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Previous issue date: 2010-09-24 / Coffee is an extremely complex food matrix and has an important role in the world?s
economy, especially in producing and exporting countries like Brazil. However this product
may suffer from technical barriers imposed for exportation because of the possible presence
of ochratoxin A, which is nefrotoxic and carcinogenic mycotoxin found in many foods
including coffee. The aim of this study was to implement chemical metrology concepts in the
development and validation of Liquid Chromatography with Mass Spectrometry in tandem
(CLAE-EM/EM) method for identification and quantification of ochratoxin A in green and
roasted coffee estimating uncertainty of measurement according to directive 2002/657/EC and
Inmetro guidelines (DOC-CGCRE-2010). The extraction method was based on Pittet (1998)
and chromatographic parameters were: flow rate of 0.3 mL/min, mobile phase 80:20 water
trifluoracetic acid 0.05 %: methanol trifluoracetic acid 0.05 %, injection volume of 50 PL,
injection mode Full loop, isocratic mode. The column was Synergi Hydro C18. The mass
spectrometry parameters were optimized and transitions selected based on the colision
energies monitored were m/z 404 >358 (-10.5 V) and m/z 404 >239 (-20.5 V). From the
validation procedure, methods were considered seletive. The evaluation and verification of
matrix effect was performed by comparing variances and averages using F and t test. Value of
Fcalculated for green coffee (25.2152) and roasted coffee (104.0353), were higher than Ftable
(4.0426). Value of t calculated for green (5.0214) and roasted coffee (10.1997) were higher than
ttable (2.0106). Both methods were considered linear in the working range of calibration curve
with linear correlation coefficients (r) of 0.98188 and 0.91754 for green and roasted coffee,
respectively.The quantification and detection limits were 1.2 Pg/kg and 3.0 Pg/kg; 0.36 Pg/kg
and 1.0 Pg/kg, for green and roasted coffee respectively. The average recoveries, RSDr and
RSDR were in range of 90.45 ? 108.81 %, 5.39 ? 9.94 % and 2.20 ? 14.34 % for green coffee
and 89.02 ? 108.85 %, 2.43 ? 13.73 % and 12.57 ? 17.84 % for roasted coffee. All results
obtained were considered within acceptable levels according to literature. Measurement value
and expanded uncertainties (U) for ochratoxin A were mass fraction w = (11.50 ? 1.11) and w
= (4.63 ? 0.63) for green coffee and roasted coffee. Both methods developed and validated
using a high sensitivity technique, that allowed detection, confirmation and quantification of
ochratoxin A in green and roasted coffee with a estimated uncertainty of measurement, and in
the future these methods can be used to help overcome possible technical barriers imposed for
exportation of Brazilian coffee. / O caf? constitui uma matriz extremamente complexa e tem importante papel na economia
mundial, especialmente nos pa?ses produtores e exportadores como o Brasil. No entanto tem
sido alvo de barreiras t?cnicas devido a uma subst?ncia denominada ocratoxina A, micotoxina
potencialmente nefrot?xica e nefrocarcinog?nica encontrada em muitos alimentos inclusive o
caf?. O presente trabalho tem como objetivo implantar os conceitos da metrologia qu?mica no
desenvolvimento, e valida??o do m?todo para identifica??o e quantifica??o de ocratoxina A
no caf? verde e caf? torrado estimando a incerteza da medi??o e utilizando a t?cnica de
Cromatografia L?quida acoplada a Espectrometria de Massas em s?rie (CLAE-EM/EM)
seguindo os crit?rios da diretiva EC-657/2002 e o documento orientativo do Inmetro (DOCCGCRE-
2010). A metodologia de extra??o baseou-se em Pittet (1998) e os par?metros
cromatogr?ficos foram: fluxo de 0,3 mL/min, fase m?vel 80:20 ?gua ?cido trifluoroac?tico
0,05%: metanol ?cido trifluoroac?tico 0,05 %, volume de inje??o de 50 PL, com o modo de
inje??o Full loop e sistema de elui??o isocr?tico. A coluna utilizada foi Synergi Hydro C18. As
condi??es do espectr?metro de massas foram otimizadas e a transi??o selecionada de acordo
com suas energias de colis?o foram m/z 404 >358 (-10,5 V) e m/z 404 >239 (-20,5 V). A
partir da valida??o os m?todos propostos foram considerados seletivos, a avalia??o e
comprova??o do efeito matriz foi realizada atrav?s da compara??o das vari?ncias e das
m?dias atrav?s do teste F e teste t. O Fcalculado para o m?todo caf? verde (25,2152) e caf?
