The use of materials such as organofunctionalized silica for application in solid phase extraction (SPE) allows the preconcentration of several ions, including Pt, and subsequent detection. This work aims to synthesize and characterize an organofunctionalized silica (Sil-TMSDT) with the silylant N’(trimethoxysilyl)propylethylenetriamine and its application as a solid phase in the preconcentration Pt4+ ions in aqueous media, using detection by flame atomization atomic absorption spectroscopy (FAAS). The Fourier-transform infrared spectroscopy (FTIR) spectra and scanning electron microscopy (SEM) coupled with energy-dispersive spectroscopy (EDS) confirmed the aminofunctionalization of the silica. For the adsorption process, a preconcentration mini-column with 200 mg of Sil-TMSDT, a solution of 0.485 mg L−1 of K2[PtCl6] at pH 10 and HNO3 0.5 mol L−1 as eluent were used, obtaining an enrichment factor of 15-fold with retention efficiency higher than 99%. The Pt4+ ion determined by FAAS showed a linear response between 0.02 and 0.40 mg L−1; a linear coefficient where R = 0.9981; a 16-fold preconcentration factor; a limit of quantification (LOQ) and limit of detection (LOD) of 0.045 and 0.014 mg L−1, respectively. The proposal system showed analytical applicability to determining Pt4+ ion in an aqueous medium and could be used to detect traces of this potentially toxic metal in biological fluids such as urine and blood. SPE (SPE Pt SilTMSDT Sil TMSDT (Sil-TMSDT Ntrimethoxysilylpropylethylenetriamine N trimethoxysilyl propylethylenetriamine Pt4 media FAAS. . (FAAS) Fouriertransform Fourier transform FTIR (FTIR SEM (SEM energydispersive energy dispersive EDS (EDS process minicolumn mini column 20 SilTMSDT, TMSDT, Sil-TMSDT 0485 0 485 0.48 L1 L 1 L− K2PtCl6 KPtCl K2 PtCl6 K PtCl K2[PtCl6 HNO 05 5 0. 15fold fold 15 99 99% 002 02 0.0 040 40 0.4 0.9981 09981 9981 16fold 16 LOQ (LOQ LOD (LOD 0045 045 0.04 0014 014 0.01 respectively blood (FAAS 2 048 48 K2PtCl K2[PtCl 9 00 04 4 0.998 0998 998 004 001 01 0.99 099 0.9 09

This work developed an effective and eco-friendly analytical method to support quality control for Brazilian Bill proposal No. 5332/2009. The bill advocates the creation of the “Brazilian bread” by mandating the incorporation of cassava byproducts into wheat flour, with the aim of reducing Brazil’s external dependency on wheat imports and promoting domestic cassava family farming. For this, a handheld near-infrared (NIR) spectrophotometer was utilized for on-site determination of cassava starch in commercial wheat flour. The quantitative analysis, which utilized NIR spectra pre-processed with offset correction (OFF) combined with linear baseline correction (LBC), alongside the successive projections algorithm for interval selection in partial least squares (iSPA-PLS), exhibited superior predictive capability, achieving a relative error of prediction below 8%. Furthermore, the classification process, which involved NIR spectra pre-processed with LBC and iSPA-PLS for discriminant analysis (iSPA-PLS-DA), yielded an impressive 94% overall accuracy, with only 3 misclassifications in the test set. ecofriendly eco friendly No 53322009 5332 2009 5332/2009 bread flour Brazils Brazil s farming this nearinfrared near infrared (NIR onsite site preprocessed pre processed OFF (OFF LBC, , (LBC) iSPAPLS, iSPAPLS iSPA PLS (iSPA-PLS) capability 8 8% Furthermore process iSPAPLSDA, iSPAPLSDA DA (iSPA-PLS-DA) 94 accuracy set 5332200 533 200 5332/200 (LBC (iSPA-PLS (iSPA-PLS-DA 9 533220 53 20 5332/20 53322 5 2 5332/2 5332/

