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1.
J Chromatogr A ; 1676: 463257, 2022 Aug 02.
Artigo em Inglês | MEDLINE | ID: mdl-35779392

RESUMO

Modified QuEChERS and triple quadrupole mass spectrometry (LC and GC-MS/MS) technology were used to sequentially analyze pesticides, veterinary drugs, and mycotoxins in feed. In order to analyze the harmful substances that may remain or occur in the feed, we performed optimization experiments for sample preparation and LC-MS/MS and GC-MS/MS conditions. Optimized sample preparation involves extracting 5 g of sample with 15 mL of 0.25 M EDTA and 10 mL of acetonitrile. And some extracts were diluted 10-fold with 100 mM ammonium formate aqueous solution and analyzed by LC-MS/MS, and some extracts were purified through 25 mg PSA and analyzed by GC-MS/MS by adding an analyte protectant. We confirmed the matrix effect of feed ingredients and compound feeds, and added a dilution process after extraction to increase on-site efficiency. Matrix-matched calibration was applied for quantification. Method validation was performed for 197 pesticides, 56 components for veterinary drugs, and 5 components for toxins. All the components showed good linearity (r2 ≥ 0.98) in the developed analytical method. For most compounds, the limit of quantitation was 0.05 mg/kg. The recovery rate experiment was repeated three times at three concentrations including LOQ in feed ingredient, compound feed for livestock, and compound feed for pets. The recovery rate was 70.09-119.76% and relative standard deviations were ≤ 18.91%. And the accuracy and precision were further verified through cross-validation between laboratories. The developed analytical method was used to monitor 414 domestically distributed and imported feeds.


Assuntos
Micotoxinas , Resíduos de Praguicidas , Praguicidas , Drogas Veterinárias , Cromatografia Líquida/métodos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Micotoxinas/análise , Resíduos de Praguicidas/análise , Praguicidas/análise , Extratos Vegetais/análise , Espectrometria de Massas em Tandem/métodos , Drogas Veterinárias/análise
2.
Artigo em Inglês | MEDLINE | ID: mdl-35081327

RESUMO

Diverse food safety programmes around the world are designed to help ensure production of safe food. To meet this need, the development and implementation of more efficient and effective analytical methods to monitor residues (pesticides and veterinary drugs) and contaminants in food is important. In this study, we report the validation results for a simple high-throughput mega-method for residual analysis of 213 pesticides and veterinary drugs, including 15 metabolites, plus 12 environmental contaminants (polychlorinated biphenyls) in tilapia muscle for implementation in routine laboratory analyses. The generic sample preparation method and analytical approach are known as QuEChERSER (more than QuEChERS). A small portion of the initial extract (204 µL) is taken for analysis by ultrahigh-performance liquid chromatography (UHPLC) tandem mass spectrometry (MS/MS) covering 145 analytes, and the remaining extract undergoes a salting out step followed by an automated robotic instrument top sample preparation (ITSP) cleanup, also known as micro-solid-phase extraction (µSPE), plus fast low-pressure gas chromatography LPGC-MS/MS for 134 analytes (66 pesticides are targeted in both UHPLC-MS/MS and LPGC-MS/MS). The mega-method was validated in spiked tilapia samples at 5, 10, 15, and 20 ng/g with 10 replicates per level over two days (n = 80 overall), and 70-140% recoveries with RSDs ≤20% were achieved for 92% of the analytes in LC and 82% in GC. No significant matrix effects were observed for the analytes in LPGC-MS/MS, and only 5% of the analytes exceeded ±20% matrix effect in UHPLC-MS/MS. Analysis of standard reference materials (NIST SRMs 1946 and 1947) for contaminants in freeze-dried fish showed acceptable results, further demonstrating that the QuEChERSER mega-method can be implemented to expand analytical scope and increase laboratory efficiency compared to the QuEChERS method.