torrado (104,0353), apresentaram valores maiores que o Ftabelado (4,0426). O tcalculado para o
caf? verde (5,0214) e torrado (10,1997) apresentaram valores superiores ao ttabelado (2,0106).
Os m?todos foram considerados lineares em toda a faixa de trabalho da curva de calibra??o
com os coeficientes de determina??o linear (r) de 0,98188 e 0,91754 para matriz caf? verde e
caf? torrado, respectivamente. O limite de quantifica??o e detec??o para os m?todos propostos
foram de 1,2 Pg/kg e 3,0 Pg/kg para caf? verde e 0,36 Pg/kg e 1,0 Pg/kg para caf? torrado. Os
valores das recupera??es m?dias, DPRr e DPRR variaram na faixa de 90,45 - 108,81 %, 5,39
- 9,94 % e 2,20 - 14,34 % para caf? verde; e de 89,02 - 108,85 %, de 2,43 - 13,73 % e 12,57 -
17,84 %, para caf? torrado. Todos os resultados obtidos encontram-se dentro dos limites
comumente aceit?veis na literatura. Todos os resultados de medi??o e as incertezas
expandidas (U) para ocratoxina A foram as fra??es m?ssicas W = (11,50 ? 1,11) Pg/kg e W =
(4,63 ? 0,63) Pg/kg para caf? verde e caf? torrado, respectivamente. Os m?todos
desenvolvidos e validados utilizaram t?cnica de elevada sensibilidade, permitindo a detec??o,
confirma??o e a quantifica??o de ocratoxina A no caf? verde e caf? torrado com c?lculo da
incerteza, podendo auxiliar futuramente na supera??o das barreiras t?cnicas para exporta??o
do caf? brasileiro.
| Identifer | oai:union.ndltd.org:IBICT/oai:localhost:jspui/2349 |
| Date | 24 September 2010 |
| Creators | Bandeira, Raquel Duarte da Costa Cunha |
| Contributors | Godoy, Ronoel Luiz de Oliveira, Caixeiro, Janaina Marques Rodrigues, Souza, Vanderl?a de, Borguini, Renata Galhardo, Saldanha, Tatiana |
| Publisher | Universidade Federal Rural do Rio de Janeiro, Programa de P?s-Gradua??o em Ci?ncias e Tecnologia de Alimentos, UFRRJ, Brasil, Instituto de Tecnologia |
| Source Sets | IBICT Brazilian ETDs |
| Language | Portuguese |
| Detected Language | English |
| Type | info:eu-repo/semantics/publishedVersion, info:eu-repo/semantics/doctoralThesis |
| Format | application/pdf |
| Source | reponame:Biblioteca Digital de Teses e Dissertações da UFRRJ, instname:Universidade Federal Rural do Rio de Janeiro, instacron:UFRRJ |
| Rights | info:eu-repo/semantics/openAccess |
| Relation | ABIC (ASSOCIA??O BRASILEIRA DA IND?STRIA DE CAF?). Estat?sticas: Indicadores da Ind?stria de caf? do Brasil. In: portal da Associa??o Brasileira da Ind?stria de caf?. Dispon?vel em: <http://www.abic.com.br/exporta??o>. Acesso: jun. 2010. ABNT, INMETRO (Associa??o Brasileira de Normas T?cnicas, Instituto Nacional de Metrologia, Normaliza??o e Qualidade Industrial); Guia para a Express?o da Incerteza de Medi??o, 3a Ed., Rio de Janeiro, 2003. ABNT, NBR ISO/IEC 17025:2005. (Associa??o Brasileira de Normas T?cnicas, Instituto Nacional de Metrologia, Normaliza??o e Qualidade Industrial); Requisitos Gerais para compet?ncia de laborat?rios de ensaio e calibra??o, 2a Ed., Rio de Janeiro, 2005. AHMED, N.E., FARAG, M.M., SOLIMAN, K.M., ABDEL-SANED, A.K.M., NAGUIB, KH. M. Evaluation