Your browser doesn't support javascript.
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 3.015
Filtrar
1.
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
3.
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
4.
Se Pu ; 37(9): 1011-1018, 2019 Sep 08.
Artigo em Chinês | MEDLINE | ID: mdl-31642307

RESUMO

In this study, ultra performance liquid chromatography-quadrupole electrostatic field orbitrap mass spectrometry was used to establish a high-throughput screening method for 20 ß -blockers and their metabolites in foods of animal origin. The sensitivity and applicability of the established method were improved by optimizing the instrument and pretreatment conditions. The samples were purified by high speed centrifugation at low temperature, and the compounds were separated by a C8 column. Qualitative and quantitative analyses of the compounds were performed in full MS/dd-MS2 (data-dependent MS2) mode. Twenty compounds showed a good linear relationship in the range 0.1-10 µg/L, with correlation coefficients (r2) greater than 0.99. The limits of detection (LODs) ranged from 1 to 5 µg/kg, while the limits of quantification (LOQs) ranged from 2 to 10 µg/kg. The average recoveries were 60.37%-100.84%, with relative standard deviations less than 10%. The method is operationally simple and has good reproducibility and high accuracy, which are essential for ß -blockers and metabolite residue screening in foods of animal-origin.


Assuntos
Antagonistas Adrenérgicos beta/análise , Resíduos de Drogas/análise , Contaminação de Alimentos/análise , Animais , Cromatografia Líquida de Alta Pressão , Limite de Detecção , Espectrometria de Massas , Carne/análise , Reprodutibilidade dos Testes
5.
J Agric Food Chem ; 67(38): 10756-10763, 2019 Sep 25.
Artigo em Inglês | MEDLINE | ID: mdl-31483626

RESUMO

AFEX treatment of crop residues can greatly increase their nutrient availability for ruminants. This study investigated the concentration of acetamide, an ammoniation byproduct, in AFEX-treated crop residues and in milk and meat from ruminants fed these residues. Acetamide concentrations in four AFEX-treated cereal crop residues were comparable and reproducible (4-7 mg/g dry matter). A transient acetamide peak in milk was detected following introduction of AFEX-treated residues to the diet, but an alternative regimen showed the peak can be effectively mitigated. Milk acetamide concentration following this transition was 6 and 10 ppm for cattle and buffalo, respectively, but also decreased over time for cattle while tending to decrease (p = 0.08) for buffalo. There was no difference in acetamide concentration in the meat of cattle consuming AFEX-treated residues for 160 days compared to controls. Further investigation is necessary to determine the metabolism of acetamide in ruminants and a maximum acceptable daily intake for humans.


Assuntos
Acetamidas/análise , Ração Animal/análise , Bovinos/metabolismo , Produtos Agrícolas/química , Resíduos de Drogas/análise , Contaminação de Alimentos/análise , Carne/análise , Leite/química , Acetamidas/metabolismo , Amônia/química , Animais , Búfalos , Dieta/veterinária , Digestão , Leite/metabolismo
6.
Artigo em Inglês | MEDLINE | ID: mdl-31535930

RESUMO

Lincomycin is the first antimicrobial agent described for the lincosamide class and it is commonly used for the treatment of infectious enteric and respiratory diseases in poultry. Maximum residue limits (MRLs) in edible tissues have been established for this antimicrobial, however, no regulation has been proposed yet for by-products that are not intended for direct human consumption. Feathers are a by-product from poultry farming that might be used as an ingredient for diets fed to other farm animal species. The presence of antimicrobial residues in them is not monitored in spite of the fact that several studies have proved that they can persist in feathers. Currently though, no evidence has been presented regarding the behaviour of lincomycin in this matrix. Hence, this work intended to assess the depletion of lincomycin residues in feathers of birds treated with therapeutic doses and compare them with those detected in muscle and liver samples. Samples were collected for several days after ceasing treatment from a group of broiler chickens treated with a 25% lincomycin formulation. Methanol and Florisil® columns were used to extract and retain the analyte, and samples were analysed using a triple quadrupole mass spectrometer (API 5500, AB SCIEX™). On day 1 after ceasing treatment, average concentrations of lincomycin detected in feather samples reached up to 8582 µg kg-1 and by day 16, these had only declined by 63%, to an average of 3138 µg kg-1. Lincomycin residues were detected in feathers at every sampling point, even after they were not detectable in edible tissues. Depletion time was 98 days for feathers, considering the LOQ established for the methodology as cut-off value for the calculations. Data showed that lincomycin is highly persistent in feathers, which may result in this matrix becoming a re-entry route for its residues into the food chain.