Assuntos
Ciclídeos , Poluentes Ambientais , Resíduos de Praguicidas , Praguicidas , Tilápia , Drogas Veterinárias , Animais , Poluentes Ambientais/análise , Resíduos de Praguicidas/análise , Praguicidas/análise , Extratos Vegetais/análise , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos , Drogas Veterinárias/análise
3.
Artigo em Inglês | MEDLINE | ID: mdl-34854800

RESUMO

Monitoring strategies for veterinary drugs in products of animal origin are shifting towards a more risk-based approach. Such strategies not only target a limited number of predefined .substances but also facilitate detection of unexpected substances. By combining the use of archive matrices such as feather meal with suspect-screening methods, early detection of new hazards in the food and feed industry can be achieved. Effective application of such strategies is hampered by complex data interpretation and therefore, targeted data analysis is commonly applied. In this study, the performance of a suspect-screening data processing workflow using a suspect list or the online spectral database mzCloudTM was explored to facilitate detection of veterinary drugs in archive matrices. Data evaluation parameters specifically investigated for application of a suspect list were mass tolerance and the addition or omission of retention times. Application of a mass tolerance of 1.5 ppm leads to an increase in the number of false positives, as does omission of retention times in the suspect list. Different acquisition modes yielding different qualities of MS2 data were studied and proved to be a critical factor, where data-dependent acquisition is preferred when matching to the mzCloudTM database. Using this approach, it is possible to search for compounds on a dedicated suspect list based on the exact mass and retention times and, at the same time, detect unexpected compounds without a priori information. A pilot study was conducted and fourteen different antibiotics were detected (and confirmed by MS/MS). Three of these antibiotics were not included in the suspect list. The optimised suspect-screening method proved to be fit for the purpose of finding veterinary drugs in feather meal, which are not in the scope of the current monitoring methods and therefore, it gives added value in the perspective of a risk-based monitoring.


Assuntos
Drogas Veterinárias/análise , Animais , Cromatografia Líquida , Avaliação Pré-Clínica de Medicamentos , Espectrometria de Massas
4.
São Paulo; s.n; s.n; 2022. 166 p. tab, graf, ilus.
Tese em Português | LILACS | ID: biblio-1416533

RESUMO

O organogel é formado por uma matriz tridimensional composta de filamentos que se auto-organizam em uma rede entrelaçada e que, por seu tipo de estrutura, pode ser utilizado com o objetivo de atuar como um implante que se forma in situ, sendo capaz de se comportar como uma forma farmacêutica de liberação prolongada. Esse trabalho tem, por tanto, o objetivo desse trabalho foi desenvolver, caracterizar, quantificar e traçar perfis de dissolução para formulações de organogel contendo meloxicam como principio ativo. O material está dividido em quatro capítulos, sendo apresentada inicialmente (I) revisão da literatura a respeito da lecitina de origem vegetal, com suas principais fontes de obtenção, como soja, girassol e colza, e também seu uso farmacêutico na obtenção de formulações como organogéis, microemulsões e lipossomas. Os demais capítulos abordam (II) desenvolvimento e otimização de uma formulação de organogel contendo lecitina de soja e Pluronic® F-127 como formadores da matriz tridimensional e meloxicam como principio ativo. (III) Desenvolvimento e validação de um método de quantificação do teor de meloxicam por cromatografia líquida de alta eficiência (CLAE). (IV) Desenvolvimento de um método de dissolução para formulações de organogel, que fosse capaz de ser utilizado na caracterização do perfil de dissolução de diferentes formulações. Com os resultados obtidos, foi possível desenvolver formulações de organogel contendo lecitina de soja, Pluronic® F-127 e meloxicam, assim como um método analítico validado para as analises de teor. Por fim, foram obtidos também os perfis de dissolução de duas formulações mais promissoras


Organogels are formed by a three-dimensional matrix composed of filaments that selforganize in an interlaced network and that, due to its type of structure, can be used with the objective of acting as an implant that forms in situ, being able to behave as an extendedrelease dosage form. This work has, therefore, the objective of this work was to develop, characterize, quantify and trace dissolution profiles for organogel formulations containing meloxicam as active ingredient. The material is divided into four chapters, initially presented (I) review of the literature on lecithin of plant origin, with its main sources of production, such as soybean, sunflower and rapeseed, and also its pharmaceutical use in obtaining formulations such as organogels , microemulsions and liposomes. The remaining chapters address (II) development and optimization of an organogel formulation containing soy lecithin and Pluronic® F-127 as three-dimensional matrix formers and meloxicam as an active ingredient. (III) Development and validation of a method for quantification of meloxicam content by high performance liquid chromatography (HPLC). (IV) Development of a dissolution method for organogel formulations, capable of being used to characterize the dissolution profile of different formulations. With the results obtained, it was possible to develop organogel formulations containing soy lecithin, Pluronic® F-127 and meloxicam, as well as a validated analytical method for content analysis. Finally, the dissolution profiles of two more promising formulations were also obtained


