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1.
Artigo em Inglês | MEDLINE | ID: mdl-32406796

RESUMO

The effect of tetracyclines used for swine food-production (tetracycline and oxytetracycline) on enriched nitrifying bacteria cultures over time was investigated in this study. Short-term exposure assays were performed in different concentrations of each antibiotic, using ammonia oxidizing bacteria (AOB) culture and nitrifying bacteria. The results pointed out a higher inhibitory effect of tetracycline on both bacterial communities. The AOB was more sensitive to antibiotic exposure when compared to the nitrifying culture. Although high antibiotic concentrations were applied, the half maximal inhibitory concentration (IC50) was achieved only for the AOB culture exposed to tetracycline at a concentration of 273 mg L-1. Nonetheless, the long-term exposure assay demonstrated a reduction of the tetracycline inhibition effect against AOB. The exposure to 100 mg L-1 of tetracycline (TC) did not show relevant influence over ammonium conversion efficiency; however, at 128 mg L-1 of TC, the efficiency decreased from 94% to 72%. Further investigation revealed that TC reduced the final effluent quality due to the development of a resistance mechanism by AOB culture against this antibiotic. This mechanism involves increasing the excretion of extracellular polymeric substances (EPS) and soluble microbial products (SMP), which probably increases BOD, and reduces ammonia consumption by the bacterial culture.


Assuntos
Compostos de Amônio/análise , Nitrificação/efeitos dos fármacos , Esgotos/microbiologia , Tetraciclinas/análise , Drogas Veterinárias/análise , Águas Residuárias/microbiologia , Purificação da Água/métodos , Animais , Bactérias/efeitos dos fármacos , Bactérias/crescimento & desenvolvimento , Matriz Extracelular de Substâncias Poliméricas/metabolismo , Oxirredução , Esgotos/química , Suínos , Tetraciclinas/toxicidade , Drogas Veterinárias/toxicidade , Águas Residuárias/química
2.
J Chromatogr A ; 1617: 460808, 2020 Apr 26.
Artigo em Inglês | MEDLINE | ID: mdl-31982099

RESUMO

An ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method based on selective accelerated solvent extraction and magnetic material purification was established to analyze the residues of various veterinary antibiotics and agricultural fungicides and insecticides in livestock and poultry excrement. Methanol-acetonitrile (4:1, V/V) was used as the extraction solvent and static extraction was conducted three times in 5 min. Preliminary purification was achieved by adding 0.5 g acidic alumina-florisil (1:1, W/W) to the extraction cell while the extraction was conducted. This preliminarily-purified extract was further purified using magnetic material, then analyzed using UPLC-MS/MS. Under optimal conditions, 33 types of antibiotics, including 3 amphenicols, 8 macrolides, 17 sulfonamides and 5 nitroimidazoles, as well as 37 types of pesticides, including 27 insecticides and 10 fungicides, were detected. Recoveries ranged from 60.3% to 110.0% at three spiked concentrations (10 µg/kg, 20 µg/kg and 50 µg/kg), the detection limits ranged from 0.2 to 3.5 µg/kg and the quantitative limits ranged from 0.5 to 11.5 µg/kg. This newly-established method was tested using 30 livestock and poultry excrement samples and confirmed its use for determining veterinary drugs and pesticides in practical samples.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Praguicidas/análise , Espectrometria de Massas em Tandem/métodos , Drogas Veterinárias/análise , Animais , Antibacterianos/análise , Fungicidas Industriais/análise , Inseticidas/análise , Limite de Detecção , Gado , Macrolídeos/análise , Resíduos de Praguicidas/isolamento & purificação , Praguicidas/análise , Aves Domésticas , Drogas Veterinárias/isolamento & purificação
3.
Molecules ; 25(2)2020 Jan 10.
Artigo em Inglês | MEDLINE | ID: mdl-31936806

