. The presence of veterinary drug residues in milk owing to the indiscriminate use of veterinary drugs may affect consumer health. In the mass spectrometric analysis of trace compounds, chromatographic co-eluting components easily interfere with the mass spectral signals obtained, affecting the accuracy of qualitative and quantitative analyses. Matrix purification is a promising method to reduce the matrix effect. Chitosan is a natural biopolymer with numerous active functional groups such as amino, acetyl, and hydroxyl groups; these groups can adsorb lipids through hydrophobic and electrostatic interactions. Chitosan also has the advantages of low production cost, stable chemical properties, and convenient modification. Novel chitosan-based materials are promising candidates for lipid purification. In this study, a chitosan membrane was modified with trimethoxyoctadecylsilane (C18-CSM). C18-CSM was prepared through one-step hydrolysis and used as a dispersive solid phase extraction (DSPE) adsorbent to purify the matrix during milk pretreatment. We combined C18-CSM with ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry (UHPLC-Q/Exactive Orbitrap MS) to develop an effective method for the extraction and determination of ofloxacin, enrofloxacin, ciprofloxacin, diazepam, and metronidazole in milk. C18-CSM was characterized using scanning electron microscopy, Fourier transform infrared spectroscopy, and water contact angle testing. The results indicated that the material has a rough surface and uniformly dense cross-section. The water contact angle of C18-CSM was 104°, indicating its good hydrophobicity. The pretreatment conditions (extraction solvent, dosage of NaCl, extraction frequency, and dosage of C18-CSM) that influenced the recoveries of the five veterinary drugs were investigated in detail. The optimal conditions were established as follows: 5% formic acid in acetonitrile, 1 g NaCl, extraction 1 time, 20 mg C18-CSM. Separation was performed on a Hypersil GOLD VANQUISH column (100 mm×2.1 mm, 1.9 µm). The mobile phase consisted of 0.1% formic acid aqueous solution and 0.1% formic acid in acetonitrile, and was flowed at a rate of 0.3 mL/min. The sample injection volume was 1 µL, and the column temperature was maintained at 25 ℃. Mass spectrometric analysis was performed in positive electrospray ionization mode. To verify the necessity of the purification material, the matrix effect was investigated using the matrix-matched standard curve method. The use of C18-CSM reduced the matrix effects of the five necessity drugs from the range of -22%-8.8% to the range of -13%-3.6%, indicating that C18-CSM is a highly efficient DSPE material. Under optimal conditions, the developed method showed good linearities within the range of 0.5-100 µg/L, with correlation coefficients (r2)≥0.9970. The limits of detection(LODs) and quantification (LOQs) were 0.2 µg/L and 0.5 µg/L, respectively. To assess the accuracy and precision of the method, we prepared milk samples with three spiked levels (low, medium, and high). The recoveries of the five veterinary drugs were ranged from 79.5% to 115%, and the intra-day and inter-day relative standard deviations were 7.0%-13% (n=6) and 1.3%-11% (n=3), respectively. This study provides a simple, accurate, and reliable method for the rapid and simultaneous determination of the five veterinary drug residues in milk.

Eco-conscious potentiometric sensing: a multiwalled carbon nanotube-based platform for tulathromycin monitoring in livestock products.

Tulathromycin (TUL) is a widely used veterinary antibiotic for treating bovine and porcine respiratory infections. Consuming animal-derived food contaminated with this medication may jeopardize human health. This work adopted the first portable potentiometric platform for direct TUL sensing in pharmaceutical and food products. The sensor employed a plasticized PVC membrane on a glassy carbon electrode doped with calix[6]arene and multi-walled carbon nanotubes (MWCNT) in a single solid contact layer for selective binding and signal stability. Characterization via scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) confirmed the material's integrity. The MWCNT-based sensor produced a stable Nernstian response (1.0 × 10-7 to 1.0 × 10-3 M) and a limit of detection (LOD) of 9.76 × 10-8 M with instantaneous response (8 ± 2 s). IUPAC validation revealed high selectivity for TUL against interfering ions, minimal drift (0.6 mV/h), and functionality over a broad pH range (2.0-7.0), allowing direct application to dosage form, spiked milk, and liver samples. Eco-Scale, AGREE, and Whiteness assessment proved the method's ecological sustainability, economic viability, and practical feasibility, surpassing traditional approaches.