of Methods Used To Determine Ochratoxin A in Coffee Beans. Journal of Agricultural and Food Chemistry, v. 55, p. 9576-9580, 2007. ALMEIDA, A.P. J. ALABURDA, L. SHUNDO, V. RUVIERI, S.A. NAVAS, L.C.A. LAMARDO, M. SABINO. Ochratoxin A in Brazilian instant coffee. Brazilian Journal of Microbiology, v. 38, p. 300-303, 2007. ANVISA (AGENCIA NACIONAL DE VIGILANCIA SANITARIA). Legisla??o. In: portal da Ag?ncia Nacional de Vigil?ncia Sanit?ria). Dispon?vel em: http://www.anvisa.gov.br/legis/portarias/377 99.htm. Acesso: jun 2009. AUGUSTO, C. R. A influ?ncia da incerteza de medi??o da an?lise cromatogr?fica do g?s natural no c?lculo do poder calor?fico superior do g?s, Rio de Janeiro, Brasil, 2007. Disserta??o (Mestrado em Tecnologia de Processos Qu?micos e Bioqu?micos) ? Escola de Qu?mica, EQ, Universidade Federal do Rio de Janeiro, RJ, p. 53-65, 2007. BAYMAN, P., BAKER, J.L. Ochratoxins: a global perspective. Mycopathologia. v.162, p.215, 2006. BECKER, M. P. DEGELMANN, M. HERDERICH, P. SCHREIER, H.U., HUMPT, H. U. Column liquid chromatography-electrospray ionization-tandem mass spectrometry for the analysis of ochratoxin. Journal of Chromatography A, v. 818, p. 260-264, 1998. BLANC, M. et al. Behavior of Ochratoxin A during Green Coffee Roasting and Soluble Coffee Manufacture. J. Agric. Food Chem., v. 46, n.2, p.673-675, 1998. BRASIL, MAPA (Minist?rio da Agricultura, Pecu?ria e Abastecimento). Metodologia anal?tica para determina??o de ocratoxina A por cromatografia liquida de alta efici?ncia (CLAE) em caf? verde, milho e feij?o. Instru??o Normativa, n.9, mar, 2000. BRESH, M., URBANEK, M., HELL, K. Ochratoxin A in coffee, tea and beer. Archiv f?r Lebensmittelhygiene, v.51, p.89-94, 2000. 98 BRUTTEL, P.; SCHLINK, R. Determina??o de ?gua por titula??o Karl Fisher. Metrohm Ltd, 2003, p. 2-70. Dispon?vel em http://www.titrators.us/applications/lit/mono.html. Acesso: jun 2009. BUCHELLI, P., TANIWAKI, M. H. Review: Research on the origin, and on the impact of post-harvest handling and manufacturing on the presence of ochratoxin in coffee. Food Additives Contaminants, v. 19, p. 655-665, 2002. BULLERMAN, L. B. In: Caballero, B.; Tr?go, L. C.; Finglas, P. Encyclopedia of Food Sciences and Nutrition. 2 nd Edition. London: Academic Press, v.6, 2003, 4080-4108 p. CECAF? (CONSELHO DOS EXPORTADORES DE CAF? DO BRASIL). Dados de Exporta??es de Agosto/2009. In: Portal do Conselho dos exportadores de caf? do Brasil. Dispon?vel em: http://www.cecafe.com.br/Menu/dados/exportacoes.pdf. Acesso: set. 2009. CHIARADIA, M.C., COLLINS, C.H., JARDIM, I. C.S.F. O estado da arte da cromatografia associada a espectrometria de massa acoplada a espectrometria de massas na an?lise de compostos t?xicos em alimentos. Qu?mica Nova, v. 31, n.3, p. 623-636, 2008. CLARKE, R.J., MACRAE, R. Coffee Chemistry. London: Elsevier Applied Science Publishers; 1985, v.1, c., 42 p. CLARKE, R.J. MACRAE, R. Green coffee, Roast and Ground. In: Encyclopedia of Food Sciences and Nutrition. CABALLERO, B.,TRtGO, L.C., FINGLAS,P. (Ed), 2? edi??o, Academic Press, 2003, v. 3, 1486, 1489 p. CODEX, 2007, Joint FAO/WHO Food Standards Programme Codex Committee on Contaminants in Food. Discussion paper on Ochratoxin A in coffee. 