RESUMO

Recent years have seen the increased utilization of ionic liquids (ILs) in the development and optimization of analytical methods. Their unique and eco-friendly properties and the ability to modify their structure allows them to be useful both at the sample preparation stage and at the separation stage of the analytes. The use of ILs for the analysis of pharmaceuticals seems particularly interesting because of their systematic delivery to the environment. Nowadays, they are commonly detected in many countries at very low concentration levels. However, due to their specific physiological activity, pharmaceuticals are responsible for bioaccumulation and toxic effects in aquatic and terrestrial ecosystems as well as possibly upsetting the body's equilibrium, leading to the dangerous phenomenon of drug resistance. This review will provide a comprehensive summary of the use of ILs in various sample preparation procedures and separation methods for the determination of pharmaceuticals in environmental and biological matrices based on liquid-based chromatography (LC, SFC, TLC), gas chromatography (GC) and electromigration techniques (e.g., capillary electrophoresis (CE)). Moreover, the advantages and disadvantages of ILs, which can appear during extraction and separation, will be presented and attention will be given to the criteria to be followed during the selection of ILs for specific applications.


Assuntos
Monitoramento de Medicamentos , Líquidos Iônicos/química , Drogas Veterinárias , Animais , Humanos , Drogas Veterinárias/análise , Drogas Veterinárias/farmacocinética
4.
J Chromatogr A ; 1611: 460613, 2020 Jan 25.
Artigo em Inglês | MEDLINE | ID: mdl-31629489

RESUMO

In this work, the use of design of experiments and posterior data modelling by artificial neural network (ANN) and least squares (LS) is presented as a suitable analytical tool for the performance optimization of a tandem mass spectrometric detector coupled to ultra-high performance liquid chromatography for the analysis of seventeen veterinary drugs. Firstly, a central composite design was built considering as factors the cone, capillary, extractor and radio frequency voltages of the mass spectrometer in order to obtain a proper combination to improve the sensitivity of the method. Secondly, a one factor design considering the collision voltage was built to define the adequate voltage for each daughter ion. The response surface methodology (RSM) was then applied, and the prediction capability of ANN and LS were compared. As conclusion, the ANN modelling provided better results than LS, both in terms of the ANOVA and predicted areas results. The accuracy of the model prediction was between 85 and 125%, confirming that the estimates of the model were correct, and endorsing the optimization procedure as a suitable way to gather excellent results. The suitability of the new approach and its implications on the simultaneous analysis of seventeen veterinary drugs by ultra-high liquid chromatography coupled to tandem mass spectrometry detection are discussed.


Assuntos
Redes Neurais de Computação , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida de Alta Pressão , Eletricidade , Análise dos Mínimos Quadrados , Solventes/química , Drogas Veterinárias/análise
5.
Food Chem ; 303: 125399, 2020 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-31470274

RESUMO

It is still a challenge to solve the matrix interferences in veterinary drug residue analysis. In this study, we reported a thin layer chromatography (TLC)-high-performance liquid chromatography (HPLC) method for determining total florfenicol (FF) residues, expressed as florfenicol amine (FFA), in porcine edible tissues. The tissue homogenate were acid-hydrolyzed to liberate the bound residues and convert them into FFA. The hydrolysates were washed with ethyl acetate and subsequently extracted with ethyl acetate under alkaline conditions. The supernatants were concentrated through evaporation, defatted with hexane, purified by TLC and analyzed by HPLC at 225 nm. The optimal developing solvent for TLC purification was ethyl acetate-acetone-ammonium hydroxide mixtures (2:8:0.5, v/v/v). The method was fully validated according to decision 2002/657/EC, and could be used for the routine monitoring of FF residues in pig. TLC showed excellent purification efficiency, and was expected to solve the matrix interferences in veterinary drug residue analysis.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Cromatografia em Camada Delgada/métodos , Resíduos de Drogas/análise , Tianfenicol/análogos & derivados , Drogas Veterinárias/análise , Estruturas Animais/química , Animais , Cromatografia Líquida/métodos , Carne/análise , Suínos , Tianfenicol/análise
6.
Food Chem ; 309: 125746, 2020 Mar 30.
Artigo em Inglês | MEDLINE | ID: mdl-31718837