Assuntos
Resíduos de Drogas/análise , Lincomicina/análise , Fígado/química , Músculos/química , Animais , Galinhas , Plumas/química
7.
Anal Bioanal Chem ; 411(26): 6913-6929, 2019 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-31418049

RESUMO

A method was developed for the analysis of 22 antiparasitic residues belonging to the benzoylurea, organophosphate, pyrimidinamine, pyrethrin and pyrethroid classes in salmon by liquid chromatography coupled with tandem mass spectrometry. Samples were extracted with acetonitrile-water as the extraction solvent with use of a vibrational shaking apparatus with a ceramic homogenizer. After extraction, the acetonitrile extracts were cleaned up by incubation at low temperature (-20 °C, 1 h) to remove fat, followed by dispersive solid-phase extraction using Z-Sep+ and primary-secondary amine as sorbents. Validation was performed following the 2002/657/EC and SANTE/11813/2017 guidelines. The trueness of the method ranged from 87% to 121% and precision ranged from 4.1% to 23.7%, with the exception of cyphenothrin, dicyclanil and azamethiphos. The method developed is particularly advantageous because the use of a vibrational shaker allows unattended extraction of samples and eliminates a laborious tissue disruption step, which increases sample throughput in the laboratory. The sample preparation and chromatographic separations can be performed in 5 and 4 h, respectively, for 36 samples. Graphical abstract.


Assuntos
Antiparasitários/análise , Praguicidas/análise , Alimentos Marinhos/análise , Animais , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/análise , Peixes/metabolismo , Análise de Alimentos/métodos , Limite de Detecção , Resíduos de Praguicidas/análise , Salmão/metabolismo , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos
8.
Se Pu ; 37(7): 735-741, 2019 Jul 08.
Artigo em Chinês | MEDLINE | ID: mdl-31271013

RESUMO

An analytical method was developed for the determination of streptomycin and dihydrostreptomycin in honey using hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). The streptomycin and dihydrostreptomycin residues in the test samples were extracted with 20 g/L trichloroacetic acid aqueous solution (including 50 mmol/L phosphate, pH 6.8) and cleaned on an Oasis HLB solid phase extraction column. The products were separated on a SIELC Obelisc R column with gradient elution using 0.5% (v/v) formic acid aqueous solution and acetonitrile as mobile phases. Streptomycin and dihydrostreptomycin were detected by liquid chromatography-tandem mass spectrometry in the positive ion mode using the external standard method. Under the optimal conditions, streptomycin and dihydrostreptomycin showed good linearity (r>0.99) in the range of 2.5-100 µg/L. The LOD and LOQ of the method was 2.0 µg/kg and 5.0 µg/kg, respectively. The spiked recoveries of the analytes from blank honey samples at the three levels of 5.0, 20.0 and 100.0 µg/kg were in the range of 86.9%-113.2% with the relative standard deviations less than 10%. With the advantages of convenience, rapidity, sensitivity and good repeatability, the method is suitable for the detection of streptomycin and dihydrostreptomycin in honey.


Assuntos
Sulfato de Di-Hidroestreptomicina/análise , Resíduos de Drogas/análise , Mel/análise , Estreptomicina/análise , Cromatografia Líquida , Interações Hidrofóbicas e Hidrofílicas , Extração em Fase Sólida , Espectrometria de Massas em Tandem
9.
Anal Bioanal Chem ; 411(23): 6129-6139, 2019 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-31278554

