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1.
Artigo em Inglês | MEDLINE | ID: mdl-38346259

RESUMO

Brazil plays an important role in ensuring its position on the international market by assuring high food safety standards for its products, and all products should meet the requirements for residues from veterinary drugs and contaminants in animal products. Statutory monitoring provides insights into the compliance of the Brazilian industry regarding these legal requirements. The objective of this study was to provide insight into the safety of Brazilian animal products by reporting the occurrence of residues from veterinary drugs and contaminants according to an analysis of an 11-year report published by the Brazilian Ministry of Agriculture, Livestock and Food Supply (MAPA). Between 2010 and 2021, 166,647 samples from animal-derived products were analyzed in Brazil, and 624 of those samples were non-compliant (0.37%) exceeding maximum residue limits (>MRLs) or showed the presence of prohibited substances. The most common types of substances found in the non-compliant samples were heavy metals, parasiticides, and antimicrobials, accounting for 82% of all documents from the MAPA. Among Brazilian products, the challenge related to occurrence of substances varied across the food supply chain, with highest incidence rates observed in the fish chain, followed by eggs, milk, equids, sheep/goat, honey, bovine, swine, and broilers chains in decreasing order. Considering the type of substance, heavy metals were found to be more prevalent in fish products, mainly arsenic in wild fish. The prevalence of contaminants and heavy metals decreased, while that of veterinary drugs increased in Brazilian products from 2010 to 2021. From these results, it can be concluded that the number of accidental incidents including those associated with environmental contaminants decreased over the last decade, opposed to those involving human adversaries and deliberate illegal actions, such as the abuse of veterinary drugs, increased. Future monitoring plans need to take this paradigm shift into account.


Assuntos
Resíduos de Drogas , Metais Pesados , Drogas Veterinárias , Humanos , Animais , Bovinos , Suínos , Ovinos , Contaminação de Alimentos/análise , Brasil , Galinhas , Drogas Veterinárias/análise , Metais Pesados/análise , Resíduos de Drogas/análise
2.
J Sep Sci ; 47(3): e2300696, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-38356232

RESUMO

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.


Assuntos
Resíduos de Drogas , Drogas Veterinárias , Animais , Bovinos , Espectrometria de Massas em Tandem/métodos , Cromatografia Gasosa-Espectrometria de Massas , Cromatografia Líquida , Cromatografia Líquida de Alta Pressão/métodos , Antibacterianos/análise , Drogas Veterinárias/análise , Resíduos de Drogas/análise
3.
Food Chem ; 443: 138493, 2024 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-38281413

RESUMO

A 15-channel pressure filtration purification method was presented for high throughput sample preparation of aquatic products. A cost-effective device was constructed and melamine sponge was selected as the cleanup sorbent. Upon interfacing with HPLC-MS/MS, the analytical procedure demonstrated its suitability for quantifying 160 pesticides and veterinary drug residues in aquatic products such as fish, shrimp, and crab. The method achieved sample recoveries ranging from 61.3 to 124.9 %. The detection limits were established between 0.5 and 1.0 µg/kg, while the quantitation limits were confirmed to be within the range of 1.0-2.0 µg/kg. The method was applied to quantify the pesticide and veterinary drug residues in mostly consumed aquatic products from five coastal provinces in China. The results showed significant differences between different aquatic products in the concentrations of pesticide and veterinary drug residues, implying the necessity of supervision for the accurate determination of pesticides and veterinary drugs.