RESUMO

A multi-class screening method for the determination of veterinary drugs and pesticides in eggs was developed by high performance liquid chromatography quadrupole-time-of-flight mass spectrometry (HPLC-QTOF-MS). A single-injection workflow was developed for qualitative analysis, and method validation was conducted in terms of retention time deviation (ΔRt), exact mass error (Δm), selectivity, specificity, precision and trueness. The characteristic fragment ions in information dependent acquisition (IDA) mode were summarized for retrospective and non-target screening. Five of 70 samples were found positive with sulfachloropyridazine, sulfamonomethoxine and fipronil sulfone. Compared with triple-quadrupole (QqQ) MS method, the obtained results showed that QTOF-MS gave comparable results to QqQ-MS with residue concentrations higher than 10 µg·kg-1, whereas QqQ-MS was more powerful at lower concentrations (<1 µg·kg-1). Moreover, the amount of fragment ions acquired by HPLC-QTOF-MS decreased substantially at trace levels, which may be a potential cause of reduced reliability of identification.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Ovos/análise , Contaminação de Alimentos/análise , Praguicidas/análise , Espectrometria de Massas em Tandem/métodos , Drogas Veterinárias/análise , Animais , Galinhas , Sensibilidade e Especificidade
7.
Spectrochim Acta A Mol Biomol Spectrosc ; 224: 117395, 2020 Jan 05.
Artigo em Inglês | MEDLINE | ID: mdl-31362184

RESUMO

This work describes the development of highly sensitive as well as simple two spectrofluorimetric methods for the determination of apramycin sulfate. The first method depends on measuring the inherent native fluorescence of the aqueous neutral solution of the drug at 388 nm (λex 335 nm). While the second method mainly based on enhancing the native fluorescence intensity of the drug using sodium dodecyl sulfate (SDS) micellar media by about 4 fold enhancement. The fluorescence intensity - concentration relationship for the two methods was found rectilinear over the concentration range 1.0-100.0 and 0.1-20.0 µg/mL for the first and second method respectively. The limit of detection for method I and II were 0.05 and 0.02 µg/mL respectively. The proposed methods can be effectively connected for the assurance of the medication without impedances from common normal excipients. Furthermore, the two methods were high sensitive enough for the assurance of the drug in spiked milk samples with high percentage recoveries.


Assuntos
Leite/química , Nebramicina/análogos & derivados , Espectrometria de Fluorescência/métodos , Animais , Resíduos de Drogas/análise , Concentração de Íons de Hidrogênio , Limite de Detecção , Modelos Lineares , Nebramicina/análise , Reprodutibilidade dos Testes , Drogas Veterinárias/análise
8.
Molecules ; 24(24)2019 Dec 17.
Artigo em Inglês | MEDLINE | ID: mdl-31861089

RESUMO

In the last years, the European Commission has adopted restrictive directives on food quality and safety in order to protect animal and human health. Veterinary drugs represent an important risk and the need to have sensitive and fast analytical techniques to detect and quantify them has become mandatory. Over the years, the availability of different modes, interfaces, and formats has improved the versatility, sensitivity, and speed of capillary electrophoresis (CE) techniques. Thus, CE represents a powerful tool for the analysis of a large variety of food matrices and food-related molecules with important applications in food quality and safety. This review focuses the attention of CE applications over the last decade on the detection of different classes of drugs (used as additives in animal food or present as contaminants in food products) with a potential risk for animal and human health. In addition, considering that the different sample preparation procedures have strongly contributed to CE sensitivity and versatility, the most advanced sample pre-concentration techniques are discussed here.


Assuntos
Resíduos de Drogas/análise , Eletroforese Capilar , Análise de Alimentos , Contaminação de Alimentos/análise , Drogas Veterinárias/análise , Animais , Eletroforese Capilar/métodos , Análise de Alimentos/métodos , Qualidade dos Alimentos , Inocuidade dos Alimentos , Humanos
9.
Se Pu ; 37(9): 946-954, 2019 Sep 08.
Artigo em Chinês | MEDLINE | ID: mdl-31642298