Study on Rapid, Quantitative, and Simultaneous Detection of Drug Residues and Immunoassay in Chickens.

Different levels of residual drugs can be monitored within a relatively safe range without causing harm to human health if the appropriate dosing methodology is considered and the drug withdrawal period is controlled during poultry and livestock raising. Antimicrobials are factors that can suppress the growth of microorganisms, and antibiotic residues in livestock farming have been considered as a potential cause of antimicrobial resistance in animals and humans. Antimicrobial drug resistance is associated with the capability of a microorganism to survive the inhibitory effects of the antimicrobial components. Antibiotic residue presence in chicken is a human health concern due to its negative effects on consumer health. Neglected aspects related to the application of veterinary drugs may threaten the safety of both humans and animals, as well as their environment. The detection of chemical contaminants is essential to ensure food quality. The most important antibiotic families used in veterinary medicines are ß-lactams (penicillins and cephalosporins), tetracyclines, chloramphenicols, macrolides, spectinomycin, lincosamide, sulphonamides, nitrofuranes, nitroimidazoles, trimethoprim, polymyxins, quinolones, and macrocyclics (glycopeptides, ansamycins, and aminoglycosides). Antibiotic residue presence is the main contributor to the development of antibiotic resistance, which is considered a chief concern for both human and animal health worldwide. The incorrect application and misuse of antibiotics carry the risk of the presence of residues in the edible tissues of the chicken, which can cause allergies and toxicity in hypersensitive consumers. The enforcement of the regulation of food safety depends on efficacious monitoring of antimicrobial residues in the foodstuff. In this review, we have explored the rapid detection of drug residues in broilers.

Status of antibiotic residues in milk and dairy products of Iran: a systematic review and meta-analysis.

Background: Today, antibiotics are widely used for treatment and feed additives to enhance livestock growth. Antibiotic residues may be found in food of animal origin for various reasons, including ignoring the withdrawal period after treatment, overuse for animals, and contamination of feed with treated animals in animal products. Among animal products, dairy products have a special place in the human diet, and antibiotic residues in them have caused a great deal of concern among consumers. Objective: This systematic review and meta-analysis aimed to evaluate and compare studies conducted in Iran on antibiotic residues in dairy products during 2000-2022. Methods: In this review, 52 eligible studies were collected by searching the Scientific Information Database (SID), Magiran, Google Scholar, Science-Direct, Scopus, and PubMed using the English or Persian keywords such as an antibiotic or antimicrobial residue, Beta-lactam residue, Tetracycline residue, Sulfonamide residue, Chloramphenicol residue, Aminoglycosides residue, Macrolide residue, Quinolones residue, Milk, Raw milk, Pasteurized milk, UHT milk, Powder milk, Cheese, Yogurt, Butter, Cream, Doogh, Kashk, Ice cream, and Iran. Results: According to the reviewed studies, the total prevalence of antibiotic residues in dairy products was 29% (95% CI: 15-43%). Among the seven evaluated antibiotic groups, most studies have been conducted on tetracycline, beta-lactam, and sulfonamide groups, with 16, 10, and 7 respectively, and the highest level of contamination with 663 ± 1540 µg/l is related to tetracycline. Most studies on antibiotic dairy product residues in Iran with 12, 11, and 8 studies are associated with East Azarbaijan province, then Tehran and Khorasan Razavi respectively, and no study has been conducted in 11 provinces of the country. According to the studies, Gilan, Qazvin and Razavi Khorasan provinces had the highest amount of antibiotic residue in milk with an average value of 56.415 ± 33.354, 45.955 ± 4.179 and 45.928 ± 33.027, respectively. Most of the methods used in the studies to measure antibiotic residues in milk were the Copan test kit and the HPLC method, which were used in 19 and 14 studies, respectively. Conclusions: Studies have shown that the prevalence of antibiotic residue in dairy products in Iran is high, so applying an effective strategy and developing the necessary standards in this field to control milk quality is a public health necessity. The findings of this study show that further evaluation of fermented dairy products, especially non-fermented ones such as butter and cream, is needed to prevent adverse health reactions.

