Fourier transform Raman spectroscopy and chemometric tools have been used for exploratory analysis of pure corn and cassava starch samples and mixtures of both starches, as well as for the quantification of amylose content in corn and cassava starch samples. The exploratory analysis using principal component analysis shows that two natural groups of similar samples can be obtained, according to the amylose content, and consequently the botanical origins. The Raman band at 480 cm(-1), assigned to the ring vibration of starches, has the major contribution to the separation of the corn and cassava starch samples. This region was used as a marker to identify the presence of starch in different samples, as well as to characterize amylose and amylopectin. Two calibration models were developed based on partial least squares regression involving pure corn and cassava, and a third model with both starch samples was also built; the results were compared with the results of the standard colorimetric method. The samples were separated into two groups of calibration and validation by employing the Kennard-Stone algorithm and the optimum number of latent variables was chosen by the root mean square error of cross-validation obtained from the calibration set by internal validation (leave one out). The performance of each model was evaluated by the root mean square errors of calibration and prediction, and the results obtained indicate that Fourier transform Raman spectroscopy can be used for rapid determination of apparent amylose in starch samples with prediction errors similar to those of the standard method.

a b s t r a c tThis study evaluated the effect of addition of modified starch on the characteristics of dulce de leche, being conducted in two phases. In the initial phase, starches were evaluated for their ability to provide viscosity in model solutions representing the composition of dulce de leche during processing, thus evaluating the effect of solid concentration, which occurs during production, on the ability of starches to increase viscosity in simulated conditions of heat treatment and agitation promoted by Rapid Visco Analyser (RVA). It has been chosen 2 starches and 2 concentrations of soluble solids from the results of the initial phase, being employed as a criterion of choice starches with the highest viscosities at each solid concentration processing phase. In the second stage, 6 treatments were applied in triplicate, in which it's been determined the chemical composition, the instrumental color, texture profile and yield. Analyses were performed on crystallization of lactose during storage. According to the established conditions of the experiment, the starch configures itself as an important optional ingredient for the production of dulce de leche providing then longer shelf life without change in texture, composition, yield and sensory characteristic.

In this work, FT-Raman spectroscopy was explored as a fast and reliable screening method for the assessment of milk powder quality and the identification of samples adulterated with whey (1-40% w/w). Raman measurements can easily differentiate milk powders without the need of sample preparation, whereas the traditional methods of quality control, including high-performance liquid chromatography, are laborious and slow. The FT-Raman spectra of whole, low-fat, and skimmed milk powder samples were obtained and distinguished from commercial milk powder samples. In addition, the exploratory analysis employing data from Raman spectroscopy and principal component analysis (PCA)allowed the separation of milk powder samples according to type,identifying differences between samples in the same group. Multivariate analysis was also developed to classify the adulterated milk powder samples using PCA and partial least squares discriminate analysis (PLS-DA). The resulting PLS-DA model correctly classified 100% of the adulterated samples. These results clearly demonstrate the utility of FT-Raman spectroscopy combined with chemometrics as a rapid method for screening milk powder.

Spectroscopic techniques, including Raman, IR, UV/vis, and NMR were used to characterize the samples of the azo dye Ponceau 4R (also known as E124, New Coccine; Cochineal Red; C.I. no. 16255; Food Red No. 102), which is 1,3-naphthalenedisulfonic acid, 7-hydroxy-8-[(4-sulfo-1-naphthalenyl) azo] trisodium salt in aqueous solution and solid state. In addition, first principle calculations were carried out for the azo (OH) and hydrazo (NH) tautomers in order to assist in the assignment of the experimental data. The two intense bands observed in the UV/vis spectrum, centered at 332 and 507 nm, can be compared to the calculated values at 296 and 474 nm for azo and 315 and 500 nm for hydrazo isomer, with the latter in closer agreement to the experiment. The Raman spectrum is quite sensitive to tautomeric equilibrium; in solid state and aqueous solution, three bands were observed around 1574, 1515, and 1364 cm(-1), assigned to mixed modes including deltaNH + betaCH + nuCC, deltaNH + nuC horizontal lineO + nuC horizontal lineN + betaCH and nuCC vibrations, respectively. These assignments are predicted only for the NH species centered at 1606, 1554, and 1375 cm(-1). The calculated Raman spectrum for the azo (OH) tautomer showed two strong bands at 1468 (nuN = N + deltaOH) and 1324 cm(-1) (nuCC + nuC-N), which were not obtained experimentally. The (13)C NMR spectrum showed a very characteristic peak at 192 ppm assigned to the carbon bound to oxygen in the naphthol ring; the predicted values were 165 ppm for OH and 187 for NH isomer, supporting once again the predominance of NH species in solution. Therefore, all of the experimental and theoretical results strongly suggest the food dye Ponceau 4R or E124 has a major contribution of the hydrazo structure instead of the azo form as the most abundant in condensate phase.