RESUMO

A method was established to rapidly determine 20 kinds of veterinary drug residues including three catagories of antibiotics (sulfonamides, quinolones, and chloramphenicols) and two kinds of triphenylmethanes (malachite green (MG) and leucomalachite green (LMG)) in fish and shrimp, based on dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry. The samples were first hydrolyzed using a dipotassium hydrogen phosphate solution, and then extracted using acetonitrile. Afterward, the extraction solution was dehydrated and salted out with sodium chloride and condensed to nearly dry using a rotating evaporator. This residue was dissolved in 1.0 mL methanol. The resulting solution was purified by dispersive solid phase extraction method with C18 and PSA sorbents, and filtered through a filter. The target compounds were separated employing a ZORBAX C18 column. The mass spectrometer datas were acquired by multiple reaction monitoring (MRM) of positive and negative modes and quantitated applying the isotope internal standard method. The 20 veterinary drugs showed a good linear relationship in the range of 0.2-300 µg/L. The limits of detection and the limits of quantification were 0.1-0.6 and 0.3-1.8 µg/kg, respectively, while the correlation coefficients were greater than 0.99. The average recoveries at the three spiked levels (1, 5, and 20 times of quantitative limits) ranged between 72.5%-118%, with the relative standard deviations of 1.9%-9.8%. The advantages of method include a simple pretreatment, a high detection efficiency, and a low cost. Moreover, it is suitable for the simultaneous determination of multiple veterinary drug residues in fish and shrimp.


Assuntos
Resíduos de Drogas/análise , Alimentos Marinhos/análise , Drogas Veterinárias/análise , Animais , Antibacterianos/análise , Cromatografia Líquida de Alta Pressão , Extração em Fase Sólida , Espectrometria de Massas em Tandem , Compostos de Tritil/análise
10.
J Sep Sci ; 42(21): 3340-3351, 2019 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-31509638

RESUMO

This research deals with the development of a stability-indicating high-performance liquid chromatography method for simultaneous determination of amprolium hydrochloride and ethopabate. To the best of our knowledge, no comprehensive stability-indicating method has been reported for analysis of this mixture. Separation was achieved using Kromasil cyano column with gradient elution of the mobile phase composed of sodium hexane sulfonate solution and methanol. Quantification was based on measuring peak areas at 266 nm. Amprolium and ethopabate peaks eluted at retention times 10.42 and 18.53 min, respectively. The proposed procedure was validated with respect to system suitability, linearity, ranges, precision, accuracy, specificity, robustness, detection, and quantification limits. Linearity ranges for amprolium and ethopabate were 1.5-240 and 1-160 µg/mL, respectively. Analytes were subjected to stress conditions of hydrolysis, oxidation and thermal degradation. The proposed method enabled resolution of drugs from their forced-degradation products and amprolium related substance (2-picoline). Moreover, specificity was verified by resolution of the analytes from about 22 drugs used in antimicrobial veterinary products. The validated method was successfully applied to assay of the combined veterinary powder dosage form, additionally it was implemented in the accelerated stability study of the dosage form when stored for six months at 40°C and 75% relative humidity.


Assuntos
Amprólio/análise , Etopabato/análise , Drogas Veterinárias/análise , Cromatografia Líquida de Alta Pressão , Estabilidade de Medicamentos , Umidade , Pós/química
11.
Environ Pollut ; 255(Pt 1): 113039, 2019 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-31521994

RESUMO

Although the poultry production sector plays a key role in sustaining the majority of animal protein demand in Egypt, the deleterious effects of widespread antibiotic resistance on health and environment are currently not well recognized. Litter and dropping samples from broiler and layer poultry farms as well as, tilapia samples from the Nile River and aquaculture farms were collected from Upper Egypt. Samples were extracted and examined for tetracycline residues [tetracycline (TC), chlortetracycline (CTC), oxytetracycline (OTC) and doxycycline (DC)] using HPLC. In addition, tetracycline resistance genes [tet (M), tet (W), tet (Q) and tet (G)] were screened from pooled intestinal contents collected from twelve broiler farms in Upper Egypt. The antibiotic resistance genes results revealed that tet (W) was confirmed to be expressed in all intestinal samples. In contrast, tet (Q) and tet (M) were detected only in 42% and 17% of the samples, respectively. CTC and OTC were the antimicrobial compounds with the highest concentrations in poultry litter and droppings, with concentrations of 6.05 and 2.47 µg g-1 (CTC) and 5.9 and 1.33 µg g-1 (OTC), respectively. However, the concentrations of DC were significantly higher than those of the other compounds in both aquaculture and Nile River tilapia. The tetracycline residue levels in aquaculture tilapia were significantly higher than those in Nile River tilapia. The hazard quotients (HQs) exceeded 1 for OTC, CTC and DC, which highlights the great risk of using broiler litter to fertilize agricultural land. Moreover, the presence of DC and CTC indicates that consumption of aquaculture tilapia poses a considerable health risk. Therefore, poultry litter or droppings containing tetracycline residues and tet resistance determinants used for aquaculture or as farmland fertilizers could be major sources of antibiotic resistance in fish, humans and environment.