Assuntos
Resíduos de Praguicidas , Praguicidas , Triazinas , Drogas Veterinárias , Animais , Praguicidas/análise , Espectrometria de Massas em Tandem/métodos , Drogas Veterinárias/análise , 60705 , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Praguicidas/análise , Extração em Fase Sólida/métodos
4.
Anal Methods ; 16(6): 856-863, 2024 02 08.
Artigo em Inglês | MEDLINE | ID: mdl-38240139

RESUMO

A rapid and highly sensitive method was established for the analysis of 37 veterinary drug residues in milk using a modified QuEChERS method based on a reduced graphene oxide-coated melamine sponge (rGO@MeS) coupled with UPLC-MS/MS. Under optimal chromatographic and mass spectrometric conditions, the effects of different dehydrated salts (MgSO4 and Na2SO4) and metal chelating agents (Na2EDTA) on extraction efficiency were first investigated. Next, the influence of a dynamic and static purification mode was evaluated in terms of drug recoveries. Calibration curves of 37 veterinary drugs were constructed in the range 0.6-500 µg kg-1, and good linearities were obtained with all determination coefficients (R2) ≥0.992. The limits of detection (LODs) and quantitation (LOQs) were in the range 0.3-1.1 µg kg-1 and 0.6-3.5 µg kg-1, respectively. The recoveries of all compounds were in the range 61.3-118.2% at three spiked levels (20, 100, and 200 µg kg-1) with RSDs ≤15.4% for both intra- and inter-day precisions. Compared to pristine melamine sponges and commercial adsorbents (C18, PSA, and GCB), rGO@MeS demonstrated an equal or even better purification performance in terms of recoveries, matrix effects, and matrix removal efficiency. This method is rapid, simple, efficient, and appropriate for the qualitative and quantitative analyses of 37 veterinary drug residues in milk, providing a new detection strategy and technical support for the routine analysis of animal-derived food.


Assuntos
Grafite , Espectrometria de Massas em Tandem , Triazinas , Drogas Veterinárias , Animais , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida , Cromatografia Líquida de Alta Pressão , Drogas Veterinárias/análise , Leite/química , 60705
5.
Artigo em Inglês | MEDLINE | ID: mdl-37582153

RESUMO

Analyte stability is more commonly a confounding factor in analytical chemistry than many analysts recognize. In this study, we assessed the stability of 31 common veterinary drugs in water and final extracts of bovine (milk and kidney/liver) and chicken (muscle and egg) matrices. Two different sample preparation methods were evaluated for one-month storage of the final extracts at typical room, refrigerator, and freezer temperatures. Liquid chromatography - mass spectrometry (LC-MS) by triple quadrupole and high-resolution techniques was used for analysis of the extracts spiked at different relevant concentrations for general regulatory purposes (10-1000 ng/g sample equivalent). Comparison of results between two labs demonstrated that stable drugs (≤20% loss) at all tested conditions consisted of danofloxacin, enrofloxacin, florfenicol, flubendazole, hydroxy-flubendazole, flumequine, flunixin, 5-hydroxy-flunixin, lincomycin, and meloxicam. The tested drugs found to be the most unstable (>20% loss at room temperature within a matter of days) consisted of the ß-lactams (ampicillin, cefalexin, cloxacillin, and penicillin G). Curiously, the following antibiotics (mostly macrolides) were apparently more stable in sample extracts than water: emamectin, erythromycin, ivermectin, lasalocid, monensin, tilmicosin, tulathromycin, and tylosin. Those and the other drug analytes (ciprofloxacin, doxycycline, florfenicol amine, 2-amino-flubendazole, oxytetracycline, sulfadiazine, sulfadimethoxine, sulfamethazine, and trimethoprim) were mostly stable for a month in refrigerated extracts, especially at higher concentrations, but not in all cases. In practice, freezer storage of extract solutions was found to be acceptable for at least a month, with a few exceptions.