2006. First Session, April 16-20, 2007 (China:WHO). COELHO, K.F. Avalia??o qu?mica e sensorial da qualidade do caf? de bebida estritamente mole ap?s a inclus?o de gr?os defeituosos, Lavras, Brasil, 2000. Disserta??o (Mestrado em Ci?ncia de alimentos) ? Universidade Federal de Lavras, p. 3-17, 2000. CROUBELS, S., DE BAERE, S., DE BACKER, P. Practical approach for the stability testing of veterinary dr?gs in solutions and in biological matrices during storage. Analytica Chimica Acta, n. 483, p. 419-427, 2003. CUNHA, R.D.C. Identifica??o de compostos vol?teis de caf? sadios e com defeito por cromatografia gasosa e an?lise multivariada, Rio de Janeiro, Brasil, 2005. Disserta??o (Mestrado em Ci?ncia de alimentos) ? Instituto de Qu?mica, IQ, Universidade Federal do Rio de Janeiro, RJ, p. 1-12, 2005. DE GRANDE, S.M. B., AQUINO NETO, F. R. A espectrometria de massas acoplada a espectrometria de massas EM-EM. Qu?mica Nova, v.13, n.3, p.191-199, 1990. DE LA CRUZ, M.H.C., RODRIGUES, J.M., COUTO, P.R., CUNHA, V.S., BREMSER,W. Estimativa da Incerteza de medi??o em an?lise cromatogr?fica: abordagem sobre a quantifica??o de carbamato de etila na cacha?a. Qu?mica Nova, v. 33, n.7, p.1-7, 2010. 99 DE MARIA, C.A.B., TRtGO, L.C., MOREIRA, R.F.A., WERNECK, C.C. Composition of green coffee fractions an theirs contribution to the volatile profile formated during roasting. Food Chemistry, v.50, p.141-145, 1994. DE OLIVEIRA, E.C., DE AGUIAR, P.F. Valida??o da Metodologia da avalia??o de incerteza em curvas de calibra??o melhor ajustada por polin?mio de segundo grau. Quim. Nova, v.32, n.6, p.1655, 2009. DIAS, J.L.M. Medida, Normaliza??o e Qualidade: aspectos da hist?ria da metrologia no Brasil. Rio de Janeiro. Inmetro, c.1-6, 1998, 11-208 p. DIAZ, G. J.; ARIZA, D.; PERILLA, N. S. Method validation for the determination of ochratoxin A in green and soluble coffee by immunoaffinity column cleanup and liquid chromatography. Mycotoxin Research, v. 20, p.59, 2004. EC. 2002. Commission Decision (EC) No. 657/2002 of 2 A?gust 2002. Official Journal of the European Communities L221/8-36. EC. 2005. Commission Regulation (EC) No. 123/2005 of 26 January 2005. Official Journal of the European Union L25: 3-5. ENTERWILSE, A., WILLIANS, A.C., MANN,P.J., RUSSELL, J. SLACK, P.T., GILBERT, J. Combined phenyl silane and immunoaffinity column cleanup with liquid chromatography for determination of ochratoxin A in roasted coffee: Collaborative study. Journal of AOAC International, v. 84, n. 2, p. 444-450, 2001. EURACHEM, CITAC Working Group (The Cooperation on International Traceability in Analytical Chemistry, A focus for Analytical Chemistry in Europe). Quantifying Uncertainty in Analytical Measurement, 2nd Edition, 2000, 4-30p. FAO (FOOD AND AGRICULTURE ORGANIZATION OF THE UNITED NATIONS/ WORLD HEALTH