Assuntos
Antibacterianos/análise , Galinhas/crescimento & desenvolvimento , Resistência a Tetraciclina/genética , Tetraciclina/análise , Tilápia/crescimento & desenvolvimento , Drogas Veterinárias/análise , Animais , Aquicultura , Ecologia , Egito , Fazendas , Fertilizantes , Conteúdo Gastrointestinal/química , Conteúdo Gastrointestinal/microbiologia , Esterco/análise , Esterco/microbiologia , Músculos/química , Aves Domésticas , Medição de Risco , Alimentos Marinhos/análise
12.
Biosens Bioelectron ; 142: 111554, 2019 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-31382098

RESUMO

Maduramicin (MD) is a type of monoglycoside polyether ionophore antibiotic that can effectively treat coccidiosis and facilitate animal growth. However, its extensive and excessive use brings potential risk to human health. Herein, an electrochemical immunosensor based on indirect competitive format was fabricated for analysis of MD residue in eggs by a multiple signal amplification system. Initially, Au nanoparticles were deposited onto glassy carbon electrode surface to load the coating antigen MD-BSA and to improve conductivity. Then the signal amplification platform was constructed by encapsulating hemin into Fe-MIL-88 NH2 metal-organic frameworks (hemin@MOFs), and then the obtained composites were decorated with AuPt nanoparticles. The synthesized hemin@MOFs/AuPt was not only used as a signal amplification mediator, but also utilized as a carrier for immobilization of horseradish peroxidase-conjugated affinipure goat anti-mouse antibody (Ab2-HRP) and horseradish peroxidase (HRP). The constructed hemin@MOFs/AuPt-Ab2-HRP bioconjugates could effectively amplify the current signal since hemin@MOFs, AuPt and HRP all exhibited high catalytic activity towards the hydrogen peroxide. Moreover, the established immunosensor showed high sensitivity and stability during the detection procedure. With the synergistic catalytic effect of hemin@MOFs, AuPt and HRP, a wide detection range of 0.1-50 ng mL-1 and a low detection limit of 0.045 ng mL-1 were achieved (S/N = 3), respectively. Ultimately, the developed method displayed excellent performance in practical applications, providing a promising probability to detect other veterinary drug residues to guarantee food safety.


Assuntos
Antibacterianos/análise , Ouro/química , Hemina/química , Lactonas/análise , Estruturas Metalorgânicas/química , Drogas Veterinárias/análise , Animais , Anticorpos Imobilizados/química , Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/métodos , Análise de Alimentos/métodos , Humanos , Imunoensaio/métodos , Limite de Detecção , Nanopartículas Metálicas/química , Nanopartículas Metálicas/ultraestrutura , Platina/química
13.
Shokuhin Eiseigaku Zasshi ; 60(3): 52-60, 2019.
Artigo em Japonês | MEDLINE | ID: mdl-31391411

RESUMO

We developed an analytical method for determining 15 antifungal drugs, 2 antiparasitic drugs, and 3 veterinary drugs in fish and livestock products using LC-MS/MS. First, 50% ethanol was added to their products, and the mixture was homogenized to reduce drug degradation. Thereafter, 20 drugs were extracted from the pretreated sample mixture using acetonitrile. Cleanup was performed using an alumina-N SPE cartridge. Finally, chromatographic separation was performed using a fully porous octadecyl silanized silica column. The new method is applicable to fish in which the matrix hampers accurate analysis. It was validated on 8 fish and livestock products. Drug recovery rates ranged from 70.2 to 109.3%, RSDs of repeatability were <18.0%, and RSDs of within-laboratory reproducibility were <18.7%. It fulfills the Japanese guideline criteria. The limits of quantification were estimated as 3 ng/g.