Assuntos
Preparações Farmacêuticas/análise , Médicos Veterinários , Drogas Veterinárias/análise , Poloxâmero/análise , Dissolução , Lecitinas/análise , Meloxicam/antagonistas & inibidores , Farmacêuticos/classificação , Química Farmacêutica/instrumentação , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida/métodos , Formas de Dosagem , Métodos
5.
J AOAC Int ; 103(2): 584-606, 2020 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-33241275

RESUMO

BACKGROUND: Validated analytical methods are needed to conduct regulatory monitoring of ready-to-eat meats and fish for food safety, risk assessment, and other purposes. The methods should be cost-effective, high-throughput, and meet acceptable performance standards for a wide scope of drugs and matrixes. OBJECTIVE: The goal of this study was to demonstrate the validity for possible implementation in the US National Residue Program of an efficient method for qualitative and quantitative analysis of 176 targeted drugs at levels as low as 10 ng/g in hot dogs, catfish and swai (Siluriformes), chicken tenders, fried bacon, and sausage using ultrahigh-performance liquid chromatography - tandem mass spectrometry (UHPLC-MS/MS). METHODS: Sample preparation simply involved a 5 min extraction by shaking 2 g comminuted samples with 10 mL of 4/1 (v/v) acetonitrile/water followed by centrifugation and UHPLC-MS/MS analysis of 2 µL injections. For cleanup comparison purposes only, sausage extracts were also prepared using a cartridge-based EMR-Lipid method prior to analysis. RESULTS: Acceptable validation of 70-120% recoveries with <25% RSDs was met for 156-176 out of 186 drugs and quality control analytes without cleanup depending on the matrix. The EMR-Lipid method for sausage improved results for some analytes, such as mectin anthelmintics, due to reduction of indirectly interfering fats in the final extracts, but it also led to significantly worse results for several other drugs, resulting in 32 fewer analytes meeting the given validation criteria than without cleanup. CONCLUSIONS: The simple, high-throughput method was demonstrated to be valid to meet routine regulatory and other monitoring needs for many diverse targeted drugs in fish and ready-to-eat meat matrixes.


Assuntos
Peixes-Gato , Resíduos de Drogas , Produtos da Carne , Drogas Veterinárias , Animais , Cromatografia Líquida de Alta Pressão , Resíduos de Drogas/análise , Carne/análise , Extratos Vegetais , Espectrometria de Massas em Tandem , Drogas Veterinárias/análise
6.
Anal Bioanal Chem ; 412(17): 3975-3982, 2020 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-32372275

RESUMO

In vivo, drug molecules interact with their biological targets (e.g., enzymes, receptors, ion channels, transporters), thereby eliciting therapeutic effects. Assays that measure the interaction between drugs and bio-targets may be used as drug biosensors, which are capable of broadly detecting entire drug classes without prior knowledge of their chemical structure. This Trends article covers recent developments in bio-target-based screening assays for detecting drugs associated with the following areas: illicit products marketed as dietary supplements, food-producing animals, and bodily fluids. General challenges and considerations associated with using bio-target assays are also presented. Finally, future applications of these assays for drug detection are suggested based upon current needs.