Assuntos
Resíduos de Drogas , Drogas Veterinárias , Animais , Bovinos , Drogas Veterinárias/análise , Espectrometria de Massas em Tandem/métodos , Antibacterianos/análise , Resíduos de Drogas/análise , Água/análise
6.
J Agric Food Chem ; 71(34): 12839-12848, 2023 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-37528805

RESUMO

Veterinary drug residues present in foods can pose severe health threats to the population. The present study aims to develop a high-resolution mass spectral library of 158 veterinary drugs of 16 different classes for their rapid identification in food samples through liquid chromatography-high-resolution electrospray ionization-tandem mass spectrometry (LC-HR-ESI-MS/MS). Standard drugs were pooled according to their log P values and exact masses before analysis. Spectra were collected at system automated collision energy, i.e., of 25-60 eV and four predetermined collision energies (10, 20, 30, and 40 eV) for each compound using a schedule precursor list of [M + H]+, [M + Na]+, and [M + NH4]+ ions. The utility of the developed database was checked by analyzing food samples. A total of 17 veterinary drugs based on the reference standard retention times (RTs), HR-MS spectra, and MS/MS spectra were identified in the analyzed samples. Moreover, five veterinary drugs were selected for quantitative analysis, including doxycycline hyclate, lincomycin, sulfasalazine, moxifloxacin, and diphenoxylate, using liquid chromatography-ion trap mass-spectrometry (LC-IT-MS). Concentrations of the drug were obtained to vary from 0.0805 to 0.9731 mg/kg in food samples and were found to be exceeded in most of the cases as per the maximum residue levels described by Food and Agriculture Organization (FAO)/World Health Organization (WHO). The MS data were submitted to the MetaboLights online database (MTBLS2914). This study will help in the high-throughput screening of multiclass veterinary drugs in foodstuffs.


Assuntos
Espectrometria de Massas em Tandem , Drogas Veterinárias , Espectrometria de Massas em Tandem/métodos , Espectrometria de Massas por Ionização por Electrospray/métodos , Drogas Veterinárias/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Cromatografia Líquida/métodos , Íons/química , Cromatografia Líquida de Alta Pressão
7.
J Hazard Mater ; 459: 132195, 2023 10 05.
Artigo em Inglês | MEDLINE | ID: mdl-37541118

RESUMO

Veterinary drugs are of concern in terms of potential environmental pollution and their negative impacts on avian scavengers. These pharmaceuticals reach vultures through the consumption of carcasses of previously treated livestock. Here, we analysed samples from livestock carcasses (n = 159), avian scavenger tissues (n = 116) and plasma (n = 312) for 49 compounds commonly used in veterinary medicine in Aragon (NE Spain) and nearby regions. Samples were analysed using liquid chromatography with electrospray ionization mass spectrometry (LC-ESI-MS/MS). We detected pharmaceuticals in 54.1% of livestock carcasses analysed (50.3% with antibiotics, 10.8% with NSAIDs). For veterinary pharmaceuticals in tissues and plasma from avian scavengers, we detected pharmaceuticals in 51.7% and 28.5% of samples, respectively. Antibiotics were detected in 50.9% and 25.3% while NSAIDs were determined in 6.0% and 5.5% of tissues and plasma from avian scavengers, respectively. Moreover, caffeine was detected in plasma in 73.7% of vultures sampled at landfill sites, indicating its usefulness as a biomarker of urban garbage ingestion. We found an association between livestock carcasses, especially pigs and chickens, and the presence of veterinary pharmaceuticals in avian scavengers. We highlight that carcass disposal for feeding avian scavengers must address the potential risks posed by veterinary pharmaceutical residues.


Assuntos
Falconiformes , Drogas Veterinárias , Animais , Suínos , Drogas Veterinárias/toxicidade , Drogas Veterinárias/análise , Gado , Cafeína/toxicidade , Espectrometria de Massas em Tandem , Galinhas , Antibacterianos , Anti-Inflamatórios não Esteroides , Instalações de Eliminação de Resíduos
8.
Food Chem ; 428: 136712, 2023 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-37441938