Assuntos
Antifúngicos/análise , Contaminação de Alimentos/análise , Carne/análise , Alimentos Marinhos/análise , Drogas Veterinárias/análise , Animais , Cromatografia Líquida , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem
14.
J Agric Food Chem ; 67(46): 12663-12669, 2019 Nov 20.
Artigo em Inglês | MEDLINE | ID: mdl-31398029

RESUMO

A fully automated high-throughput method using solid-phase microextraction (SPME) was developed and validated for quantitative analysis of more than 100 veterinary drugs in chicken and beef tissue. The work also encompassed a comparison of the SPME method to two well-documented sample preparation procedures, solvent extraction (SE) and quick, easy, cheap, effective, rugged, and safe (QuEChERS). SPME showed considerably less matrix effects, with only two compounds showing significant matrix effects in comparison to 30% of analytes in QuEChERS and 42% in SE in beef tissue. Excellent accuracy and precision results were achieved with all methods in the chicken matrix, with more than 91% of analytes falling within the 70-120% range of their true concentrations and relative standard deviation of ≤25% at 0.75X and 1.5X, where X is the maximum residue level. Similar results were achieved in beef tissue. All methods were able to meet regulatory limit of quantitation levels for the majority of target analytes.


Assuntos
Fracionamento Químico/métodos , Resíduos de Drogas/análise , Resíduos de Drogas/isolamento & purificação , Contaminação de Alimentos/análise , Carne/análise , Microextração em Fase Sólida/métodos , Drogas Veterinárias/análise , Drogas Veterinárias/isolamento & purificação , Animais , Bovinos , Galinhas , Limite de Detecção
15.
Bull Environ Contam Toxicol ; 103(4): 610-616, 2019 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-31468105

RESUMO

A growing concern exists over water contamination by veterinary pharmaceuticals from small pig farms in Yucatan, Mexico, where the anaerobic digesters installed as the wastewater treatment system are not operated properly. Therefore, considerable interest exists to develop analytical methods to detect these compounds and characterize their fate in the environment. In this study, the detection of three antibiotics (enrofloxacin, oxytetracycline and sulfamethoxazole) and a ß-agonist (ractopamine) was carried out using fluorescence spectrophotometry, with a semi-quantitative approach and a low environmental impact. Wastewater samples from 10 pig farms were analyzed, detecting concentrations of approximately 0.043 µg mL-1 for enrofloxacin, 1.427 µg mL-1 for oxytetracycline, and 9.748 µg mL-1 for sulfamethoxazole. The detection of these pharmaceuticals in the effluents of treated wastewater from the biodigesters of the pig farms suggests the need to optimize the system and prevent the entry of these compounds into the environment.


Assuntos
Monitoramento Ambiental/métodos , Espectrometria de Fluorescência/métodos , Drogas Veterinárias/análise , Poluentes Químicos da Água/análise , Animais , Antibacterianos , Fazendas , Química Verde , México , Fenetilaminas , Suínos , Águas Residuárias/análise , Águas Residuárias/química
16.
Artigo em Inglês | MEDLINE | ID: mdl-31361192

RESUMO

A liquid chromatography high resolution mass spectrometry (LC-HRMS) screening method was developed previously to analyze for veterinary drug residues commonly found in different types of aquaculture products. This method has been further evaluated for its feasibility to detect several other classes of compounds that might also be a concern as possible contaminants in farmed tilapia, salmon, eel and shrimp. Some chemicals could contaminate water sources used in aquaculture production through agricultural run-off. These compounds include several widely used triazine herbicides, organophosphate and carbamate pesticides, as well as various discarded human pharmaceuticals. Other possible contaminants investigated were selected disinfectants, some newer antibiotics, growth promoters, and various parasiticides. The sample preparation consisted of an acidic acetonitrile extraction followed by solid-phase extraction clean-up. Data were collected with a quadrupole-Orbitrap MS using both non-targeted and targeted acquisition. This rapid clean-up procedure and HRMS detection method described previously for veterinary drug residues also worked well for many other types of compounds. Most analytes had screening limit levels between 0.5-10 ng/g in the matrices examined using exact mass identification criteria. The strategy described in this paper for testing the performance of additional analytes will help expand the applicability of the HRMS procedure as aquaculture samples can now be analyzed for a wider range of contaminants.