RESUMO

Antibiotics may be present in agricultural soils through the application of organic amendments as fertilizers or by irrigation of fields with recycled water. As a result of these agricultural practices, antibiotics in soil can lead to their uptake by plants, entering in this way the food chain. Studies on the levels of antibiotics in cereal samples are scarce in the available literature. In this work, an analytical method was developed for the determination of 19 antibiotics (fluoroquinolones, sulfonamides, tetracyclines, and lincosamides) in four types of cereal grains (wheat, barley, rice, and oat). Ultrasound-assisted matrix solid-phase dispersion was selected as extraction technique with recoveries of target analytes ranging from 73 to 127% for the four cereals analyzed. Limits of quantification obtained ranged from 0.8 to 5.8 ng g-1. Compared with methods described for the analysis of antibiotics in cereals, the developed method uses a lower volume of extraction solvent and very good recoveries were obtained for all compounds. The validated method was applied to the analysis of different types of cereals samples, harvested from agricultural fields or purchased from local supermarkets. The analysis of the five cereal samples grown in fields with 3 years of consecutive organic amendments revealed that none of the nineteen antibiotics selected were found in any sample. Eleven commercial samples of cereals of different types and presentations were analyzed and enrofloxacin was detected in one rice sample; the presence of enrofloxacin in cereals or its incorporation into crops from soil or water not previously reported. Graphical abstract.


Assuntos
Antibacterianos/análise , Resíduos de Drogas/análise , Grão Comestível/química , Contaminação de Alimentos/análise , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida/métodos , Fluoroquinolonas/análise , Limite de Detecção , Lincosamidas/análise , Extração em Fase Sólida/métodos , Sulfonamidas/análise , Tetraciclinas/análise
10.
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
11.
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
12.
Food Chem ; 293: 204-212, 2019 Sep 30.
Artigo em Inglês | MEDLINE | ID: mdl-31151602

RESUMO

Near-infrared microscopy (NIRM) technology can analyze different components within a sample while also obtaining spatial information about the sample. No rapid detection methods are available for effectively identifying antibiotic mycelia residues (AMRs) in protein feeds materials to date. In this study, the feasibility of using NIRM to identify AMRs (oxytetracycline residue, streptomycin sulfate residue and clay colysin sulfate residue) mixed in cottonseed meals was studied. The samples were scanned by NIRM, then the spectra of images were analyzed by principal component analysis (PCA) to select characteristic bands for further identification with one-class partial least squares analysis (OCPLS). The results showed that: a) AMRs were effectively identified in cottonseed meal; b) screening characteristic bands and increasing the spectral number of the calibration set improved the identification results of the model; and c) the sensitivity, specificity, accuracy and class error of the method were 100%, 95.93%, 99.01% and 2.03%, respectively.


Assuntos
Óleo de Sementes de Algodão/química , Resíduos de Drogas/análise , Microscopia/métodos , Micélio/química , Oxitetraciclina/química , Estreptomicina/química , Calibragem , Óleo de Sementes de Algodão/metabolismo , Resíduos de Drogas/química , Análise dos Mínimos Quadrados , Microscopia/normas , Análise de Componente Principal , Espectroscopia de Infravermelho com Transformada de Fourier
13.
Artigo em Inglês | MEDLINE | ID: mdl-31192769

RESUMO

This paper presents the results from a residue study conducted on a statistically representative number of chicken broilers that were individually orally treated with the selected nitroimidazoles (metronidazole, ornidazole and ipronidazole) in an appropriate amount close to the theoretical therapeutic dose. A mutual persistence comparison of the monitored analytes in feathers, serum, muscle and shanks was performed and attention was also paid to selected metabolites (hydroxymetronidazole and hydroxyipronidazole). An analytical LC/MS/MS method using SupelMIP SPE nitroimidazoles cartridges was developed for the determination of nitroimidazoles residues in poultry feathers, serum, muscle and shanks and the method was validated according to Commission Decision 2002/657/EC. High concentrations of nitroimidazoles residues in feathers were observed 19 days after the broilers' treatment unlike the muscle and serum samples, where nitroimidazoles depletion was significantly faster (residue concentrations were below detection limits in 5 days in muscle and in 12 days in serum). Shanks (chicken claws) also proved to be a very useful matrix for the detection of nitroimidazoles drugs misuse due to the longer persistence of these drugs residues and their metabolites in this matrix (determinable concentrations were observed 19 days after the broilers' last treatment). Feathers and shanks appear to be suitable matrixes for the screening of various nitroimidazoles in poultry because long-term persistence of residues enables reliable detection of the illegal use of nitroimidazoles compounds in official checks.