RESUMO

Excessive use of veterinary drugs in livestock growth poses a threat to food safety. It is, however, challenging to quantify these multi-class veterinary drugs within animal muscles, because of their varied physicochemical properties. In this work, we presented a simple, efficient and sensitive method for the simultaneous determination of multi-class veterinary drugs with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The method involves a highly efficient extraction using a EDTA (pH 7)-ACN (30:70, v/v) solvent system, followed by a one-step solid-phase extraction cleanup approach with PRiME HLB sorbent (Reversed-phase N-vinylpyrrolidone and divinylbenzene copolymer). For all the analytes, over a wide range of polarity, satisfactory recoveries were obtained between 70% and 120%, with relative standard deviations <15%. Excellent sensitivities were achieved with the limits of quantification ranging from 0.2 µg/kg to 3.0 µg/kg. This developed method provides a new targeted strategy for the analysis of multi-class veterinary drugs in muscle matrices.


Assuntos
Resíduos de Drogas , Drogas Veterinárias , Animais , Cromatografia Líquida de Alta Pressão/métodos , Espectrometria de Massas em Tandem/métodos , Drogas Veterinárias/análise , Resíduos de Drogas/análise , Músculos/química , Extração em Fase Sólida/métodos
9.
Molecules ; 28(10)2023 May 17.
Artigo em Inglês | MEDLINE | ID: mdl-37241891

RESUMO

Food safety is recognized as a main requirement for consumers, food industries, and official laboratories. Here, we present the optimization and screening qualitative validation of two multianalyte methods in bovine muscle tissues by ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry with an Orbitrap-type analyzer, operated with a heated ionization source in positive and negative mode. This aims for not only the simultaneous detection of veterinary drugs regulated in Brazil but also the prospection of antimicrobials not yet monitored. Two different sample preparation procedures were applied: method A-generic solid-liquid extraction with 0.1% formic acid (v/v) in an aqueous solution of EDTA 0.1% (w/v)-acetonitrile-methanol (1:1:1, v/v/v), followed by an additional ultrasound-assisted extraction and method B-QuEChERS. In both procedures, selectivity showed satisfactory conformity. From a detection capability (CCß) equivalent to ½ the maximum residue limit, >34% of the analyte resulted in a false positive rate of <5%, preponderant by the QuEChERS method, which exhibited a higher yield of the sample. The results showed the potential application of both procedures in the routine analysis of foods by official laboratories, enabling the expansion of this methodological portfolio as well as its analytical scopes, thus optimizing the control of residues of veterinary drugs in the country.


Assuntos
Drogas Veterinárias , Animais , Bovinos , Cromatografia Líquida de Alta Pressão/métodos , Brasil , Drogas Veterinárias/análise , Limite de Detecção , Músculos/química
10.
J Hazard Mater ; 445: 130570, 2023 03 05.
Artigo em Inglês | MEDLINE | ID: mdl-37055976

RESUMO

This study investigated the behavior of veterinary antibiotics (VAs) in a small farm ecosystem. Manure and environmental samples were collected around a large pig farm in northeast China. Thirty-four VAs in six categories were analyzed. Then, a multimedia fugacity model was used to estimate the fates of VAs in the environment. The results showed that VAs were prevalent in manure, soil, water, and sediment, but not in crops. Compared with fresh manure, VA levels were significantly lower in surface manure piles left in the open air for 3-6 months. The main VAs, tetracyclines and quinolones, decreased by 427.12 and 158.45 µg/kg, respectively. VAs from manure piles were transported to the surroundings and migrated vertically into deep soil. The concentrations of ∑VAs detected in agricultural soils were 0.03-4.60 µg/kg; > 94% of the mass inventory of the VAs was retained in soil organic matter (SOM), suggesting that SOM is the main reservoir for antibiotics in soil. Risk assessment and model analysis indicated that the negative impact of mixed antibiotics at low concentrations in farmland on crops may be mediated by indirect effects, rather than direct effects. Our findings highlight the environmental fates and risks of antibiotics from livestock farms.