Assuntos
Aquicultura , Resíduos de Drogas/análise , Produtos Pesqueiros/análise , Peixes , Análise de Alimentos , Contaminação de Alimentos/análise , Praguicidas/análise , Drogas Veterinárias/análise , Animais , Cromatografia Líquida , Humanos , Espectrometria de Massas
17.
Artigo em Inglês | MEDLINE | ID: mdl-31287377

RESUMO

Four analytical methods were developed and validated for the determination of veterinary drug residues and environmental pesticide residues in honey: (a) GC-MS method for the analysis of amitraz and all metabolites containing the 2,4-dimethylaniline moiety; (b) GC-MS method for the analysis of thymol, chlorfenvinphos and coumaphos; (c) GC-MS method for the analysis of 75 active substances; (d) LC-MS/MS method for the analysis of 60 active substances. Between the GC-MS (method c) and the LC-MS/MS method (method d) there was no overlap among active substances, meaning that using both methods 135 active substances originating from the environment in total were included and validated. The first method involved hydrolysis of amitraz and its metabolites containing the 2,4-dimethylaniline moiety to 2,4-dimethylaniline and extraction of 2,4-dimethylaniline to n-hexane. The other three methods had the same extraction procedure with a mixture of solvents: acetone, dichloromethane and petroleum ether. All 4 methods were tested in practice. Sixty samples of honey were analysed: 22 from organic and 38 from conventional production. Overall, residues were mainly higher than reported in literature but did not exceed MRLs. Risk assessment confirmed that the analysed samples are of no cause for concern for consumers.


Assuntos
Resíduos de Drogas/análise , Análise de Alimentos , Contaminação de Alimentos/análise , Mel/análise , Resíduos de Praguicidas/análise , Drogas Veterinárias/análise , Cromatografia Líquida , Cromatografia Gasosa-Espectrometria de Massas , Resíduos de Praguicidas/metabolismo , Eslovênia , Espectrometria de Massas em Tandem , Drogas Veterinárias/metabolismo
18.
Sci Total Environ ; 692: 259-266, 2019 Nov 20.
Artigo em Inglês | MEDLINE | ID: mdl-31349167

RESUMO

Traditional swine manure treatments are not fully effective in the removal of veterinary drugs. Moreover, they are costly and entail a significant carbon footprint in many cases. Innovative biological approaches based on phototrophic microorganisms have recently emerged as promising alternatives to overcome those limitations. This work evaluated the removal of 19 veterinary drugs (i.e., 16 antibiotics, 1 analgesic, 1 anti-parasitic and 1 hormone) from piggery wastewater (PWW) in two open photobioreactors (PBR) operated with a consortium of microalgae-bacteria (AB-PBR) and purple photosynthetic bacteria (PPB-PBR). Multiple hydraulic retention times (HRT), in particular 11, 8 and 4 days, were tested during stage I, II and III, respectively. Ten out of 19 target compounds were detected with inlet drug concentrations ranging from 'non-detected' (n.d.) to almost 23,000 ng L-1 for the antibiotic oxytetracycline. Moreover, three of the antibiotics (i.e., enrofloxacin, sulfadiazine and oxytetracycline) were found at concentrations above the analytical linearity range in some or all of the samples under study. AB-PBR supported higher removal efficiencies (REs) than PPB-PBR, except for danofloxacin. Overall, REs progressively decreased when decreasing the HRT. The highest REs (>90%) were observed for doxycycline (95 ±â€¯3%) and oxytetracycline (93 ±â€¯3%) in AB-PBR during stage I. The other drugs, except sulfadimidine that was the most recalcitrant, showed REs above 70% during stage I in the same photobioreactor. In contrast, no removal was observed for danofloxacin in AB-PBR during stage III, sulfadimidine in PPB-PBR during stage III or marbofloxacin in PPB-PBR during the entire experiment.