Assuntos
Galinhas , Resíduos de Drogas/análise , Plumas/química , Nitroimidazóis/análise , Administração Oral , Animais , Nitroimidazóis/administração & dosagem
14.
Artigo em Inglês | MEDLINE | ID: mdl-31192771

RESUMO

Violative residues of florfenicol (FF) in porcine edible tissues pose a potential risk for human health. In this study, urine was selected as target matrix for routine residue monitoring of FF in pig, and a thin layer chromatography (TLC)-high-performance liquid chromatography (HPLC) method was developed for simultaneously determining FF and florfenicol amine (FFA) in porcine urine. The urine samples were extracted with ethyl acetate under alkaline environment. The extracts were enriched through evaporation, purified by TLC and analysed by HPLC at 225 nm. A Waters Symmetry C18 column was used for the separation of the two analytes. The mobile phase was acetonitrile-phosphate buffer mixtures (33.3: 66.7, v/v), and was pumped at 0.6 mL/min. The TLC-HPLC method was well validated and successfully applied to residue depletion study. Good analytical specificity was confirmed by the lack of interfering peaks at the retention times of FF and FFA. The standard curves showed good linearity (FF: y = 143064x - 1045.3, r= 0.9999; FFA: y = 275826x + 1888.8, r= 0.9999) over the range of 0.0625-8 µg/mL. The precision ranged from 0.83% to 11.66% and 2.19% to 8.75% for intraday and interday determination, respectively. The corresponding accuracy ranged from -13.38% to 10.78% and -12.15% to 7.14%, respectively. The limits of quantification (LOQs) for FF and FFA were 0.125 µg/mL. The residue depletion study showed that the concentrations of FF and FFA in urine were higher than those in edible tissues at three time points. This method was reliable, simple and cost efficient, and could be used to monitor FF residues in porcine edible tissue without slaughtering animals. TLC showed excellent purification efficiency and is expected to solve matrix interferences in veterinary drug residue analysis.


Assuntos
Antibacterianos/urina , Resíduos de Drogas/análise , Contaminação de Alimentos/análise , Suínos/urina , Tianfenicol/análogos & derivados , Drogas Veterinárias/urina , Animais , Cromatografia Líquida de Alta Pressão , Cromatografia em Camada Delgada , Resíduos de Drogas/química , Tianfenicol/urina
15.
J Sci Food Agric ; 99(14): 6234-6240, 2019 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-31250461

RESUMO

BACKGROUND: The application of exogenous plant growth regulator, for example forchlorfenuron (CPPU), on kiwifruits has become an important factor that influences kiwifruit economic efficiency and the health development of the kiwifruit industry. Owing to the slight difference in calyx shape between the kiwifruits treated with CPPU (CPPU-treated kiwifruits) and the kiwifruits without CPPU treatment (CPPU-untreated kiwifruits), this study aims to provide a cheap, quick, convenient, and non-destructive method for identifying CPPU-treated kiwifruits based on the images of kiwifruits captured at visible lights. RESULTS: The identification method includes three steps. Firstly, the kiwifruit was extracted from the background by using Otsu algorithm, hole filling operation and 'bwareaopen' function. Secondly, the calyx was extracted by using corrosion, image enhancement, hole filling and closing operations. Finally, the length/width ratio of the minimum enclosing rectangle of calyx region was calculated. The kiwifruit was regarded as a CPPU-treated kiwifruit if the length/width ratio of the rectangle was higher than 1.6. Otherwise, the kiwifruit was regarded as a CPPU-untreated one. The method had the total identification accuracy rate of 90.0% when the kiwifruit images were captured either by utilizing a smartphone at normal lighting condition or by using an image acquisition system. CONCLUSION: The programs run on computer and smartphone were developed, and they could realize kiwifruit identification in 0.6 s and 2 s, respectively. The study makes identifying CPPU-treated kiwifruits in online processing be realizable, and offers a convenient method for kiwifruit consumers. © 2019 Society of Chemical Industry.


