Analytical And Regulatory Aspects For Determination Of Macrolide Residues In Animal-derived Foods By Liquid Chromatography Associated With Mass Spectrometry [aspectos AnalÍticos E RegulatÓrios Na DeterminaÇ Ão De ResÍduos De MacrolÍdeos Em Alimentos De Origem Animal Por Cromatografia LÍquida Associada À Espectrometria De Massas]

This is an overview of LC-MS techniques applied for macrolide determination in food, including sample preparation and method validation, as well as the policies adopted by international agencies regarding their presence in food. Techniques for the analysis of macrolides in food normally include solid phase or liquid-liquid extraction followed by HPLC. UHPLC presents advantages in running time, detectability and solvent consumption. Triple-quadrupoles are the most common analyzers in instruments used for the determination of contaminants in food, but time-of-flight and ion-trap spectrometers have been successfully applied for analyses focusing on the investigation of structural formula or the presence of degradation products.363449461Horie, M., (1995) Chemical Analysis for Antibiotics Used in Agriculture, , Oka, H.Nakazawa, H.Harada, K.MacNeil, J. D., eds.AOAC International: Arlington, chap. 6Gustafson, R.H., Bowen, R.E., (1997) J. Appl. 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Chem, 74, p. 835Agência Nacional de Vigilância Sanitária, Ministério da Saúde, BrasilRE No 899, de 29/05/2003, Diário Oficial da União de 02/05/2003Instituto Nacional De Metrologia Normalização e Qualidade Industrial (INMETRO)DOQ-CGCRE-008, 2003Ministério da Agricultura, Pecuária e Abastecimento, BrasilDiário Oficial da União de 22/07/2009, Seção 1, Página 7(1999) ISO/EC 17025, , International Standard Organization;(1996) Validation of Analytical Procedures: Methodology, Q2B, Step 4, Consensus Guideline, , International Conference on HarmonizationNovember(2002) Off. J. Eur. 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Validation Of Chromatographic Methods For The Determination Of Residues Of Veterinary Drugs In Foods [validação De Métodos Cromatográficos Para A Determinação De Resíduos De Medicamentos Veterinários Em Alimentos]

Different agencies that supply validation guidelines worldwide establish almost the same parameters to be evaluated in the validation process of bioanalytical methods. However, they recommend different procedures, as well as establish different acceptance criteria. The present review delineates and discusses the stages involved in the validation procedures of bioanalytical methods designed for determining veterinary residues in food, explaining the main differences in the guidelines established for this purpose by the main regulatory agencies in the world.31511901198http://www.who.int/foodsafety/en/, acessada em Março 2007http://www. anvisa.gov.br, acessada em Janeiro 2007http://www. inmetro.gov.br, acessada em Janeiro 2007Agência Nacional de Vigilância Sanitária (ANVISA)Guia para Validação de Métodos Analíticos e Bioanalíticos, RE no 899, de 29/05/2003Normalização e Qualidade Industrial (INMETRO)(2003) Orientações sobre Validação de Métodos de Ensaios Químicos, DOQ-CGCRE-008, , Instituto Nacional de Metrologiahttp://goldbook.iupac.org/R05305.html, acessada em Janeiro 2007(1999) General Requirements for the Competence of Testing and Calibration Laboratories, , http://www.ich.org, International Standard Organization;, ISO/EC 17025, 8, acessada em Janeiro(1993) Guide to the Expression of Uncertainty in Measurements, , International Standard Organization ISO, Geneva(1995) Quantifying Uncertainty in Analytical Measurement, , EURACHEM;, Londonhttp://jecfa.ilsi.org/section1.htm#1, acessada em Abril 2007European CommissionOfficial Journal of the European Communities, 17/08/2002, L221/8-36International Conference on Harmonization (ICH)Validation of Analytical Procedures: Methodology, Q2B, Step 4, Consensus Guideline, 6 November 1996(2004) US Pharmacopeia 27, , United States Pharmacopeia (USP) Convention;, RockvilleCollins, C.H., Braga, G.L., Bonato, P.S., (2005) Fundamentos de Cromatografia, , Editora UNICAMP: CampinasCenter for Drug Evaluation and Research, Center for Veterinary Medicine, Department of Health and Human Services (2001) Guidance for Industry, Bioananalytical Method Validation, , United States Food and Drug Administration US-FDA, MayThompson, M., Stephen, L.R., Wood, R., (2002) Pure Appl. Chem, 74, p. 835(1997) Validation of Analytical Methods for Food Control, , Food and Agriculture Organization of the United Nations FAO, DecemberHuber, L., (1998) LC-GC Int, 11, p. 96Rogatsky, E., Stein, S., (2005) J. Am. Soc. Mass Spectrom, 16, p. 1757Thompson, M., Ellison, S.R., Wood, R., (2006) Pure Appl. Chem, 78, p. 145http://www.inmetro.gov.br/kits/ctle05_protocolo.pdf, acessada em Março 2007Miller, J.C., Miller, J.N., (1993) Statistics for Analytical Chemistry, , Ellis HorwoodNew Yor