Assuntos
Técnicas Biossensoriais/métodos , Suplementos Nutricionais/análise , Drogas Ilícitas/análise , Preparações Farmacêuticas/análise , Animais , Técnicas Biossensoriais/instrumentação , Análise de Alimentos/instrumentação , Análise de Alimentos/métodos , Humanos , Detecção do Abuso de Substâncias/instrumentação , Detecção do Abuso de Substâncias/métodos , Drogas Veterinárias/análise
7.
Ecotoxicol Environ Saf ; 165: 376-385, 2018 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-30216896

RESUMO

Residue of veterinary antibiotics (VAs) in the animal breeding industry has become a problematic environmental issue. However, the residual levels of VAs as well as their variation tendency, degradation mechanisms and relationships with other parameters during animal wastewater disposal processes are still obscure. This study measured different samples during wastewater disposal processes from three farms, and systematically analyzed the residue, migration and removal of 58 kinds of typical VAs (6 classes) in Tianjin, China. The results showed that about 44 kinds of VAs were quantitatively detected. Tetracycline antibiotics (TCs) usually had higher residual concentrations than other classes of VAs in the raw wastewater; the highest residual concentration was 130.67 ±â€¯5.90 µg/L which occurred for chlortetracycline (CTC). Pig farms generally had more VAs species and higher residual concentrations than dairy farms, and the proportion of different VAs was similar for dairy farms. The final removal rates of different VAs classes varied largely (negative to > 99.87%), and the highest removal rates usually occurred in biological processes for adsorption and biodegradation effects, and occasionally occurred in the final effluents. The correlation coefficients between VAs removal rates and chemical oxygen demand (COD) removal rates were much higher than those of total nitrogen (TN), total phosphorus (TP) and ammonia nitrogen (NH4-N) in pig farms, while opposite conclusion was obtained in dairy farms. Among different classes, TCs presented the highest daily mass loading of ND ~ 10,453.8 ±â€¯471.7 mg/d in the influent and ND ~ 1141.6 ±â€¯58.9 mg/d in the effluent in farm 1.


Assuntos
Antibacterianos/análise , Águas Residuárias/química , Poluentes Químicos da Água/análise , Criação de Animais Domésticos , Animais , Biodegradação Ambiental , Análise da Demanda Biológica de Oxigênio , Bovinos , China , Indústria de Laticínios , Nitrogênio/análise , Fósforo/análise , Suínos , Drogas Veterinárias/análise , Eliminação de Resíduos Líquidos/métodos
8.
Artigo em Inglês | MEDLINE | ID: mdl-29377759

RESUMO

A study on stability of veterinary drugs in standard solutions stored at -80°C and at -20°C was conducted over 1 year. Data were acquired on 152 individual stock standard solutions and also on 15 family mixes and 2 working standard solutions. All solutions were prepared, stored and compared 1 year later against freshly prepared ones by LC-MS/MS. A statistical analysis was performed to set the acceptability criteria, taking into account the variability of standard preparations. In individual stock standard solutions stored at -80°C (12 months) and -20°C (9 months), stability was demonstrated for 141 and 140 out of 152 compounds, i.e. for 92% and 93% of compounds, respectively. Drugs were even more stable when solubilised in either diluted family mixes or working standard solutions, with more than 99% and 94% of compounds found unaltered when stored at -80°C and at -20°C, respectively. In mixes, beta-lactams from the cephalosporin (cefadroxil and cephalexin) and penicillin (amoxicillin and ampicillin) families were found to be the least stable compounds when stored at -20°C (6 months), necessitating storage at -80°C to achieve a 1-year shelf life. The study also evidenced solubility issues for two sulfonamides (sulfadiazine and sulfamerazine) in methanol-based solutions. An independent stability study conducted by a second laboratory confirmed the 1-year stability of 3 family mixes-quinolones, sulfonamides and tetracyclines.


Assuntos
Análise de Alimentos , Contaminação de Alimentos/análise , Drogas Veterinárias/análise , Drogas Veterinárias/química , Cromatografia Líquida , Avaliação Pré-Clínica de Medicamentos , Estabilidade de Medicamentos , Soluções/normas , Espectrometria de Massas em Tandem , Temperatura
9.
Artigo em Inglês | MEDLINE | ID: mdl-27189753