Veterinary Drug Residues in the Food Chain as an Emerging Public Health Threat: Sources, Analytical Methods, Health Impacts, and Preventive Measures.

Veterinary medications are necessary for both contemporary animal husbandry and food production, but their residues can linger in foods obtained from animals and pose a dangerous human risk. In this review, we aim to highlight the sources, occurrence, human exposure pathways, and human health effects of drug residues in food-animal products. Following the usage of veterinary medications, pharmacologically active compounds known as drug residues can be found in food, the environment, or animals. They can cause major health concerns to people, including antibiotic resistance development, the development of cancer, teratogenic effects, hypersensitivity, and disruption of normal intestinal flora. Drug residues in animal products can originate from variety of sources, including water or food contamination, extra-label drug use, and ignoring drug withdrawal periods. This review also examines how humans can be exposed to drug residues through drinking water, food, air, and dust, and discusses various analytical techniques for identifying these residues in food. Furthermore, we suggest some potential solutions to prevent or reduce drug residues in animal products and human exposure pathways, such as implementing withdrawal periods, monitoring programs, education campaigns, and new technologies that are crucial for safeguarding public health. This review underscores the urgency of addressing veterinary drug residues as a significant and emerging public health threat, calling for collaborative efforts from researchers, policymakers, and industry stakeholders to develop sustainable solutions that ensure the safety of the global food supply chain.

Simultaneous detection of residues of 34 beta-lactam antibiotics in livestock and fish samples through liquid chromatography-tandem mass spectrometry.

ß-Lactam is one of the widely used veterinary drugs, but simultaneous analytical methods for ß-lactam on various animal foods have not been established. In this study, we aimed to detect 34 ß-lactam antibiotics simultaneously in livestock samples (beef, pork, chicken, egg, and milk) by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted using phosphate buffer/acetonitrile or water/acetonitrile and then cleaned with 150 mg of C18 and 900 mg of MgSO4. The method showed acceptable recovery and repeatability of 66.1-119% and 1.5-26%, respectively. The method was employed to monitor 127 real samples from the domestic market to confirm its applicability, and no ß-lactam residues were detected. It was also applied to other matrices (eel, flat fish, and shrimp) and showed acceptable recovery (62.1-120%) and repeatability (1.0-28%). The method is expected to improve the efficiency of monitoring veterinary drug residues in domestic livestock products and fishery foods.

Antibiotic residues and microbial contamination in pasteurized whole milk intended for human consumption.

Background and Aim: Milk contamination for human consumption is one of the biggest concerns worldwide. To prevent milk contamination, it is important to implement sustainable production practices that ensure animal health and guarantee veterinary drugs have been used properly. This study aimed to detect antibiotic residues and microbial contamination in commercially available pasteurized whole milk intended for human consumption. Materials and Methods: We conducted a cross-sectional study on all brands of pasteurized milk (n = 17) for human consumption in Medellín, Colombia, from February 30 to April 30, 2022. Six milk samples of each brand were collected every 15 days, resulting in 102 samples. IDEXX SNAPduo™ ST Plus test (IDEXX Laboratories Inc, Maine, USA) was used to detect cephalosporins residues to detect beta-lactam and tetracyclines. We detected mesophilic aerobic bacteria and coliforms using Chromocult Coliform Agar® (Merck KGaA, Darmstadt, Germany) and Plate-Count Agar® (Merck KGaA), respectively. Results: Beta-lactam residues were found in 24.4% of the brands. No tetracyclines or cephalosporins were detected. Mesophilic aerobic bacteria and coliform contamination were detected in 42.6% and 12.8% of the brands, respectively. No fecal coliform contamination was detected. Conclusion: This study demonstrated the presence of antibiotic residues and microbial contamination in commercially available pasteurized whole milk intended for human consumption in the study area, highlighting its potential public health implications.