Assuntos
Actinidia/efeitos dos fármacos , Resíduos de Drogas/análise , Frutas/química , Fotografação/métodos , Reguladores de Crescimento de Planta/análise , Polietilenoglicóis/análise , Poliuretanos/análise , Actinidia/química , Resíduos de Drogas/farmacologia , Frutas/efeitos dos fármacos , Reguladores de Crescimento de Planta/farmacologia , Polietilenoglicóis/farmacologia , Poliuretanos/farmacologia , Smartphone
16.
J Agric Food Chem ; 67(27): 7569-7586, 2019 Jul 10.
Artigo em Inglês | MEDLINE | ID: mdl-31198037

RESUMO

The abundant use of antibiotics leads to antibiotic residues in frequently consumed foods. Residual antibiotics in food may have adverse effects on humans by directly causing disease via low-dose exposure and indirect harm via antibiotic resistance. However, the current methods for antibiotic extraction and analysis in food have not yet formed a uniform standard, and only a few data exist regarding the residual antibiotic condition in various types of foods. Hence, we review the literature since 2008 to summarize analytical methods and residue status of antibiotics in food. Then, we discuss the causes of antibiotic residues in food and the possible hazards to human health. We hope that the joint efforts of the scientific community and political circles will lead to the formation of a unified standard for the extraction and analysis of antibiotics in food, to allow for comprehensive monitoring of residual antibiotics and ensure human health.


Assuntos
Antibacterianos/efeitos adversos , Antibacterianos/análise , Resíduos de Drogas/análise , Contaminação de Alimentos/análise , Animais , Cromatografia Líquida/métodos , Resistência Microbiana a Medicamentos , Ovos/análise , Peixes , Nível de Saúde , Humanos , Espectrometria de Massas/métodos , Carne/análise , Leite/química , Produtos Avícolas/análise , Fatores de Risco , Sensibilidade e Especificidade , Verduras/química
17.
Artigo em Inglês | MEDLINE | ID: mdl-31140948

RESUMO

A simple and reliable method using liquid chromatography with diode array detector was developed for the simultaneous determination of florfenicol and thiamphenicol in medicated feed. The analytes were extracted from the minced feed with methanol and ethyl acetate (1:1, v/v). Next, the extract was further cleaned up by dispersive solid phase extraction using anhydrous magnesium sulfate, PSA and C18 sorbents. Finally, 1 mL of extract was evaporated, the residue resuspended in Milli-Q water, and filtered. The method was validated in-house at medicated levels, in the concentration range 10-300 µg/mL (50-1500 mg/kg). Values of <6.5% and <6.0% were found, respectively, for repeatability and within-laboratory reproducibility. The LODs for the two fenicols were 2.4-5.3 mg/kg, while the LOQs were 3.8-5.6 mg/kg. The expanded uncertainty was estimated to be in the range of 10.0-14.5%, depending on the analyte. Recoveries varied from 81.7% to 97.5%. The methodology was applied to the analysis of animal feedingstuffs collected from poultry and pig farms.


Assuntos
Antibacterianos/análise , Resíduos de Drogas/análise , Tianfenicol/análogos & derivados , Tianfenicol/análise , Medicina Veterinária , Ração Animal/análise , Animais , Antibacterianos/administração & dosagem , Antibacterianos/farmacologia , Calibragem , Bovinos , Galinhas , Cromatografia Líquida de Alta Pressão , Prescrições de Medicamentos/veterinária , Resíduos de Drogas/farmacologia , Cavalos , Suínos , Tianfenicol/administração & dosagem , Tianfenicol/farmacologia
18.
Ecotoxicol Environ Saf ; 180: 549-556, 2019 Sep 30.
Artigo em Inglês | MEDLINE | ID: mdl-31128553