RESUMO

A ranking system for veterinary medicinal products and coccidiostat feed additives has been developed as a tool to be applied in a risk-based approach to the residue testing programme for foods of animal origin in the Irish National Residue Control Plan (NRCP). Three characteristics of substances that may occur as residues in food are included in the developed risk ranking system: Potency, as measured by the acceptable daily intake assigned by the European Medicines Agency Committee for Medicinal Products for Veterinary Use, to each substance; Usage, as measured by the three factors of Number of Doses, use on Individual animals or for Group treatment, and Withdrawal Period; and Residue Occurrence, as measured by the number of Non-Compliant Samples in the NRCP. For both Number of Doses and Non-Compliant Samples, data for the 5-year period 2008-12 have been used. The risk ranking system for substances was developed for beef cattle, sheep and goats, pigs, chickens and dairy cattle using a scoring system applied to the various parameters described above to give an overall score based on the following equation: Potency × Usage (Number of Doses + Individual/Group Use + Withdrawal Period) × Residue Occurrence. Applying this risk ranking system, the following substances are ranked very highly: antimicrobials such as amoxicillin (for all species except pigs), marbofloxacillin (for beef cattle), oxytetracycline (for all species except chickens), sulfadiazine with trimethoprim (for pigs and chickens) and tilmicosin (for chickens); antiparasitic drugs, such as the benzimidazoles triclabendazole (for beef and dairy cattle), fenbendazole/oxfendazole (for sheep/goats and dairy cattle) and albendazole (for dairy cattle), the avermectin ivermectin (for beef cattle), and anti-fluke drugs closantel and rafoxanide (for sheep/goats); the anticoccidials monensin, narasin, nicarbazin and toltrazuril (for chickens). The risk ranking system described is a relatively simple system designed to provide a reliable basis for selecting the veterinary medicinal products and coccidiostat feed additives that might be prioritised for residue testing.


Assuntos
Suplementos Nutricionais/análise , Resíduos de Drogas/análise , Carne/análise , Nível de Efeito Adverso não Observado , Drogas Veterinárias/análise , Ração Animal/análise , Animais , Anti-Helmínticos/análise , Antibacterianos/análise , Antifúngicos/análise , Antiprotozoários/análise , Bovinos , Galinhas , Coccidiostáticos/análise , União Europeia , Inocuidade dos Alimentos , Cabras , Medição de Risco , Ovinos , Suínos
10.
J Pharm Biomed Anal ; 106: 136-43, 2015 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-25483174

RESUMO

As annual sales of antibiotics continue to rise, the mass of these specially-designed compounds entering municipal wastewater treatment systems has also increased. Of primary concern here is that antibiotics can inhibit growth of specific microorganisms in biological processes of wastewater treatment plants (WWTPs) or in downstream ecosystems. Growth inhibition studies with Escherichia coli demonstrated that solutions containing 1-10 µg/L of fluoroquinolones can inhibit microbial growth. Wastewater samples were collected on a monthly basis from various treatment stages of a 30 million gallon per day WWTP in Maryland, USA. Samples were analyzed for the presence of 11 fluoroquinolone antibiotics. At least one fluoroquinolone was detected in every sample. Ofloxacin and ciprofloxacin exhibited detection frequencies of 100% and 98%, respectively, across all sampling sites. Concentrations of fluoroquinolones in raw wastewater were as high as 1900 ng/L for ciprofloxacin and 600 ng/L for ofloxacin. Difloxacin, enrofloxacin, fleroxacin, moxifloxacin, norfloxacin, and orbifloxacin were also detected at appreciable concentrations of 9-170 ng/L. The total mass concentration of fluoroquinolones in raw wastewater was in the range that inhibited E. coli growth, suggesting that concerns over antibiotic presence in wastewater and wastewater-impacted surface water are valid. The average removal efficiency of fluoroquinolones during wastewater treatment was approximately 65%; furthermore, the removal efficiency for fluoroquinolones was found to be negatively correlated to biochemical oxygen demand removal and positively correlated to phosphorus removal.