In-tube solid phase extraction with graphitic-based polyurethane sponge as a superhydrophobic sorbent and determination of drug residues in foodstuffs using high-performance liquid chromatography.

Veterinary drugs used in animal husbandry raise public health concerns due to their residues in the bodies of animals. This study employs a simple and quick sample preparation technique, in-tube solid phase extraction, to extract drug residues from foodstuffs, including eggs, honey, and water. This technique utilizes the synergy of graphitic-based materials and polyurethane sponges (PU) combined through dip coating method to make reusable sorbents for extracting drugs, including amoxicillin, paracetamol, ciprofloxacin, and cefixime. These prepared sorbents were characterized using FTIR, SEM, and XRD. HPLC analysis assessed the extraction efficiency, considering various parameters such as analyte concentration, sample solution pH, extraction time, type of eluting solvent, and graphitic-based polyurethane sponge reusability and stability. The proposed method exhibited a linear response for all three sorbents in the range of 0.03-1000 µg mL-1, with LOD 0.03-1.60 µg mL-1 and LOQ 0.18-4.84 µg mL-1. The % RSD ranged from 1.3 to 9.3 %, with recoveries of up to 98.42 %.

Comparison of filter membranes in the analysis of 183 veterinary and other drugs by liquid chromatography-tandem mass spectrometry.

Although filtration is one of the most common steps in sample preparation for chemical analysis, filter membrane materials can leach contaminants and/or retain some analytes in the filtered solutions. In multiclass, multiresidue analysis of veterinary drugs, it is challenging to find one type of filter membrane that does not retain at least some of the analytes before injection in ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). In this study, different filter membranes were tested for use in UHPLC-MS/MS analysis of 183 diverse drugs in bovine muscle, kidney, and liver tissues. Membranes evaluated consisted of polytetrafluoroethylene (PTFE), polyvinylidene difluoride (PVDF), polyethersulfone, nylon, and regenerated cellulose. Drug classes represented among the analytes included ß-agonists, ß-lactams, anthelmintics, macrolides, tetracyclines, sulfonamides, tranquilizers, (fluoro)quinolones, anti-inflammatories, nitroimidazoles, coccidiostats, phenicols, and others. Although the presence of a matrix helped reduce the binding of analytes on surface active sites, all of the filter types partially retained at least some of the drugs in the final extracts. In testing by flow-injection analysis, all of the membrane filters were also observed to leach interfering components. Ultimately, filtration was avoided altogether in the final sample preparation approach known as the quick, easy, cheap, effective, rugged, safe, efficient, and robust (QuEChERSER) mega-method, and ultracentrifugation was chosen as an alternative.

Analysis of 14 ß-agonists in pork using an automated wooden tip-based solid-phase microextraction device and ultra-high-performance liquid chromatography-tandem mass spectrometry.

This study introduces a cost-effective, automated ultra-high-performance liquid chromatography-tandem mass spectrometry method for the detection of 14 ß-agonists in pork using a novel solid-phase microextraction probe composed of polyacrylonitrile and molecularly imprinted polymer. Integrated into an automated extraction device, the probe optimizes extraction prior to analysis while reducing expenses and time compared to traditional solid-phase extraction procedures. The method validation followed the Chinese National Standard (GB/T 27404-2008) and examined limits of detection, limits of quantification, matrix effects, linearity, intraday, and interday precision. Average recovery rates ranged from 71.6% to 82.2%, with relative standard deviations less than 15%. Limits of detection and limits of quantification ranged from 0.09 to 0.39 and 0.27 to 0.99 µg/kg, respectively. The new method identified positive samples more accurately than the current National Standard GB/T 31658.22-2022 and demonstrated its potential for routine assessment and regulatory compliance in the detection of ß-agonists in pork.