Assuntos
Antibacterianos , Monitoramento Ambiental , Poluentes do Solo , Drogas Veterinárias , Animais , Antibacterianos/análise , China , Produtos Agrícolas , Ecossistema , Monitoramento Ambiental/métodos , Fazendas , Esterco/análise , Solo , Poluentes do Solo/análise , Suínos , Drogas Veterinárias/análise
11.
BMC Vet Res ; 19(1): 39, 2023 Feb 09.
Artigo em Inglês | MEDLINE | ID: mdl-36759841

RESUMO

BACKGROUND: Otitis externa is a commonly diagnosed dermatological disorder in canines. The pathogens primarily involved in canine otitis externa (COE) include Staphylococcus pseudintermedius, Pseudomonas aeruginosa, Proteus mirabilis, and Malassezia pachydermatis. As COE tends to be superficial, medications delivered topically are often effective and practical in managing the condition. As such, there is a wide variety of approved topical products currently available in the market. The efficacy of topical dosage forms can be dependent on various factors such as the pharmacology of active constituents and the physicochemical properties of the formulation, including pH, viscosity, spreadability, and bio-adhesion. Currently, there is a lack of published literature available on the optimal properties of topical COE products. In this study, we compared the physicochemical properties of nine commercially available otic veterinarian products in Australia used clinically to manage COE. RESULTS: Based on our comparative analysis, the pH (6.26 ± 0.04) of an aqueous-based product was similar to a healthy dog's external auditory canal. Products containing polymers exhibited higher viscosity and bio-adhesion. Spreadability was inversely related to viscosity and Osurnia ® a product with high viscosity demonstrated the lowest spreadability. Aqueous-based otic products showed better syringebility whereas oil-based systems required higher force to expel the products. Variability in droplet size was noted. Derm Otic, Baytril Otic, and Aurizon Ear Drops had the lower standard deviation which indicates they would give a more consistent dose. CONCLUSIONS: Findings from this work provide considerations for industry researchers or formulation scientists working in the area of otic dosage formulations.


Assuntos
Fármacos Dermatológicos , Doenças do Cão , Otite Externa , Drogas Veterinárias , Animais , Cães , Austrália , Doenças do Cão/tratamento farmacológico , Otite Externa/tratamento farmacológico , Otite Externa/veterinária , Fármacos Dermatológicos/análise , Fármacos Dermatológicos/química , Drogas Veterinárias/análise , Drogas Veterinárias/química
12.
Food Chem ; 408: 135207, 2023 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-36527921

RESUMO

This work aimed to develop an integrated high-throughput screening and quantification for multi-class veterinary drug residues by HPLC-Q-Orbitrap mass spectrometry. A qualitative screening mass database of 171 veterinary drugs was created using full scanning mode, which improved the screening accuracy and scope. Beef and chicken samples were chosen to validate the quantification method at three spiked concentration levels. The quantification method of 146 veterinary drug residues was developed. After enzymatic hydrolysis, beef and chicken samples were treated using optimized QuEChERS. The calibration curves showed good linearities with correlation coefficients of 0.9921-0.9994. The recovery rates were within 52.1-138.2 % with relative standard deviations 0.4-17.7 %. The limits of detection and limits of quantification were in the range of 0.15-3.03 µg/kg and 0.5-10 µg/kg, respectively. The proposed method was demonstrated to be reliable for the simultaneous analysis of multi-class veterinary drugs. It is of significance to expand the screening scope and quantitative analysis efficiency.