Assuntos
Antibacterianos/análise , Escherichia coli/efeitos dos fármacos , Fluoroquinolonas/análise , Águas Residuárias/análise , Animais , Antibacterianos/administração & dosagem , Antibacterianos/farmacologia , Análise da Demanda Biológica de Oxigênio , Relação Dose-Resposta a Droga , Fluoroquinolonas/administração & dosagem , Fluoroquinolonas/farmacologia , Humanos , Fósforo/química , Drogas Veterinárias/administração & dosagem , Drogas Veterinárias/análise , Drogas Veterinárias/farmacologia , Poluentes Químicos da Água/análise , Purificação da Água/métodos
11.
Artigo em Inglês | MEDLINE | ID: mdl-25371582

RESUMO

BACKGROUND: A survey relative to the use of plants for the cure of animals in Tunisia was conducted in order to make a comparison with the same species (or similar ones) in central and southern Italy. MATERIALS AND METHODS: available bibliographical data both for Italy and for Tunisia were consulted. RESULTS: Thirty-nine plants, representing 22 families, used in Tunisia in ethnoveterinary medicine were reported, and comparisons made with close species used in Central and Southern Italy. Seven of the 39 species (about the 18% of the total) are not present in Italian flora. Fourteen of the 39 species (35% of the total) are also used in Italy. Camelidae (dromedaries and camels) are the most valuable types of domestic animals cured in Tunisia, but ovines, horses, bulls, dogs are also treated. Some uses coincide with those existing in different Italian regions. The plants used are the most common and most easily found in these areas. CONCLUSION: The present study confirms the convergence in ethnoveterinary medicine between Tunisia and Italy, even if it appears less significant than in human ethnobotany. Further studies are required in areas of Tunisia that have not yet been studied, in order to get the possibility of an evaluation of active compounds.


Assuntos
Doenças dos Animais/tratamento farmacológico , Extratos Vegetais/uso terapêutico , Plantas Medicinais/classificação , Drogas Veterinárias/uso terapêutico , Animais , Animais Domésticos , Bovinos , Bases de Dados Factuais , Cães , Etnobotânica , Cavalos , Itália , Extratos Vegetais/análise , Plantas Medicinais/química , Tunísia , Drogas Veterinárias/análise , Medicina Veterinária
12.
Huan Jing Ke Xue ; 35(7): 2650-7, 2014 Jul.
Artigo em Chinês | MEDLINE | ID: mdl-25244851

RESUMO

Pollution characteristics of digested piggery wastewater (DPW), including not only the chemical oxygen demand (COD), nitrogen and phosphorus but also the veterinary antibiotics and heavy metals, were investigated in ten large-scale pig farms in Jiaxing City. Results showed that the water quality of DPW greatly varied with farms and seasons. DPW in the spring group showed the highest pollutant concentration, with seven of the ten pig farms demonstrating COD of over 2 000 mg x L(-1), total nitrogen and ammonia nitrogen of over 1 000 mg x L(-1) and total phosphorus of over 60 mg x L(-1). Pollutant concentrations of DPW were lower in the autumn and winter groups, while the lowest was observed in the summer group. Unbalanced nutrient was observed in DPW, the carbon nitrogen ratio showed the lowest value of 0.8-4.3 in the autumn group. Four classes (tetracyclines, quinolones, macrolides and sulfonamides) of ten antibiotics and six heavy metals (Cu, Zn, Pb, Cd, Ni and Cr) were detectable in DPW from all the ten farms. Cu and Zn were the top two dominant heavy metals, with an average concentration of 1.88 mg x L(-1) and 7.63 mg L(-1), respectively. Tetracyclines (including Tetracycline, Oxytetracycline and Chlortetracycline) were always the dominant antibiotics. The total concentration of the ten antibiotics was in the range of 10.1 microg x L(-1) to 1090 microg x L(-1), far exceeding the antibiotics limit of 10 ng x L(-1) in the water environment specified by EU. Efficient but low cost treatment technologies are in urgent need in order to deal with the pollution by DPW, a wastewater that is not only difficult to remove nitrogen and phosphorus, but also seriously polluted by heavy metals and antibiotics.