RESUMO

Occurrence of pharmaceutical residues in drinking water has been widely reported in countries that have registered steady economic growth. This can exert concerns among the general consumers, prompting them to explore the potential human health risks associated with continuous exposure to pharmaceuticals. However, such an occurrence is rarely reported in developing or under-developed countries. To give more contexts, this study looked at the presence of nine pharmaceutical residues in drinking water (amoxicillin, caffeine, chloramphenicol, ciprofloxacin, dexamethasone, diclofenac, nitrofurazone, sulfamethoxazole, and triclosan) at Putrajaya residential area in Malaysia. Additionally, the potential health risks associated with contaminated drinking water were investigated. This study has found the presence of pharmaceutical residue concentrations up to 0.38 ng/L, with the highest concentration of caffeine (0.38 ng/L) and the lowest concentration of diclofenac (0.14 ng/L). In comparison, all the nine pharmaceutical residues were substantially lower than previously reported studies. In general, Hazard Quotient (HQ) values indicated that low potential health hazards were present for all age groups. Nevertheless, quantitative occurrences of pharmaceutical residues in drinking water will help guide future toxicological studies to examine other chronic effects, while canvassing for proper framework to look into the water risk management and regulation in Malaysia.


Assuntos
Água Potável/química , Resíduos de Drogas/toxicidade , Poluentes Químicos da Água/toxicidade , Adolescente , Adulto , Idoso , Criança , Pré-Escolar , Resíduos de Drogas/análise , Monitoramento Ambiental , Humanos , Lactente , Malásia , Pessoa de Meia-Idade , Medição de Risco , Poluentes Químicos da Água/análise , Adulto Jovem
19.
Artigo em Inglês | MEDLINE | ID: mdl-31084473

RESUMO

The available information on drug residue stability in chicken egg is scarce. The objective of this study was to evaluate the stability of drug residues in egg under different traditional cooking procedures. Fresh eggs were spiked with different drug concentrations of albendazole (ABZ) and its albendazole sulphoxide (ABZSO) and albendazole sulphone (ABZSO2) metabolites; flubendazole (FLBZ) and its reduced flubendazole (R-FLBZ) and hydrolyzed flubendazole (H-FLBZ) metabolites; amoxicillin (AMX); and enrofloxacin (EFX) and its ciprofloxacin (CFX) metabolite. The egg samples were cooked in different ways, namely, boiling, microwaving, and omelette making. Drug residue concentrations in egg were quantified by HPLC with UV or fluorescence detectors. ABZ and ABZSO concentrations in egg were not affected by boiling and microwaving, while the omelette processing significantly reduced these molecules. Residues of ABZSO2 in egg were stable or increased after all cooking procedures. In contrast, FLBZ and its metabolites FLBZ-H and FLBZ-R residues in egg decreased after all treatments. The residue concentration quantified for EFX and CFX did not show significant changes after any cooking method. AMX residues were unstable, with extremely significant drug reduction after all cooking processes. Conventional methods of egg cooking cannot be considered a tool to eliminate all veterinary drug residues.


Assuntos
Galinhas , Culinária , Resíduos de Drogas/análise , Ovos/análise , Drogas Veterinárias/análise , Animais
20.
J Chromatogr B Analyt Technol Biomed Life Sci ; 1118-1119: 203-209, 2019 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-31059927

RESUMO

A convenient, simple, selective and reliable method was established for separating diclazuril enantiomers and detecting their residues in chicken edible tissues by using high-performance liquid chromatography. The potential effects of chiral column, mobile phase and column temperature on chiral separation of racemic diclazuril were evaluated. Average recovery rates of R-diclazuril and S-diclazuril in three spiking levels ranged from 84.3% to 109.5%, and the relative standard deviations were <15.8%. The limits of quantification of two enantiomers were all 25 ng g-1 in all chicken tissues. The method proposed was successfully applied to monitor distributions and residue elimination of diclazuril enantiomers in chicken muscle, liver, kidney and fat following oral administration. There are no obvious differences (p > 0.05) between R-diclazuril and S-diclazuril in the same tissue for each sampling time. The elimination rates in liver were the fastest and the residual time in kidney was the longest. These results can help further evaluate pharmokinetics, pharmodynamics and toxicity of each enantiomer of diclazuril in food-producing animals.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/análise , Carne/análise , Nitrilos/análise , Triazinas/análise , Animais , Galinhas , Resíduos de Drogas/química , Resíduos de Drogas/farmacocinética , Limite de Detecção , Modelos Lineares , Nitrilos/química , Nitrilos/farmacocinética , Reprodutibilidade dos Testes , Estereoisomerismo , Distribuição Tecidual , Triazinas/química , Triazinas/farmacocinética
SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA