Free amino acid profile in Mimosa scabrella honeydew honey from Brazil and chemometric analysis for geographical discrimination.

In this study, twenty free amino acids (FAA) were investigated in samples of bracatinga (Mimosa scabrella) honeydew honey (BHH) from Santa Catarina (n = 15) and Paraná (n = 13) states (Brazil), followed by chemometric analysis for geographic discrimination. The FAA determination was performed by gas chromatography-mass spectrometry (GC-MS) after using a commercial EZ:faast™ kits for GC. Eight FAA were determined, being proline, asparagine, aspartic and glutamic acids found in all BHH, with significant differences (p < 0.05). In addition, with the exception of proline, the others FAA (asparagine, aspartic and glutamic) normally showed higher concentrations in samples from Santa Catarina state, being that in these samples it was also observed higher FAA sums (963.41 to 2034.73 mg kg-1) when compared to samples from Paraná state. The variability in the results did not show a clear profile of similarity when the heatmap and hierarchical grouping were correlated with the geographic origin and the concentration of eight determined FAA. However, principal component analysis (PCA) demonstrated that serine, asparagine, glutamic acid, and tryptophan were responsible for the geographic discrimination among samples from Santa Catarina and Paraná states, since they were the dominant variables (r > 0.72) in the PCA. Therefore, these results could be useful for the characterization and authentication of BHH based on their FAA composition and geographic origin.

Fraude alimentario: Pasado, presente y futuro

La adulteración y el fraude de productos alimenticios son tan antiguos como los sistemas de procesamiento y producción de alimentos, sin embargo, en la actualidad son cada vez más frecuentes. Con la globalización y los sistemas de producción y distribución de alimentos cada día más complejos, la adulteración puede ocurrir en distintos puntos de la cadena alimentaria y tener un impacto de gran alcance, e incluso, consecuencias adversas para la salud de las personas. Los enfoques regulatorios de la comunidad internacional para enfrentar y resolver el fraude alimentario están dispersos y en constantes ajustes. Se necesita un enfoque colectivo y coordinado para identificar a todos los interesados en la cadena de suministro de alimentos, calificarlos y certificarlos, excluir a aquellos que no cumplan con los estándares adecuados y rastrear los alimentos en tiempo real. Este artículo de actualización revisará conceptos claves asociados a la integridad alimentaria, historia del fraude alimentario y episodios de fraude alimentario de connotación pública en el mundo y en Chile, herramientas analíticas y alimentos más vulnerables al fraude, reglamentos y nuevas acciones en el mundo y en Chile para enfrentar la inocuidad y el riesgo de fraude alimentario.

Food adulteration and food fraud is as old as food production and processing however, it is increasingly prevalent today. With globalization and increasingly complex food production and distribution systems, adulteration can occur at different points in the food chain and may have far-reaching impacts and even adverse consequences for human health. The international community's regulatory approaches to confronting and resolving food fraud are scattered and in constant adjustment. A collective and coordinated approach is needed to identify all stakeholders in the food supply chain, certify and qualify them, exclude those who do not meet applicable standards, and trace food in real time. This update provides definitions and background on key concepts associated with food integrity, episodes of food fraud in Chile and the world, main foods vulnerable to food fraud, common fraud practices and analytical techniques, regulations and new actions in Chile and the world to face food safety and the risk of food fraud.

Lab-made 3D printed electrochemical sensors coupled with chemometrics for Brazilian coffee authentication.

Analytical assurance of coffees' geographical indication (GI) authenticity is essential for producers and consumers. In this way, chemometric methods, electrochemical techniques, and 3D printed sensors become attractive to assure the coffee's quality. These sensors are low-cost, fast, and simple, with the possibility of miniaturization and portability. Therefore, 3D printed electrodes with chemometrics were used to classify-three Brazilian coffees from regions with GI. Further, Au/Gpt-PLA electrodes with partial least squares regression were used to detect the blending of GI coffee with traditional coffee. Soft independent modelling of class analogies coupled with cyclic voltammetry had the best performance, with 91-95% accuracy, specificity of 94-100%, and 80-83% sensitivity. Furthermore, the calibration models detected and quantified traditional coffee in all three coffees from regions with GI. The detection limits ranged from 1.4 to 10% (w/w), and quantification 4.6-32%, depending on the specific coffee.

Capillary electromigration methods for fatty acids determination in vegetable and marine oils: A review.

