2015
Autores
Coelho, L; Viegas, D; Santos, JL; de Almeida, JMMM;
Publicação
FOOD AND BIOPROCESS TECHNOLOGY
Abstract
A new sensing system for the detection of thermal deterioration of extra virgin olive oil based on long period fibre grating is reported. It is demonstrated the feasibility of long period fibre grating sensor for the analysis of high refractive index edible oils. The detection principle is the wavelength dependence of the attenuation bands of a TiO2-coated long period fibre grating on the changes in the refractive index of the medium surrounding the cladding surface of the optical fibre. The quality of the sensor was tested by measuring the wavelength shift of the attenuation bands in response to thermal deterioration of an edible oil (extra virgin olive oil) with refractive index higher than the fibre cladding. Absorption spectroscopy has allowed the effects of thermal deterioration to be detected, for example, in the decreasing of the absorption band at 677 nm, attributed to chlorophyll A. A detection limit of about 5 min at 180 A degrees C and of about 2 min at 225 A degrees C was observed for the sensing system. The proposed sensing system could lead to the realisation of a biochemical sensor for the food industry. The change in refractive index of extra virgin olive oil as a function of heating time and temperature was systematically measured for the first time.
2015
Autores
Vasconcelos M.; Coelho L.; Barros A.; de Almeida J.M.M.M.;
Publicação
Cogent Food and Agriculture
Abstract
A methodology based on Fourier transform infrared spectroscopy with attenuated total reflectance sampling technique, combined with multivariate analysis, was developed to monitor adulteration of extra virgin olive oil (EVOO) with peanut oil (PEO). Principal components regression (PCR), partial least squares regression (PLS-R), and linear discriminant analysis (LDA) allowed quantification of percentage of adulteration based on spectral data of 192 samples. Wavenumbers associated with the biochemical differences among several types of edible oils were investigated by principal component analysis. Two sets of frequencies were selected in order to establish a robust regression model. Set A consisted on the frequency regions from 600 to 1,800 cm-1 and from 2,750 to 3,050 cm-1. Set B comprised 17 discrete peak absorbance frequencies for which the communality value was higher than 0.6. Analysis of an external set of 25 samples allowed the validation and evaluation of the predictability of the models. When using a specific set of discrete peak absorbance frequencies, the R 2 coefficients for the prediction were 0.960 and 0.977, and the root mean square error (RMSE) were 1.49 and 1.05% V/V when using the PCR or PLS-R models, respectively. LDA was successful in the binary classification presence/absence of PEO in adulterated EVOO (with 5% V/V of less of PEO). LDA provided 92.3% correct classification for the calibration set and 88.3% correct classification when cross-validated. The lowest detectable concentration of PEO in EVOO was the lowest adulteration level studied, 0.5% V/V.
2015
Autores
Vilela J.; Coelho L.; de Almeida J.M.M.M.;
Publicação
Cogent Food and Agriculture
Abstract
Fourier transform infrared spectroscopy based on attenuated total reflectance sampling technique, combined with multivariate analysis methods was used to monitor the adulteration of pure sunflower oil (SO) with thermally deteriorated oil (TDO). Contrary to published research, in this work, SO was thermally deteriorated in the absence of foodstuff. SO samples were exposed to temperatures between 125 and 225°C from 6 to 24 h. Quantification of adulteration of SO with TDO, based on principal components regression (PCR), partial least squares regression (PLS-R), and linear discriminant analysis (LDA) applied to mid-infrared spectra and to their first and second derivatives is reported for the first time. Infrared frequencies associated with the biochemical differences between TDO samples deteriorated in different conditions were investigated by principal component analysis (PCA). LDA was effective in the twofold classification presence/absence of TDO in adulterated SO (with 5% V/V of less of TDO). It provided 93.7% correct classification for the calibration set and 91.3% correct classification when cross-validated. A detection limit of 1% V/V of TDO in SO was determined. Investigation of an external set of samples allowed the evaluation of the predictability of the models. The regression coefficient (R 2) for prediction was 0.95 and 0.96 and the RMSE was 2.1 and 1.9% V/V when using the PCR or PLS-R models, respectively, and the first derivative of spectra. To the best of our knowledge, no investigation of adulteration of SO with TDO based on PCR, PLS-R, and LDA has been reported so far.