Assuntos
Resíduos de Drogas , Drogas Veterinárias , Animais , Bovinos , Cromatografia Líquida de Alta Pressão/métodos , Galinhas , Drogas Veterinárias/análise , Espectrometria de Massas/métodos , Resíduos de Drogas/análise
13.
Food Chem ; 408: 135244, 2023 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-36565550

RESUMO

The use of veterinary drugs (VDs) is widely administered to animals for both therapeutic and prophylactic purposes. However, their improper use may involve their occurrence in the final products intended for human consumption. In this scientific work, a method for the investigation of target (n = 30) VDs residues and retrospective suspect screening followed by confirmation using analytical standards of others 38 contaminants in ready-to-eat cooked ham by ultra-high performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was developed. The extraction was performed based on the QuEChERS approach and validated in accordance with the European Regulation 2021/808. The application of the in-house validated method to ready-to-eat cooked ham showed the occurrence of fourteen VDs residues. Despite the important incidence, the concentration levels found were below the maximum residue limits set for VDs in porcine muscle, except for colchicine. Constant monitoring of animals derived food is strongly recommended to ensure the food safety of consumers.


Assuntos
Inocuidade dos Alimentos , Drogas Veterinárias , Humanos , Animais , Suínos , Cromatografia Líquida de Alta Pressão/métodos , Estudos Retrospectivos , Limite de Detecção , Espectrometria de Massas/métodos , Drogas Veterinárias/análise
14.
Environ Pollut ; 316(Pt 2): 120626, 2023 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-36370968

RESUMO

Modern agriculture depends highly on pesticides and pharmaceutical preparations, so controlling exposure to these substances in the feed and food chain is essential. This article presents the first study on residues of a broad spectrum of pesticides and veterinary drugs in the diets of dairy cattle. One hundred and two representative samples of the complete diets, including basal feed rations and additional fed concentrate, were collected in three Austrian provinces (Styria, Lower and Upper Austria) in 2019 and 2020. The samples were tested for >700 pesticides, veterinary drugs and related metabolites using a validated method based on liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS). In total, 16 residues (13 pesticides and three veterinary drug residues) were detected. > 90% of the diets contained pesticide residues and <10% veterinary drug residues, whereas banned pesticides were not found. The most frequent pesticide residues were fluopyram (62%), piperonyl butoxide (39%) and diethyltoluamide (35%). The following pesticides exceed the default EU maximum residue level (MRL) (10 µg kg-1) for products exclusively used for animal feed production: Benzovindiflupyr (proportion of samples > MRLs: 1%), bixafen (2%), fluopyram (6%), ipconazole (1%) and tebuconazole (3%). Three residues (dinitrocarbanilide, monensin and nicarbazin) of veterinary drugs were identified, all below the MRLs. Over 60% of the evaluated samples contained mixtures of two to six residues/sample. Only one pesticide (diethyltoluamide) presented a significant difference among regions, with higher concentrations in Upper Austria. Brewery's spent grains were the dietary ingredient that showed the strongest correlation to pesticide residues. These findings evidence the realistic scenario of highly occurrent low doses of pesticides cocktails in the feed/food chain, which may affect the animal, human and environmental health. Since the risk assessments are based on single pesticides, the potential synergistic effect of co-occurring chemicals ("cocktail effect") requires further investigations.


Assuntos
Resíduos de Praguicidas , Praguicidas , Drogas Veterinárias , Animais , Humanos , Bovinos , Resíduos de Praguicidas/análise , Drogas Veterinárias/análise , Praguicidas/análise , Espectrometria de Massas em Tandem/métodos , Áustria , Agricultura Orgânica , Dieta , Contaminação de Alimentos/análise
16.
Molecules ; 27(19)2022 Sep 20.
Artigo em Inglês | MEDLINE | ID: mdl-36234695