Fatty acids determination is of paramount importance for quality control and suitable labeling of edible oils, required by regulatory agencies in several countries, and fast methods for this determination are worldly desired. This review article aimed to explore the available analytical methods for vegetable and marine oils analyses employing CE, which can be a straightforward and faster alternative than GC methods for fatty acid determination, considering some purposes. CE usually offers the possibility of a rapid analysis with a simple preparation of the sample, without requiring specific columns, which are inherent advantages of the technique. Instrumental conditions and the key points about fatty acids determination employing the technique are highlighted, and the main challenges and perspectives are also approached. Potential use of CE for edible oil analyses has been demonstrated for research and routine, which can be of interest for industries, regulatory agencies, and edible oil researchers. Therefore, we have explored the analytical approaches described in the last decades, intending to spread the interest of CE methods for fatty acid monitoring, label accuracy assessment, and food authenticity evaluation of edible oils.

Brown rice authenticity evaluation by spark discharge-laser-induced breakdown spectroscopy.

Rice is the most consumed food worldwide, therefore its designation of origin (PDO) is very useful. Laser-induced breakdown spectroscopy (LIBS) is an interesting analytical technique for PDO certification, since it provides fast multielemental analysis requiring minimal sample treatment. In this work LIBS spectral data from rice analysis were evaluated for PDO certification of Argentine brown rice. Samples from two PDOs were analyzed by LIBS coupled to spark discharge. The selection of spectral data was accomplished by extreme gradient boosting (XGBoost), an algorithm currently used in machine learning, but rarely applied in chemical issues. Emission lines of C, Ca, Fe, Mg and Na were selected, and the best performance of classification were obtained using k-nearest neighbor (k-NN) algorithm. The developed method provided 84% of accuracy, 100% of sensitivity and 78% of specificity in classification of test samples. Furthermore, it is simple, clean and can be easily applied for rice certification.

Characterization of Brazilian coffee based on isotope ratio mass spectrometry (δ13C, δ18O, δ2H, and δ15N) and supervised chemometrics.

Authentication of ground coffee has become an important issue because of fraudulent activities in the sector. In the current work, sixty-seven Brazilian coffees produced in different geographical origins using organic (ORG, n = 25) and conventional (CONV, n = 42) systems were analyzed for their stable isotope ratios (δ13C, δ18O, δ2H, and δ15N). Data were analyzed by inferential analysis to compare the factors whereas linear discriminant analysis (LDA), k-nearest neighbors (k-NN), and support vector machines (SVM) were used to classify the coffees based on their origin. ORG and CONV cultivated coffees could not be differentiated according to C stable isotope ratio (δ13C; p = 0.204), but ORG coffees presented higher values of the N stable isotope ratio (δ15N; p = 0.0006). k-NN presented the best classification results for both ORG and CONV coffees (87% and 67%, respectively). SVM correctly classified coffees produced in São Paulo (75% accuracy), while LDA correctly classified 71% of coffees produced in Minas Gerais.

Assessing fish authenticity by direct analysis in real time-high resolution mass spectrometry and multivariate analysis: discrimination between wild-type and farmed salmon.

The constant increase in seafood consumption worldwide has led to a parallel growth of the incidence of products obtained by aquaculture on the market, but also of the fraudulent commercialization of farmed products as wild-type ones. A careful characterization of the lipid component of seafood products based on chromatography-mass spectrometry techniques has been reported as a promising approach to reliably differentiate farmed from wild-type products. In this context, a fast method based on Direct Analysis in Real Time (DART) coupled to High Resolution Mass Spectrometry (HRMS) based on a single stage Orbitrap mass analyzer, integrated by Principal Component Analysis (PCA), was developed in the present study and applied to scout for spectral features useful to discriminate wild-type from farmed salmon of Salmo salar species. In particular, normalized intensities obtained for the 30 most intense signals (all referred to fatty acids, FA) detected in negative ion DART-HRMS spectra of the lipid extracts of salmon fillets [26 wild-type from Canada, 74 farmed from Canada (25), Norway (25) and Chile (24)] were considered as the variables for PCA. The scatterplot referred to the first two principal components showed a clear distinction between wild-type and farmed salmon, which gathered as a unique cluster, despite the remarkable differences in their geographical origin. In accordance with previous studies based on more complex and time-demanding analytical approaches, three saturated (14:0, 16:0 and 18:0) FA, along with unsaturated ones having 20 or 22 carbon atoms, were found as the main discriminating variables for wild-type salmons, whereas FA with compositions 18:1, 18:2, 18:3 and several oxidized forms arising from them were found to have a significantly higher incidence in farmed salmon. The method was further validated by Discriminant Analysis (DA) performed on the same dataset used for PCA integrated by data obtained from 6 commercial samples, putatively referred to farmed Norwegian salmon. Results showed that 100% of the latter were correctly classified as farmed type. Relative abundances of DART-HRMS signals related to specific FA appear then very promising for the differentiation of wild-type salmon from farmed ones, a very relevant issue in the context of consumers' protection from seafood frauds.