ORGANIZATION). International Conference on Mycotoxins; Report of Joint FAO/WHO/UNEP. Tunis: WHO, 1999. FAO (FOOD AND AGRICULTURE ORGANIZATION OF THE UNITED NATIONS/ WORLD HEALTH ORGANIZATION). Manual on the application of the Haccp System in mycotoxin prevention and control. In: portal Food and agriculture organization of the united nations. Dispon?vel em: http://www.fao.org/docrep/005/y1390e/y1390e00.htm>. Acesso: set. 2009. FAO/WHO (FOOD AND AGRICULTURE ORGANIZATION OF THE UNITED NATIONS/ WORLD HEALTH ORGANIZATION). Reducing OTA in Coffee. In: portal da Food and agriculture organization of the united nations. Dispon?vel em <http://www.coffee-ota.org/faq.asp>. Acesso: set. 2009. FARAH, A. Distribui??o nos gr?os, import?ncia na qualidade da bebida e biodisponibilidade dos ?cidos clorogenicos do caf?, Rio de Janeiro, Brasil. 2004. Tese (Doutorado em Ci?ncia de alimentos) - Instituto de Qu?mica, CT, Universidade Federal do Rio de Janeiro, RJ, 2004. 100 FROTA, M.N., OHAYON, P. Padr?es e Unidades de Medida ? Refer?ncias Metrol?gicas da Fran?a e do Brasil. Rio de Janeiro. Inmetro, 1999, 120 p. FROTA, M.N., MULLER, T.H., SEMERIJAN, H.G. Metrology in Chemistry: a new challenge for the Americas: prodeedings of the First Interamerican Workshop on Metrology in Chemistry. Rio de Janeiro. Inmetro, 1998, 1-244 p. FUJII, S. ONO, E.Y.S., RIBEIRO, R.M.R., ASSUN??O, F.G.A., TAKABAYASHI, C.R., OLIVEIRA, T.C.R.M., ITANO, E.N., UENO, Y., KAWAMURA, O., HIROOKA, E.Y. A comparison between enzyme immunoassay and HPLC for Ochratoxin A detection in green, roasted and instant coffee. Brazilian Archives of Biology and Technology, v. 50, p. 349- 359, 2007. FUJII, S.; ONO, E. Y. S., HIROOKA, E.Y. Ocratoxina A em caf?: controle e metodologia anal?tica com ?nfase a inova??o no contexto de seguran?a alimentar. Semin?rio de Ci?ncias Agr?rias, v.23, n.2, p.273-292, 2002. FURLANI, R.P.Z., SOARES, L.M.V.,OLIVEIRA, P.L.C. Avalia??o de m?todos para determina??o de Ocratoxina A em caf?s verdes e torrados. Revista do Instituto Adolfo Lutz, v. 58, p. 87-98, 1998. GILBERT, J.; ANKLAM, E. Validation of analytical methods for determining mycotoxins in foodstuffs. Trends in Analytical Chemistry, n. 21, n.6, p. 468, 2002. GOLLUCKE, A. P. B., TANIWAKI, M. H.; TAVARES, D. Q. Survey on ochratoxin A in Brazilian green coffee destined for exports. Ci?ncia e Tecnologia de Alimentos, v.24, p.641-645, 2004. GONZALEZ, E.A.S. Estudo da viabilidade de implanta??o de pequenas unidades de torrefa??o de caf?, Rio de Janeiro, Brasil, 2003. Trabalho de Conclus?o de Curso. Gradua??o em Engenharia de Alimentos - Universidade Est?cio de S?, RJ, 2003. HORWITZ, W. Uncertainty: a chemist?s view. J. AOAC Int., v.81, n.4, p.785-794, 1998. HORWITZ, W., ALBERT, R. Quality Issues the concept of uncertainty as applied to chemical measurements. Analyst , v.122, p.615, 1997. INDEX MERCK. 