Assuntos
Agricultura , Suínos , Águas Residuárias/análise , Poluentes Químicos da Água/análise , Animais , Análise da Demanda Biológica de Oxigênio , Carbono/análise , China , Metais Pesados/análise , Nitrogênio/análise , Fósforo/análise , Drogas Veterinárias/análise
13.
J Small Anim Pract ; 55(9): 447-50, 2014 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-25040219

RESUMO

OBJECTIVES: To measure the percentage of the stated amount of S-adenosyl methionine present in a range of commercially available S-adenosyl methionine supplements for veterinary use. METHOD: Sixty-four samples of products containing S-adenosyl methionine marketed to support liver function were obtained from five manufacturers via three commercial wholesalers. The amount of S-adenosyl methionine in each product was measured using high-pressure liquid chromatography. RESULTS: There were greater than threefold variation in the percentage of measured S-adenosyl methionine compared to the stated amount on the packaging which was significantly (P < 0 · 001) related to the product group being measured. CLINICAL SIGNIFICANCE: Differences in received dose of S-adenosyl methionine between different products were marked and this could have a profound influence on studies that evaluate any variation in absorption of S-adenosyl methionine between different product formulations, the effectiveness of S-adenosyl methionine-based products in clinical cases or when translating the results of studies that have used a specific S-adenosyl methionine product to those produced by a different manufacturer.


Assuntos
Suplementos Nutricionais/análise , S-Adenosilmetionina/análise , Animais , Química Farmacêutica , Cromatografia Líquida de Alta Pressão/veterinária , Drogas Veterinárias/análise , Drogas Veterinárias/normas
14.
Bioanalysis ; 1(8): 1475-89, 2009 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-21083096

RESUMO

Anabolic steroids are the main abused class of prohibited substances in doping control. These steroids are associated with enhancement of muscular mass and aggressiveness, resulting in increased performance. Chromatography and MS have a key role among methods developed to detect anabolic steroids in doping control laboratories. However, the classical analytical approach fails in detection of the so-called 'designer steroids'. This review focuses on the rise of tetrahydrogestrinone, a drug that became synonymous with designer steroids. The reasons why classical methods fail in tetrahydrogestrinone detection are discussed and how the detection was implemented is shown. Alternative strategies for detection of new drugs designed to cheat current analytical methodology are highlighted. Concern for the abuse of veterinary designer drugs and supplements is also acknowledged.


Assuntos
Anabolizantes/análise , Drogas Desenhadas/análise , Gestrinone/análogos & derivados , Detecção do Abuso de Substâncias/métodos , Drogas Veterinárias/análise , Técnicas de Química Analítica/métodos , Suplementos Nutricionais/análise , Dopagem Esportivo , Gestrinone/análise , Humanos
15.
Equine Vet J ; 36(2): 113-7, 2004 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-15038432

RESUMO

REASONS FOR PERFORMING STUDY: Analysis of human hair for drug residues is being used increasingly as a diagnostic tool in the investigation of drug use and abuse. Hair analysis is complementary to urine/blood testing in that it can provide an extensive historical record of drug use, is noninvasive, impersonal and can facilitate retesting. However, the technique has not been studied in horses. HYPOTHESIS: That the systemic administration of drugs in horses could be identified by the detection of drug residues in hair. OBJECTIVE: To evaluate hair analysis as a potential retrospective diagnostic test for drug administration in horses by studying the deposition of systemically administered drugs in tail hair. METHODS: Tail hairs (n = 40-50) from 4 horses with known drug histories were washed, chopped into 3-5 mm fragments and extracted overnight, in 0.1 mol/l hydrochloric acid, prior to solid-phase extraction and analysis by high-performance liquid chromatography. Horse 1, a 3-year-old Thoroughbred colt (gastric ulcer), was treated for 14 days with omeprazole; Horse 2, a 3-year-old Thoroughbred colt (anaerobic infection), was treated for 5 days with metronidazole; Horse 3, an 8-year-old Thoroughbred gelding (sinusitis), was treated for 10 days with trimethoprim/sulphadiazine; and Horse 4, a 3-year-old Thoroughbred colt (respiratory infection), was treated for 5 days with procaine benzylpenicillin. RESULTS: Omeprazole was not detected in tail hair. Metronidazole was detected in tail hair at a concentration of 0.57 ng/mg, trimethoprim and sulphadiazine at concentrations of 9.14 and 2.26 ng/mg, respectively, and procaine at a concentration of 1.66 ng/mg. CONCLUSIONS: The data presented suggest that hair analysis may become a useable technique for the retrospective detection of drug administration in horses. POTENTIAL RELEVANCE: This technique could ultimately be used as part of a prepurchase veterinary examination to identify misuse of anti-inflammatory and sedative drugs, in an in-training testing programme to identify use of anabolic agents, or to provide evidence to support post race blood or urine test results. Clearly, more extensive research will be required to evaluate the effectiveness of the technique over a much broader range of drugs.