RESUMO

The presence of unauthorized substances, such as residues of veterinary medicines or chemical contaminants, in food can represent a possible health concern. For this reason, a complete legislative framework has been established in the European Union (EU), which defines the maximum limits allowed in food and carries out surveillance programs to control the presence of these substances. Official food control laboratories, in order to ensure a high level of consumer protection, must respond to the challenge of improving and harmonizing the performance of the analytical methods used for the analysis of residues of authorized, unauthorized, or prohibited pharmacologically active substances. Laboratories must also consider the state of the art of the analytical methodologies and the performance requirements of current legislation. The aim of this work was to develop a multiresidue method for the determination of antibiotics in milk, compliant with the criteria and procedures established by Commission Implementing Regulation (EU) 2021/808. The method uses an LC-Orbitrap-HRMS for the determination of 57 molecules of antibiotic and active antibacterial substances belonging to different chemical classes (beta-lactams, tetracyclines, sulfonamides, quinolones, pleuromutilins, macrolides, and lincosamides) in bovine, ovine, and goat milk samples. It provides a simple and quick sample pretreatment and a subsequent identification phase of analytes, at concentrations equal to or lower than the maximum residual limit (MRL), in compliance with Commission Regulation (EU) 2010/37. The validation parameters: selectivity, stability, applicability, and detection capability (ccß), are in agreement with the requirements of Commission Implementing Regulation (EU) 2021/808 and demonstrated the effectiveness of the method in detecting veterinary drug residues at the target screening concentration (at the MRL level or below), with a false positive rate of less than 5%. This method represents an effective solution for detecting antibiotics in milk, which can be successfully applied in routine analyses for official food control plans.


Assuntos
Quinolonas , Drogas Veterinárias , Animais , Antibacterianos/análise , Bovinos , Feminino , Inocuidade dos Alimentos , Cabras , Lincosamidas/análise , Macrolídeos/análise , Leite/química , Quinolonas/análise , Ovinos , Sulfonamidas/análise , Tetraciclinas/análise , Drogas Veterinárias/análise , beta-Lactamas
17.
Environ Sci Process Impacts ; 24(12): 2357-2367, 2022 Dec 14.
Artigo em Inglês | MEDLINE | ID: mdl-36285718

RESUMO

The content of veterinary drugs in manure is usually estimated by the amount of residues determined in its solid or liquid phase, individually, which previously required a separation step. As an alternative, a multiresidue method for the analysis of 48 veterinary drugs and other contaminants of emerging concern (CECs) in swine raw manure as a whole has been developed and in-house validated in this work. The impact of several experimental factors during ultrasound assisted extraction was assessed. Hence, the use of alumina seemed to especially decrease the matrix effect and improve the overall recovery of drugs, mainly those with a high octanol-water partition coefficient. CECs in the extracts were analyzed by ultra-high performance liquid chromatography coupled to mass spectrometry in tandem. A standard addition-matrix matched calibration was used for quantification. Application of the method to two related samples (raw manure and farm centrifuged raw manure) from a facility revealed that the concentrations of CECs determined in the raw manure by the comprehensive methodology were higher than those calculated by adding the concentrations measured in the solid and liquid phases, separately. This was attributed to the loss of CECs adsorbed on fine particles in the suspension during the sample preparation procedure of the liquid-phase. Furthermore, the decrease of residues in the raw manure when this is centrifuged in the farm to yield compost is shown.


Assuntos
Esterco , Drogas Veterinárias , Suínos , Animais , Esterco/análise , Drogas Veterinárias/análise , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida de Alta Pressão/métodos , Extração em Fase Sólida/métodos
18.
J Agric Food Chem ; 70(35): 10886-10898, 2022 Sep 07.
Artigo em Inglês | MEDLINE | ID: mdl-36018326

RESUMO

Current screening capabilities for veterinary drugs (VDs) in foods are limited, requiring time-consuming and expensive trace-level analyses. For the first time, a high-throughput planar solid-phase extraction (HTpSPE) cleanup, controlled by UV/vis/FLD imaging, was developed for screening 81 VDs from 6 different groups (glucocorticoids, anthelmintics, antiparasitics, coccidiostats, nonsteroidal anti-inflammatory drugs, and antibiotics) in 4 different matrices (honey, pig muscle, cow milk, and chicken eggs). It consumed 13 times less solvent and was more eco-friendly and 5 times faster than routine methods. The VDs were automatically eluted using the autoTLC-LC-MS interface, separated online on a high-performance liquid chromatography column via a 10-min gradient, and detected by Orbitrap high-resolution tandem mass spectrometry. The screening method was validated according to the latest European Commission Implementing Regulation 2021/808. Most VDs except penicillins and cephalosporins were detected at the 5-µg/kg level in pig muscle, cow milk, and chicken eggs and 25-µg/kg level in honey.