20 th Edition. New Jersey; Merck & CO. Inc; 1996, 1521-1529 p. INMETRO. DOQ-CGCRE N? 008, 2010. Orienta??o sobre Valida??o do M?todos de Ensaios Qu?micos, Instituto Nacional de Metrologia, Normaliza??o e Qualidade Industrial. Rio de Janeiro, n.3, 2010. INMETRO. VIM, 2008. Vocabul?rio Internacional de Metrologia: Conceitos Fundamentais e Gerais e Termos Associados, Instituto Nacional de Metrologia, Normaliza??o e Qualidade Industrial, JCGM, 3a Ed., Rio de Janeiro, 2008. ISENGARD, H. D.; F?RBER, J. M. Hidden parameters of infrared drying for determining low water contents in instant powders. Talanta, v. 50, n. 2, p. 239-246, 1999. 101 ISO GUIDE 35. Reference Material ? General and Statistical principles for certification. International Organization for Standardization. Geneva, 3 rd edition, 2006. JOSEPHS, R. D., KRSKA, R., MACDONALD, S., WILSON, P., PETTERSON, H. Preparation of calibrant as certified reference material for determination of the Fusarium Mycotoxin Zearalenone. J. AOAC Int., v. 86, p. 50, 2006. LAU, B. P. Y., SCOTT, D.A., KANHERE, L., KANHERE, S.R. Quantitative determination of ochratoxin A by liquid chromatography/electrospray tandem mass spectrometry. Journal of Mass Spectrometry, v.35, p.23-32, 2000. LEONI, L.A.B.; FURLANI, R.P.Z.; VALENTE SOARES, L.M.; OLIVEIRA, P.L.C. Ochratoxin A in brazilian green coffee. Ci?ncia e Tecnologia de Alimentos, v. 21, n.1, p.105, 2001. LINDENMEIER, M., SCHIEBERLE, P., RYCHLIK, M. Quantification of Ochratoxin A in food by stable isotope dilution assay using high-performance liquid chromatography-tandem mass-spectrometry. Journal of Chromatography A, v. 1023, p. 57-66, 2004. MANTLE, P.G. Risk assessment and the importance of ocharatoxins. Int Biodet & Biodeg, v.50, p.143-146, 2002. MARC?, A., COMPANY?, R., RUBIO, R., PUEYO, M., VILALTA, E.; Microchim. Acta, v.159, p. 387, 2007. MARTIN, S.K. Coffee and tea. In: William HORWITZ; George W. LATIMER, Jr. (Ed.) Official methods of analysis of the AOAC International. Gaithersburg: AOAC International, 2005, p. 1-12. MASOUD, W.; KALTOFT, C. H. The effects of yeasts involved in the fermentation of Coffea arabica in East Africa on growth and ochratoxin A (OTA) production by Aspergillus ochraceus. International Journal of Food Microbiology, v.106, p.229 -234, 2006. MELLO, A.A. Estudo dos compostos vol?teis formados por pir?lise da fra??o de alto Massa Molecular isolada de caf?, Rio de Janeiro, Brasil, 1998. Disserta??o (Mestrado em Bioqu?mica) ? Instituto de Qu?mica , IQ, Universidade Federal do Rio de Janeiro, RJ, 1998. MICCO, C. et al. A study of the contamination by ochratoxin A of green and roasted coffee beans. Food Addit. Contam., v. 6, p.333-339, 1989. MOBERG, M., BYLUND, D. B., MARKIDES, K. Optimization strategy for liquid chromatography-electrospray ionization mass spectrometry methods. Analyst, v. 125, p. 1970-1976, 2000. MONACI, L.; PALMISANO, F. Determination of ochratoxin A in foods: state-of-the-art and analytical challenges. Anal Bioanal Chem, n.378, p.96-103, 2004. MORELLO, L.G.; SARTORI, D.; MARTINEZ, A.L.O.; VIEIRA, M.L.; TANIWAKI, M.H., FUNGARO, M.H. Detection and quantification of Aspergillus westerdijkiae in coffee 102 beans based