A Fast Immunoassay For The Screening Of Alfa-trenbolone In Bovine Urine [um Imunoensaio Rápido Para A Detecção De Alfa-trembolona Em Urina Bovina]

Brazil is one of the many countries that forbids the use of anabolic compounds, which generates difficulties on monitoring its use, once it has one of the biggest cattle herd. Therefore, several anabolic compounds are used, including trenbolone acetate. With the agreement of "Ministério da Agricultura, Pecuária e Abastecimento", an ELISA based test was done with the production of polyclonal antibodies in rabbits and testing in steers urine which received trenbolone acetate implants. The test showed to be cheap, easy and reliable to use in bovine urine to determine alfa- trenbolone, trenbolone acetate major metabolite, released in the animals urine until 60 days after implant was been injected. The results in comparison to the ones obtained by the commercial kit used by the Brazilian "Ministério da Agricultura, Pecuária e Abastecimento" were similar, with no significant differences.43SUPPL7479Boots, R., Anderson, P., Dehaan, K., Growth stimulants: Compounds, concentrations, combinations and regulations (1997) Proceedings, pp. 10-14. , IMPACT AND CARCASS VALUE OF BEEF CATTLE-SYMPOSIUM, Oklahoma, Oklahoma: [s. n.]Lone, K.P., Natural sex steroids and their xenobiotic analogs in animal production: Growth, carcass quality, pharmacokinetics, metabolism, mode of action, residues, methods and epidemiology (1997) Critical Review in Food Science and Nutrition, 37 (1-2), pp. 93-209Hayden, J.M., Bergen, W.G., Merkel, R.A., Skeletal muscle protein metabolism and serum hormone, insulin and cortisol concentrations in growing steers implanted with estradiol 17b, trenbolone acetate or estradiol-17b plus trenbolone acetate (1992) Journal of Animal Science, 70 (7), pp. 2109-2119Orr, R., (2004) Growth Promoting Hormones in Cattle, , http//www.foodsafetynetwork.ca/animal/growth-hormones-cattle.html, Available, Cited: 13 abrFerrando, R., (2004) Methods of Measuring Hormone Levels in Animal Products, , http://www.fao.org/DOCREP/004/X6533E/X6533E02.htm, Available, Cited: 13 abrPaschoal, J.A.R., (2002) Padronização De Um Ensaio Imunoenzimático (ELISA) a Partir De Anticorpos Policlonais Produzidos Contra Progesterona, , 81 f. Dissertação (Mestrado) - Centro de Energia Nuclear na Agricultura, Universidade de São Paulo, Piracicaba, 2002ELISA - theory and practice (1995) Methods in Molecular Biology, 42, p. 223Baxter, G.A., Specificity enhancement of polyclonal antiserum by the induction of tolerance to una wanted cross-reacting determinants (1996) Food & Agricultural Immunology, 8, pp. 85-95Erlanger, B.F., Steroid-protein conjugates. I.Preparation and characterization of conjugates of bovine serum albumin with testosterone and with cortisone (1957) Journal of Biological Chemistry, 228, pp. 713-727van de Wiel, D.F.M., Koops, W., Development and validation of an enzyme immunoassay for progesterone in bovine milk or blood plasma (1985) Animal Reproduction Science, 10, pp. 201-213Plaizier, J.C.B., Field validation of an EIA kit for progesterone measurement in milk and blood plasma (1993) International Atomic Energy Agency, pp. 157-170. , Improving the productivity of indigenous African livestock, Vienna: IAEA: FAO, IAEATECDOC, 708Dubois, M., GC-MS determination of anabolic steroids after multi-immunoaffinity purification (1998) The Analyst, 123 (12), pp. 2611-2616Yoshioka, N., Akiyama, Y., Takeda, N., Determination of a and b- trenbolone in bovine muscle and liver by liquid chromatography with fluorescence detection (2000) Journal of Chromatography B, 739, pp. 363-367Sterk, S., (1998) Production and Stability Testing of Incurred Reference Materials for the Anabolic Steroid Trenbolone in Bovine Urine, 123 (12), pp. 2563-2566. , The Analys