FT-Raman spectroscopy has been explored as a quick screening method to evaluate the presence of lactose and identify milk powder samples adulterated with maltodextrin (2.5-50% w/w). Raman measurements can easily differentiate samples of milk powder, without the need for sample preparation, while traditional quality control methods, including high performance liquid chromatography, are cumbersome and slow. FT-Raman spectra were obtained from samples of whole lactose and low-lactose milk powder, both without and with addition of maltodextrin. Differences were observed between the spectra involved in identifying samples with low lactose content, as well as adulterated samples. Exploratory data analysis using Raman spectroscopy and multivariate analysis was also developed to classify samples with PCA and PLS-DA. The PLS-DA models obtained allowed to correctly classify all samples. These results demonstrate the utility of FT-Raman spectroscopy in combination with chemometrics to infer about the quality of milk powder.

In this work, FT-Raman spectroscopy is explored as a rapid technique for the assessment of the milk powder quality. Based on information provided by Raman spectra of samples adulterated with starch and whey, a quantitative method is developed to identify the fraud, using Partial Least Squares regression (PLS). In regression models using PLS the results are satisfactory, and such models can be used to identify and quantify samples presenting whey and starch in milk powder at concentrations of 2.32% and 1.64% (w/w), respectively. In the whey determination, the obtained values in the PLS model of the new samples are compared with those obtained by the spectrophotometric method of acid ninhydrin. This result shows that there is no significant difference with the 95% level of confidence between the values provided by the PLS regression method and the acid ninhydrin. The present work shows Raman spectroscopy as an analytical tool which can be used in quality control of milk powder, even in fraud processes, and the calculated figures of merit such as sensitivity, accuracy, limit of detection and limit of quantification clearly demonstrate this potential use. Although the multivariate models developed are not strictly quantitative, especially for low concentrations, they can be used as screening methods for routine analysis, as showed by this work. The authors wish to thank CNPq, FAPEMIG, CAPES, and FINEP (Brazilian agencies) for financial support. This work is a collaboration research project of members of the Rede Mineira de Química (RQ-MG) supported by FAPEMIG.

Originally hailing from Latin America, dulce de leche (DL) is one of the most widely manufactured dairy products in South America, where it is marketed as a paste or bar. Due to DL's low moisture content, the product can be safely stored at room temperature, which facilitates storage and transportation logistics. The primary ingredients used to manufacture DL are milk, sucrose, and an acidity reducer. Needless to say, the raw materials must be of good quality from reliable suppliers in order for the final product to have the desired characteristics. The milk used to make DL must be microbiologically safe, remain stable during thermal processing, and preferably exhibit a high solid content. Dulce de leche is defined as a product made with or without the addition of other food substances that is obtained from milk or reconstituted milk and added sucrose (either partially substituted or not by monosaccharides and/or other disaccharides) via concentration and heat action at normal or reduced pressure. This chapter aims to explore the chemistry, processing technology, and most common industrial practices for manufacturing DL in South America.

Few reports describe the effect of lactose hydrolysis on the properties of milk powder during production and storage. Hence, the aim of this study was to evaluate the effects of five different levels of enzymatic lactose hydrolysis during the production and storage of milk powder. As the lactose hydrolysis rate increased, adhesion to the drying chamber also increased, due to higher levels of particle agglomeration. Additionally, more brown powder was obtained when the lactose hydrolysis rate was increased, which in turn negatively affected rehydration ability. Using Raman spectroscopy, crystallization of the lactose residues in various samples was assessed over 6 weeks of accelerated aging at a room temperature environment with 75.5 % of air moisture.Products with 25% or greater lactose hydrolysis showed no signs of crystallization, in contrast to the non-hydrolyzed sample.