on selective amplification of beta-tubulin gene by using real-time PCR. Inter Journal Food Micro, n.119, p.270, 2007. MORGANO, A. M.; FARIA, C. G.; FERR?O, M. F.; BRAGAGNOLO, N.; FERREIRA, M. M. C.; Determina??o de umidade em caf? cru usando espectroscopia NIR e regress?o multivariada. Ci?ncia e Tecnologia de Alimentos, v. 28, n. 1, p. 12-17, 2008. NESHEIM, S. TRUCKSESS, M. W., PAGE, S. W. Molar absorptivities of aflatoxins B1, B2, G1 and G2 in acetonitrile, methanol and toluene-acetonitrile (9:1) (Modification of AOAC Official Method 971.22): Collaborative study. Journal of AOAC International, v.82, n.2, p. 251-257, 1999. NIESSEN, W.M.A., TINKE, A.P. Liquid chromatography ? mass spectrometry General principles and instrumentation. Journal of Chromatography A, v. 703, p. 35-57, 1995. NIST. An approach to the metrologically sound traceable assessment of the chemical purity of organic reference materials, National Institute of Standards and Technology. United States, 53 p., 2004. PATEL, S., HAZEL, C.M., WINTERTON, A. G. M., GLEADLE, A.E. Survey of ochratoxin A in UK retail coffees. Food Additives Contaminants, v.14, p.217-222, 1997. PITTET, A.; TORNARE, D.; HtGGETT, A.; VIANI, R. Liquid chromatography determination of ochratoxin A in pure and adulterated soluble coffee using an immunoaffinity column cleanup procedure. Journal of Agricultural and Food Chemistry, v. 44, p. 3564-3569, 1996. POHLAND, A.E., NESHEIM, S., FRIEDMAN, L. Ochratoxin A: a review. Pure and Applied Chemistry, v.64, n.7, p.1029-1049, 1992. PRADO, G., OLIVEIRA, M.S., ABRANTES, F.M., SANTOS, L.G., VELOSO, T., BARROSO, R.E.S. Incid?ncia de Ocratoxina A em caf? torrado e mo?do e em caf? sol?vel consumido na cidade de Belo Horizonte, MG. Ci?ncia e Tecnologia de Alimentos, v.20, n.2, p.192-196, 2000. RAND, R.N. Practical Spectrophotometric Standards. Clinical Chemistry, v. 15, n.9, p. 839-863, 1969. RODRIGUA-AMAYA, D.B.; SABINO, M. Mycotoxin research in Brazil: the last decade in review. Braz J of Microb, 33, 1, 2002. SARTORI, A. V; SANTOS, R. P; MORAES, M. H. P; de la CRUZ, M. H. C. Estimativa da Incerteza de Medi??o Associada ? determina??o da concentra??o de solu??es padr?o de micotoxinas por espectrofotometria de UV. Anais do XVI Encontro Nacional e II Congresso Latino Americano de Analistas de Alimentos, 2009, Belo Horizonte. SCHUMACHER, P. GORENBEIN, A. RASKIN, I. KUSELMAN, Development of an obidoxime chloride reference material: a metrological approach to the determination of chromatographic purity. Accred. Qual. Assur, v.12, p.629-636, 2007. 103 SFORZA, S., DALL?ASTA, C. E MARCHELLI, R. Recent advances in mycotoxin determination in food and feed by hyphenated chromatographic techniques/ Mass spectrometry. Mass Spectrometry Reviews, v.25, n.1, p.54-76, 2006. SIBANDA, L., DE SAEGER, S., VAN PETEGHEM, C. Optimization of solid-phase cleanup prior to liquid chromatographic analysis of ochratoxin A in roasted coffee. Journal of Chromatography A, v.959, p.327?330, 2002. STUDER-ROHR, I.; DIETRICH, D.R.; SCHLATTER, J.; SCHLATTER, C. The