Development, validation, and implementation of an ultratrace analysis method for the determination of moenomycin A, in aquatic animal products.

Moenomycin A, an antimicrobial growth promoter widely used as an additive in aquaculture feedstuffs, has been restricted for use in the European Union and China due to its potential risk of promoting resistant strains of pathogenic bacteria and causing residues in aquatic animal products. Although methods for analyzing moenomycin A in feedstuffs have been developed, no established method exists for aquatic matrices. In this study, we present, for the first time, a sensitive and validated high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of moenomycin A in aquatic animal products. Samples were extracted using methanol and purified with the QuEChERS method employing C18 sorbent. The aliquot was dried under a nitrogen stream, reconstituted with methanol-water solvent, and analyzed by HPLC-MS/MS. The developed method exhibited good linearity (r2 > 0.995) over a wide concentration range (1-100 µg/L) and a low limit of detection (1 µg/kg). Average recoveries ranged between 70 and 110% at spiked concentrations of 1, 50, and 100 µg/kg, with associated intra- and inter-day relative standard deviations of 1.25 to 7.32% (n = 6) and 2.91 to 10.08% (n = 3), for different representative aquatic animal production, respectively. To the best of our knowledge, this is the first reported HPLC-MS/MS method for the quantification of moenomycin A in aquatic animal products. The new approach was effectively employed in the analysis of moenomycin A across various aquatic samples.

Surveillance of veterinary drug residues in food commonly consumed in Singapore and assessment of dietary exposure.

Non-judicious and indiscriminate use of veterinary drugs in animal husbandry may result in accumulation of residues in animal tissues, and consequently in food for human consumption. The abuse of veterinary drugs presents a potential risk to consumer health, especially if the residue level is higher than the health-based guidance value (HBGV) such as the acceptable daily intake (ADI). Contamination of drug residues in food also promotes the emergence of antimicrobial resistance (AMR) which poses a serious threat to public health globally. There has been limited information on the occurrence and dietary exposure to veterinary drug residues in Singapore to date. In this study, the occurrence of four classes of veterinary drugs, namely beta-agonists, coccidiostats, fluoroquinolones and macrolides, were determined using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in food widely consumed by Singapore residents. The magnitude of dietary exposure was assessed based on the consumption profile of Singapore population. Out of 216 food samples, 9.72 % were detected positive with veterinary drug residues, where majority of the positive samples were poultry and its derived products, followed by eggs and egg products. 7 veterinary drugs, specifically ciprofloxacin, enrofloxacin, clopidol, diclazuril, lasalocid, nicarbazin and tilmicosin, were detected in the samples, with clopidol and enrofloxacin being the most frequently detected drugs. Dietary exposure was evaluated using the estimated daily intake (EDI) of the detected drugs and benchmarked against the corresponding acceptable daily intake (ADI). All the %ADI values were far less than 100 in both the average and high consumer scenarios, indicating that the health risk associated with dietary exposure to these drugs in Singapore is low.

Novel filter-press single-step cleanup approach facilitated rapid screening and accurate quantification of 112 veterinary drugs in aquatic products.

In this study, a novel filter-press cleanup column was developed as a single-step cleanup approach for the rapid screening and quantification of 112 veterinary drugs in fish samples. Fish muscle samples were extracted with acetonitrile and ethyl acetate, sequentially. After concentration and reconstitution, N-propylethylenediamine (PSA) sorbent, packed in filter-press column, allows rapid single-step cleanup operation, while UHPLC-Q-Orbitrap-HRMS provides high-precision mass information in multi-residue screening. Under optimum settings, the detection and quantification limits were validated at 0.5 and 2.0 µg·kg-1, for all analytes, respectively. The ranges of recoveries were from 35.3 to 138.4%. Most of these target analytes (82%) could be measured with recoveries between 60 and 130%, and intra-day RSDs ranging from 1.9 to 26.1%. This method was further applied to evaluate the residual of veterinary drugs in fish samples from four cities in China, and results demonstrated its practicability for multi-residue monitoring veterinary residues for food safety administration.