2015
Autores
Machado, M; Machado, N; Gouvinhas, I; Cunha, M; de Almeida, JMMM; Barros, AIRNA;
Publicação
FOOD ANALYTICAL METHODS
Abstract
The phenolic compound concentration of olives and olive oil is typically quantified using HPLC; however, this process is expensive and time consuming. The purpose of this work was to evaluate the potential of Fourier transform infrared (FTIR) spectroscopy combined with chemometrics, as a rapid tool for the quantitative prediction of phenol content and antioxidant activity in olive fruits and oils from "Cobran double dagger osa" cultivar. Normalized spectral data using standard normal variate (SNV) and first and second Savitzky-Golay derivatives were used to build calibration models based on principal component regression (PCR) and on partial least squares regression (PLS-R), the performance of both models have been also compared. It was shown the possibility of establishing optimized regression models using the combined frequency regions of 3050-2750 and 1800-790 cm(-1) instead of the full mid-infrared spectrum was shown. It was concluded that, in general, the first derivative of data and PLS-R models offered enhanced results. Low root-mean-square error (RMSE) and high correlation coefficients (R (2)) for the calibration and for the validation sets were obtained.
2015
Autores
Gouvinhas, I; de Almeida, JMMM; Carvalho, T; Machado, N; Barros, AIRNA;
Publicação
FOOD CHEMISTRY
Abstract
A methodology based on Fourier transform infrared (FTIR) spectroscopy, combined with multivariate analysis methods, was applied in order to monitor extra virgin olive oils produced from three distinct cultivars on different maturation stages. For the first time, this kind of methodology is used for the simultaneous discrimination of the maturation stage, and different cultivars. Principal component analysis and discriminant analysis were utilised to create a model for the discrimination of olive oil samples. Partial least squares regression was employed to design calibration models for the determination of chemical parameters. The performance of these models was based on the multiple coefficient of determination (R-2), the root mean square error of calibration (RMSEC) and root mean square error of cross validation (RMSECV). The prediction models for the chemical parameters resulted in a R-2 ranged from 0.93 to 0.99, a RMSEC ranged from 1% to 4% and a RMSECV from 2% to 5%. It has been shown that this kind of approach allows to distinguish the different cultivars, and to clearly discern the different maturation stages, in each one of these distinct cultivars. Furthermore, the results demonstrated that FTIR spectroscopy in tandem with chemometric techniques allows the creation of viable and accurate models, suitable for correlating the data collected by FTIR spectroscopy, with the chemical composition of the EVOOs, obtained by standard methods.
2015
Autores
Gouvinhas, I; Machado, N; Carvalho, T; de Almeida, JMMM; Barros, AIRNA;
Publicação
TALANTA
Abstract
Extra virgin olive oils produced from three cultivars on different maturation stages were characterized using Raman spectroscopy. Chemometric methods (principal component analysis, discriminant analysis, principal component regression and partial least squares regression) applied to Raman spectral data were utilized to evaluate and quantify the statistical differences between cultivars and their ripening process. The models for predicting the peroxide value and free acidity of olive oils showed good calibration and prediction values and presented high coefficients of determination ( > 0.933). Both the R-2, and the correlation equations between the measured chemical parameters, and the values predicted by each approach are presented; these comprehend both PCR and PLS, used to assess SNV normalized Raman data, as well as first and second derivative of the spectra. This study demonstrates that a combination of Raman spectroscopy with multivariate analysis methods can be useful to predict rapidly olive oil chemical characteristics during the maturation process.
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