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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 |
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