Residue Depletion Profile and Estimation of Withdrawal Period for Sulfadimethoxine and Ormetoprim in Edible Tissues of Nile Tilapia (Oreochromis sp.) on Medicated Feed.

Sulfadimethoxine (SDM) and ormetoprim (OMP) are antimicrobials used in combination to treat bacterial infections in fish farming. The use of this drug combination is not yet regulated in some countries, such as Brazil. Due to the lack of regulated drugs for aquaculture in Brazil, this study investigated the residue depletion profile of SDM and OMP in Nile tilapia (Oreochromis sp.) after oral administration. Fish were treated with medicated feed containing a 5:1 ratio of SDM:OMP at the dose of 50 mg kg BW-1 for five consecutive days with an average water temperature of 28 °C. The drugs were incorporated into the feed by using a gelatin coating process which promoted homogeneity in drug concentration and prevented the drug leaching into the water during medication. The SDM and OMP determination in fish fillets (muscle plus skin in natural proportions) was performed using the QuEChERS approach followed by LC-MS/MS quantification. The analytical method was validated according to Brazilian and selected international guidelines. A withdrawal period of 9 days (or 252 °C days) was estimated for the sum of SDM and OMP residues at concentration levels below the maximum residue level of 100 µg kg-1.

A review on recent advances in mass spectrometry analysis of harmful contaminants in food.

Food safety is a widespread global concern with the emergence of foodborne diseases. Thus, establishing accurate and sensitive detection methods of harmful contaminants in different food matrices is essential to address and prevent the associated health risks. Among various analytical tools, mass spectrometry (MS) can quantify multiple impurities simultaneously due to high resolution and accuracy and can achieve non-target profiling of unknown pollutants in food. Therefore, MS has been widely used for determination of hazardous contaminants [e.g., mycotoxin, pesticide and veterinary drug residues, polychlorinated biphenyls (PCBs), dioxins, acrylamide, perfluorinated compounds (PFCs) and p-Phenylenediamine compounds (PPDs) in food samples]. This work summarizes MS applications in detecting harmful contaminants in food matrices, discusses advantages of MS for food safety study, and provides a perspective on future directions of MS development in food research. With the persistent occurrence of novel contaminants, MS will play a more and more critical role in food analysis.

A single exposure to sub-lethal concentrations of a glyphosate-based herbicide or fluoxetine-based agent on growth performance in Nile tilapia.

The aim of the present study was to determine e whether a single acute 96 hr exposure of a glyphosate-based herbicide (GBH) to Nile tilapia fingerlings affected growth performance during the first 90 days of culture. This association was considered as GBH increases serotoninergic activity that affect fish anorexically. Although these findings were based upon chronic investigations, this study was designed to examine whether a single, acute, but excessive concentration GBH might impair growth performance in fish. In parallel, fish were also exposed to fluoxetine (FLU), a drug that selectively inhibits the reuptake of serotonin in brain synapses, leading to increased serotoninergic activity. Data demonstrated a decreased growth performance in fingerlings exposed to GBH or FLU compared to unexposed fingerlings. In fact, FLU-exposed fingerlings exhibited lower average weight and length, diminished weight gain, which resulted in lower final biomass. GBH-exposed fish, despite displaying a lower mean body weight, exhibited a biomass similar to biomass on controls. These body weight differences were noted after 30-60- and 90-day growth period in clean water. In an aquaculture context, these observed changes may be considered harmful to the production or economic performance of large-scale farming as currently practiced in tilapia farming.