Assuntos
Resíduos de Drogas , Drogas Veterinárias , Animais , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/análise , Extração em Fase Sólida/métodos , Suínos , Espectrometria de Massas em Tandem/métodos , Drogas Veterinárias/análise
19.
Molecules ; 27(14)2022 Jul 08.
Artigo em Inglês | MEDLINE | ID: mdl-35889250

RESUMO

Manure is a major source of soil and plant contamination with veterinary drugs residues. The aim of this study was to evaluate the uptake of 14 veterinary pharmaceuticals by parsley from soil fertilized with manure. Pharmaceutical content was determined in roots and leaves. Liquid chromatography coupled with tandem mass spectrometry was used for targeted analysis. Screening analysis was performed to identify transformation products in the parsley tissues. A solid-liquid extraction procedure was developed combined with solid-phase extraction, providing recoveries of 61.9-97.1% for leaves and 51.7-95.6% for roots. Four analytes were detected in parsley: enrofloxacin, tylosin, sulfamethoxazole, and doxycycline. Enrofloxacin was detected at the highest concentrations (13.4-26.3 ng g-1). Doxycycline accumulated mainly in the roots, tylosin in the leaves, and sulfamethoxazole was found in both tissues. 14 transformation products were identified and their distribution were determined. This study provides important data on the uptake and transformation of pharmaceuticals in plant tissues.


Assuntos
Poluentes Ambientais , Poluentes do Solo , Drogas Veterinárias , Doxiciclina/análise , Enrofloxacina/análise , Poluentes Ambientais/análise , Esterco/análise , Petroselinum , Solo/química , Poluentes do Solo/análise , Extração em Fase Sólida/métodos , Sulfametoxazol , Tilosina , Drogas Veterinárias/análise
20.
Molecules ; 27(14)2022 Jul 13.
Artigo em Inglês | MEDLINE | ID: mdl-35889354

RESUMO

A method was developed for the rapid and quantitative analysis of 30 veterinary drugs belonging to 17 classes (amphenicols (1), anthelmintics (1), cephalosporins (4), coccidiostats (1), lincosamides (1), macrolide (1), nitroimidazole (1), penicillins (3), phenylhydrazines (1), polypeptides (1), pyrethrins (1), quinolones (5), sulfonamides (3), tetracycline (3), neuroleptic agents (1), triazene trypanocidal agents (1), other. (1)) in feeds. The proposed method with a modified Quick Polar Pesticides (QuPPe) sample preparation was validated for the determination of 30 veterinary drugs in feed samples by liquid chromatography triple-quadrupole mass spectrometry (LC-MS/MS). The sample was extracted with methanol containing 1% acetic acid and purified by dispersive solid-phase extraction (d-SPE) with C18. Good linearity (r2 ≥ 0.98) was observed, and the LOQ values ranged from 10 to 200 µg/kg. Average recoveries ranged from 70.8 to 118.4%, and the relative standard deviation was ≤ 18.7%. This validated method was used in the determination of 30 veterinary drugs in 142 feed samples obtained from South Korea. The results show that lincomycin was present in only one of the tested feed samples, although it was detected at a value lower than the LOQ. In conclusion, this multi-residue method can be used for screening through the detection and quantitation of residual multiclass veterinary drugs in feed samples.


Assuntos
Praguicidas , Drogas Veterinárias , Antibacterianos/análise , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida/métodos , Praguicidas/análise , Extração em Fase Sólida , Espectrometria de Massas em Tandem/métodos , Drogas Veterinárias/análise
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