occurrence of ochratoxin A in coffee. Food and Chemical Toxicology, v. 33, p. 341,1995. TANIWAKI, M. H.; PITT, J. I.; TEIXEIRA, A. A.; IAMANAKA, B. T. The source of ochratoxin A in Brazilian coffee and its formation in relation to processing methods. International Journal of Food Microbiology, v. 82, n. 2, p. 173-179, 2003. TOLEDO, J.L.B., BARBOSA, A.T., Classifica??o e degusta??o de caf?. Bras?lia: Ed Sebrae, Rio de Janeiro, ABIC, 1998, 27-34 p. TRUCKNESS, M.W. Natural Toxins. AOAC (Association of Official Analytical Chemists): Official Methods of Analysis of AOAC International, Gaithesburg, 18 th Edition. Maryland, v. 1, c. 49, 2005, 58-65 p. TRUGO, L.C. Efeito da Torrefa??o no Perfil Cromatogr?fico obtido por Filtra??o em Gel e Extratos de Caf? Ar?bica. Archivos Latino Americanos de Nutricion, v. XXXVI, n. 4; p. 745-753, 1986 TRUGO, L.C., MACRAE, R. Application of high performance liquid chromatography to the analyses of some non-volatil coffee components. Archivos Latino Americanos de Nutrition, v. 39, n.1, p. 60-64,1989. VALENTE SOARES, L. M. Como obter resultados confi?veis em cromatografia. Rev. Inst. Adolfo Lutz, v. 60, n.1, p. 79-84, 2001. VARGAS, E.A., SANTOS, E.A. E PITTET, A. Determination of ochratoxin A in green coffee by immunoaffinity column cleanup and liquid chromatography: collaborative study. Journal of AOAC International, v.88, n.3, p.773-779, 2005. VATINNO, R; ARESTA, A.; ZAMBONIN, C.G.; PALMISANO, F. Determination of Ochratoxin A in green coffee beans by solid-phase microextraction and liquid chromatography with fluorescence detection. Journal of Chromatography A, n.1187, v.145, 2008. VEGA, F.E.; POSADA, F.; PETERSON, S.W.; GIANFAGNA, T., CHAVES, F. Penicillium species endophytic in coffee plants and ochratoxin A production. Mycologia, n.98, p.31, 2006. VENTURA, M.; VALLEJOS, C.; ANAYA, I.A.; BROTO-PUIG, F.; AGUT, M.; COMELLAS, L. Analysis of Ochratoxin A in Coffee by Solid-Phase Cleanup and Narrow- Bore Liquid Chromatography-Fluorescence Detector-Mass Spectrometry. Journal of Agricultural and Food Chemistry, v.51, p.7564-7567, 2003. 104 WIBERG, K.; ANDERSSON, M.; HAGMANA, A.; JACOBSSON, S. P. Peak purity determination with principal component analysis of high-performance liquid chromatography?diode array detection data. Journal of Chromatography A., v. 1029, p. 13 -20, 2004. WIESER, M.E. Atomic Weights of the elements 2005. (Iupac Technical Report). Pure Appl. Chem., v.78, n. 11, p. 2051?2066, 2006. WILLIAMS, A. Measurement uncertainty in analytical chemistry. Accred. Qual. Assur. v.1, n.1, p. 14-17, 1996. ZENEBON, O.; PASCUET, N.S.; TIGLEA, P. M?todos f?sico-qu?micos para an?lise de alimentos. 1a edi??o digital. S?o Paulo: Instituto Adolfo Lutz, c.12, 2008, 489- 501 p. ZOLLNER, P., MAYER-HELM, B. Trace mycotoxin analysis in complex biological and food matrices by liquid chromatography - atmospheric pressure ionisation mass spectrometry. J of Chrom A, n.1136, p.123, 2006. |
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