A Simple Liquid Chromatography Coupled To Quadrupole Time Of Flight Mass Spectrometry Method For Macrolide Determination In Tilapia Fillets

A method for the identification and quantification of macrolides (erythromycin, josamycin, tilmicosin, tylosin, spiramycin and neospiramycin) in tilapia fillets by liquid chromatography coupled to quadrupole time of flight mass (LC-QToF) spectrometry is presented. Sample preparation was quite simple and low cost: proteins were precipitated and the analytes were extracted with ethanol, extract was defatted with hexane and concentrated by solvent evaporation. The matrix effect was statistically demonstrated during method validation, in which matrix-matched calibration was applied. Matrix effect mechanism was clarified thanks to the capability of QToF mass spectrometer of generating full scan spectra with accurate mass measurement. The limits of quantification were at least 45% lower than the maximum residue limits. The method was able to identify the studied macrolides with relative m/z errors lower than 2.5. ppm and to monitor two fragment ions per analyte, which is in accordance with the European Community recommendations for the analysis of contaminants in foods. Samples from the retail market of São Paulo State, Brazil, were analyzed by the developed method and none of them presented positive results for the macrolides studied. © 2014 Elsevier Inc.342153162Barcelo, D., Petrovic, M., Challenges and achievements of LC-MS in environmental analysis: 25 years on (2007) TRAC Trends in Analytical Chemistry, 26, pp. 2-11(2009) Veterinary Drug Residues in Food - Maximum Residue Limits Home Page, Rome, Italy, , http://www.codexalimentarius.net/mrls/vetdrugs/jsp/vetd_q-e.jsp, Retrieved from:(20.06.11), Codex AlimentariusCommission Decision of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results (2002) Official Journal of the European Communities, 221, pp. 8-36. , EC, European Commission(2011) European Medicines Agency. Maximum Residue Limits Reports Home Page, London, England, , http://www.ema.europa.eu/ema/index.jsp?curl=pages/medicines/landing/vet_mrl_search.jsp&murl=menus/regulations/regulations.jsp&mid=WC0b01ac058006488e, Retrieved from:(20.06.11)., EMA(2009) Food and Agriculture Organization of the United Nations, , ftp://ftp.fao.org/docrep/fao/012/i1013t/i1013t.pdf, Fishery and Aquaculture Statistics, Rome, Italy, Retrieved from:(17.11.10), FAO(2010) Food and Agriculture Organization of the United Nations. Cultured Aquatic Species Information Programme - Oreochromis niloticus, , http://www.fao.org/fishery/culturedspecies/Oreochromis_niloticus/en#tcN90112, Retrieved from:(17.11.10), FAOGobel, A., McArdell, C.S., Suter, M.J., Giger, W., Trace determination of macrolide and sulfonamide antimicrobials, a human sulfonamidemetabolite, and trimethoprim in wastewater using liquid chromatography coupled to electrospray tandem mass spectrometry (2004) Analitical Chemistry, 76, pp. 4756-4764Hernández, F., Ibáñez, M., Sancho, J.V., Pozo, O.J., Comparison of different mass spectrometric techniques combined with liquid chromatography for confirmation of pesticides in environmental water based on the use of identification points (2004) Analytical Chemistry, 76, pp. 4349-4357Horie, M., Takegami, H., Toya, K., Nakazawa, H., Determination of macrolide antibiotics in meat and fish by liquid chromatography-electrospray mass spectrometry (2003) Analytica Chimica Acta, 492, pp. 187-197Horie, M., Chemical analysis of macrolides antibiotics (1995) Chemical Analysis for Antibiotics Used in Agriculture, pp. 165-205. , AOAC International, Arlington, VA, USA, H. Oka, H. Nakazawa, K. Harada, J.D. MacNeil (Eds.)(2010) The Japan Food Chemical Research Foundation. 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