Evaluation of a multiplex PCR for detection of a fraud in the minced beef meat by adding buffalo meat / Avaliação da técnica PCR multiplex para detecção de fraude por adição de carne bubalina em carne moída bovina

This study aimed at evaluating the sensitivity of a multiplex PCR technique for detecting fraud by the deliberate addition of buffalo meat into the minced bovine beef. The minced bovine beef containing 0.01 %, 0.1 %, 1.0 %, 5.0 %, 10.0 %, 25.0 %, 50.0 %, 75.0 %, 90.0 %, 95.0 %, 99 %, 99.9 %, 99.99 % of minced buffalo beef were produced in triplicate, with five replicates. The minced meats exclusively of each animal species were used as control samples. Every prepared sample was analyzed by means of multiplex polymerase chain reaction. For performing the assay sensitivity analysis, the known concentrations of DNA samples (0.01 %, 0.1 %, 1.0 %, 5.0 %, 10.0 %, 25.0 %, 50.0 %, 75.0 %, 90.0 %, 95.0 %, 99.0 %, 99.9 %, 99.99 %) from Bos taurus and Bubalus bubalis species were diluted and mixed into a final volume of 10 L; and these DNA samples were also assayed by the proposed PCR methodology. The multiplex PCR showed to be is an effective and highly sensitive technique enough for detecting increments of 10 % (2.05 ng) of bubaline DNA and of 0.1 % (0.041 ng) of bovine DNA.(AU)

O presente trabalho avaliou a sensibilidade de uma modalidade de técnica de PCR multiplex para efetuar a detecção de fraude por adição intencional de carne moída bubalina em carne moída bovina. Neste contexto, as amostras de carnes moídas de bovinos com adição de 0,01 %, 0,1 %, 1,0 %, 5,0 %, 10,0 %, 25,0 %, 50,0 %, 75,0 %, 90,0 %, 95,0 %, 99,0 %, 99,9 %, 99,99 % de carne moída bubalina foram produzidas em triplicata com cinco réplicas. As carnes moídas exclusivamente de cada uma das espécies foram utilizadas como amostras controle. Cada uma das amostras produzidas foi analisada por meio de Reação em Cadeia da Polimerase multiplex. A fim de realizar a análise da sensibilidade do teste, percentagens conhecidas de amostras de DNA (0,01 %, 0,1 %, 1,0 %, 5,0 %,10,0 %, 25,0 %, 50,0 %, 75,0 %, 90,0 %, 95,0 %, 99,0 %, 99,9 %, 99,99 %) das espécies Bos taurus e Bubalus bubalis foram diluídas e misturadas em um volume final de 10 L; e estas foram também analisadas pela metodologia de PCR proposta. A técnica de PCR multiplex mostrou ser eficaz e de alta sensibilidade, capaz de detectar incrementos de 10,0 % (2,05 ng) de DNA bubalino e de 0,1 % (0,041 ng) de DNA bovino.(AU)

Authentication of geographical origin of palm oil by chromatographic fingerprinting of triacylglycerols and partial least square-discriminant analysis.

Main goals of the present work were to develop authentication models based on liquid and gas chromatographic fingerprinting of triacylglycerols (TAGs) from palm oil of different geographical origins in order to compare them. For this purpose, a set of palm oil samples were collected from different continents: South eastern Asia, Africa and South America. For the analysis of the information in these fingerprint profiles, a pattern recognition technique such as partial least square discriminant analysis (PLS-DA) was applied to discriminate the geographical origin of these oils, at continent level. The liquid chromatography, coupled to a charged aerosol detector, (HPLC-CAD) TAGs separation was optimized in terms of mobile phase composition and by means of a solid silica core column. The gas chromatographic method with a mass spectrometer was applied under high temperature (HTGC-MS) in order to analyze the intact TAGs. Satisfactory chromatographic resolution within a short total analysis time was achieved with both chromatographic approaches and without any prior sample treatment. The rates of successful in prediction of the geographical origin of the 85 samples varied between 70% and 100%.