Assuntos
Resíduos de Drogas/análise , Cabelo/química , Cavalos/metabolismo , Detecção do Abuso de Substâncias/veterinária , Drogas Veterinárias/análise , Animais , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida de Alta Pressão/veterinária , Relação Dose-Resposta a Droga , Masculino , Metronidazol/análise , Omeprazol/análise , Projetos Piloto , Procaína/análise , Detecção do Abuso de Substâncias/métodos , Sulfadiazina/análise , Trimetoprima/análise , Drogas Veterinárias/administração & dosagem , Drogas Veterinárias/metabolismo
16.
Ecotoxicol Environ Saf ; 48(3): 311-20, 2001 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-11222042

RESUMO

The use of veterinary drugs (primarily antibiotics) in animal husbandry harbors the risk that these compounds end up in the farmland when manure is used as fertilizer. The biodegradability of three compounds, olaquindox (OLA), metronidazole (MET), and tylosin (TYL), was simulated in soil--manure slurries with 50 g of soil per liter. Supplemental batch sorption tests revealed that insignificant amounts of OLA and MET were located in the soil phase, whereas only 0.1 to 10% of the added amounts of TYL remained in the liquid phase. This may reduce the bioavailability and thus biodegradation rates of TYL. Unidentified metabolites of OLA and TYL and four known TYL metabolites were detected using HPLC. However, none of these substances were seen to persist in the biodegradation experiments, indicating that OLA and TYL most likely were mineralized in the experiments. Neither the use of sandy or clayey soil nor the use of 0, 1, or 10% (V/V) of manure added to these soils had a significant effect on the degradation rates. Degradation half-lives for the primary degradation were 3.3--8.1 days for TYL, 5.8--8.8 days for OLA, and 13.1--26.9 days for MET. Based on comparisons of results obtained with the benchmark chemical aniline and degradation half-lives of this compound in nature, it was assessed that results obtained with the current test method slightly overestimate real-world biodegradation rates.


Assuntos
Antibacterianos/metabolismo , Metronidazol/metabolismo , Quinoxalinas/metabolismo , Poluentes do Solo/metabolismo , Tilosina/metabolismo , Drogas Veterinárias/metabolismo , Aerobiose , Antibacterianos/análise , Biodegradação Ambiental , Esterco/análise , Metronidazol/análise , Quinoxalinas/análise , Solo/análise , Poluentes do Solo/análise , Drogas Veterinárias/análise
17.
J Chromatogr Sci ; 35(1): 38-42, 1997 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-8989871

RESUMO

This paper describes a general screening method for the determination of anabolic steroids in oil-based injectables, water suspensions, dietary supplements, and herbal drugs marketed in the form of capsules or tablets. The compounds are extracted into methanol, separated on a reversed-phase column with an acetonitrile-water gradient, and detected by using an ultraviolet visible (UV-vis) photodiode array detector and a particle beam mass spectrometric detector coupled in series. Identification is based on retention time, UV-vis spectra, and mass spectra. Mass spectral confirmation is accomplished by matching with a standard when available and by comparison with an electron impact mass spectra library that is either commercially available or generated in our laboratory. The tandem arrangement of the detectors provides qualitative and quantitative information from a single experiment by fully utilizing the inherent advantages associated with each detector. This method is applicable to all the anabolic steroids encountered in this laboratory so far.


Assuntos
Anabolizantes/análise , Cromatografia Líquida de Alta Pressão/métodos , Anabolizantes/química , Espectrometria de Massas , Espectrofotometria , Espectrofotometria Ultravioleta , Testosterona/análise , Testosterona/química , Drogas Veterinárias/análise , Drogas Veterinárias/química
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