Assuntos
Bactérias/metabolismo , Microalgas/metabolismo , Consórcios Microbianos , Fotobiorreatores/microbiologia , Drogas Veterinárias/análise , Eliminação de Resíduos Líquidos/métodos , Criação de Animais Domésticos , Animais , Proteobactérias/metabolismo , Sus scrofa , Eliminação de Resíduos Líquidos/instrumentação , Águas Residuárias/análise
19.
Food Chem ; 293: 187-196, 2019 Sep 30.
Artigo em Inglês | MEDLINE | ID: mdl-31151600

RESUMO

A generic extraction and UHPLC-Q-Orbitrap™-HRMS method was developed for four insect species (mealworm, grasshopper, house cricket and black soldier fly) analyzing a large spectrum of organic chemical contaminants, including pesticides (n = 25), (veterinary) drugs (n = 29), and mycotoxins (n = 23). To prove the method as 'fit-for-purpose', a successful validation was performed, both qualitatively, by determining the screening detection limit (SDL), selectivity and specificity, as well as semi-quantitatively, by assessing the within-day precision (relative standard deviation (RSD)) and recovery. For both the mealworm, grasshopper, house cricket and black soldier fly, 64, 61, 59 and 62 compounds were detected at the respective SDL levels (1-100 µg kg-1), predominantly below existing maximum residue limits for other edible matrices. Mean recoveries ranged between 70% and 120% and RSD-values were in line with European regulations (CD 2002/657/EC; SANCO). Finally, the potential of the screening methodology was demonstrated on real insect samples, revealing minor to no contamination.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Insetos/química , Espectrometria de Massas/métodos , Micotoxinas/análise , Praguicidas/análise , Drogas Veterinárias/análise , Animais , Inocuidade dos Alimentos , Insetos/metabolismo , Limite de Detecção , Micotoxinas/isolamento & purificação , Praguicidas/isolamento & purificação , Extração em Fase Sólida , Drogas Veterinárias/isolamento & purificação
20.
Chemosphere ; 230: 337-346, 2019 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-31108445

RESUMO

We developed a QuEChERS (quick, easy, cheap, effective, rugged and safe) method for the high through-put determination of 28 common veterinary antibiotics in swine wastewater using one-step dispersive solid-phase extraction (d-SPE) for sample cleanup and ultra-performance liquid chromatography-tandem mass spectrometry for detection. The orthogonal test method was used to systematically investigate the parameters that might influence d-SPE efficiency. The optimal d-SPE procedure utilized 40 mg primary secondary amine sorbent and 3 g L-1 Na2EDTA. The recoveries ranged from 50 to 100% with relative standard deviations <20% for all target analytes except for enrofloxacin and chlortetracycline. The limits of detection and limits of quantification for all the analytes ranged from 0.002 to 0.200 ng mL-1 and 0.005-0.500 ng mL-1, respectively. The developed method was successfully applied to the analysis of 28 antibiotic residues in swine wastewater from 10 pig farms located in central China. Fourteen antibiotics including 4 sulfonamides (sulfadiazine, sulfamerazine, sulfamonomethoxine and trimethoprim), 5 fluoroquinolones (norfloxacin, ciprofloxacin, pefloxacin, enrofloxacin, and ofloxacin), 1 lincosamide (lincomycin) and 4 tetracyclines (doxycycline, tetracycline, oxytetracycline, and chlortetracycline) were detected at levels ranging from 0.0560 to 1793 ng mL-1. Our results demonstrated that the optimized method is a simple but reliable analytical technique for the routine monitoring of veterinary antibiotics in swine wastewater. Swine wastewater samples that we analyzed from 10 pig farms in Jiangxi Province, China were highly contaminated and pose a serious threat to ecosystems and to public health.


Assuntos
Antibacterianos/análise , Drogas Veterinárias/análise , Águas Residuárias/química , Poluentes Químicos da Água/análise , Animais , China , Cromatografia Líquida , Ensaios de Triagem em Larga Escala , Extração em Fase Sólida/métodos , Suínos , Espectrometria de Massas em Tandem/métodos
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