ABSTRACT This work aimed at investigating the viability of near infrared spectrometry (NIR), associated with chemometric methods, in order to identify differences at the levels of vigor of naturally and artificially aged soybean seeds. Seeds of six soybean genotypes were analyzed when freshly harvested, after natural aging in storage for eight months, and after artificial aging at the temperature of 41 °C for 96 hours. The seed moisture content, germination potential and vigor were evaluated. Also, there were measured the content of protein, oil and of the fatty acids: palmitic, stearic, oleic, linoleic and linolenic. The NIR spectra were obtained from the freeze-dried and grinded seeds. The natural and artificial aging of the seeds promote deterioration at distinct levels, reflecting in differences in seed vigor. The regions of the electromagnetic spectrum between wavelengths of 1000-1200 nm, 1350-1450 nm, 1800-1900 nm and 2300-2400 nm are important to distinguish the levels of quality of the soybean seeds. The contents of oil and protein have a relationship with the physiological quality of the seeds. Also, the most relevant wavelengths for the classification of seed vigor present a relationship with these compounds. NIR spectroscopy, in combination with chemometric methods, presents potential to be used in the classification of soybean seeds regarding their physiological quality. NIR, , (NIR) methods harvested months 4 C 9 hours evaluated Also acids palmitic stearic oleic linolenic freezedried freeze dried 10001200 1000 1200 1000-120 13501450 1350 1450 1350-145 18001900 1800 1900 1800-190 23002400 2300 2400 2300-240 compounds spectroscopy (NIR 1000120 100 120 1000-12 1350145 135 145 1350-14 1800190 180 190 1800-19 2300240 230 240 2300-24 100012 10 12 1000-1 135014 13 14 1350-1 180019 18 19 1800-1 230024 23 24 2300-2 10001 1 1000- 13501 1350- 18001 1800- 23002 2 2300-

Abstract Bio-high density polyethylene (BHDPE) films with organoclay and antimicrobial additives (zinc pyrithione) were evaluated. The composites were prepared in a single-screw extruder using the melt intercalation technique, and the films were obtained by flat extrusion. The diffractograms indicated the formation of an intercalated nanocomposite (BHDPE/6 wt% of clay). Infrared spectra suggested that the polymer predominates over the antimicrobial agent bands. Thermal stability was slightly reduced by up to 3°C. The clay and antimicrobial agent reduced the melting point and crystallinity of BHDPE by up to 12 °C and 13.3%, respectively. In addition, the presence of clay and antimicrobial agent significantly (p < 0.05) affected all mechanical properties. Proliferation of Staphylococcus aureus demonstrated that both evaluated additives did not significantly (p > 0.05) inhibit microbial growth. The results emphasize a promising application of the films for packaging that does not require antimicrobial control, with films highlighted by 6 wt% of clay. Biohigh Bio high (BHDPE zinc pyrithione singlescrew single screw technique extrusion BHDPE/6 BHDPE6 (BHDPE/ wt . clay) bands 3C C 3 3°C 1 133 13 13.3% respectively addition p 0.05 005 0 05 properties growth control BHDPE/ 13.3 0.0 00 13. 0.

ABSTRACT Hybrid materials formed between polyaniline and layered double hydroxides of Zn and Al (Pani/ZnAlHDL) were obtained by adding previously prepared polyaniline (Pani) to the reaction medium during the synthesis of the HDLs, including HDLs modified with the anionic surfactants sodium dodecyl sulfate and sodium dodecylbenzenesulfonate. The composites exhibited a blue color characteristic of the emeraldine base phase of Pani. X-ray diffraction (XRD) patterns of these compounds showed a shift of the peaks (003) and (006) of ZnAlHDL to lower 2θ values, indicating the presence of both phases in the composites. Additionally, it was observed that the anionic surfactants also influence the structural characteristics of the composites. Fourier-transform infrared (FTIR) spectra support the XRD results. Composites obtained with surfactants were subjected to colorimetric sensor tests for HCl. After only 5 minutes of exposure to HCl vapors, the materials changed their color from blue to green, indicating the formation of the Pani emeraldine salt phase. This indication was confirmed by UV-Vis spectroscopy, as spectra after acid interaction showed new bands in the 400 nm and 820 nm regions, characteristic of the emeraldine salt, the green-colored structural form of Pani. These results demonstrate the feasibility of using these materials in acid sensing, providing a rapid and effective response. Pani/ZnAlHDL PaniZnAlHDL (Pani/ZnAlHDL (Pani dodecylbenzenesulfonate Xray X ray (XRD 003 (003 006 (006 θ values Additionally Fouriertransform Fourier transform FTIR (FTIR vapors green UVVis UV Vis spectroscopy 40 82 regions greencolored colored sensing response 00 (00 4 8 0 (0 (

RESUMO Materiais híbridos formados entre polianilina e hidróxidos duplos lamelares de Zn e Al (Pani/ZnAlHDL) foram obtidos adicionando a Polianilina (Pani) previamente preparada ao meio reacional da síntese dos HDLs e também HDLs modificado com os surfactantes aniônicos dodecilsulfato de sódio e dodecilbenzenosulfato de sódio. Os compósitos apresentaram cor azul que é característica da fase base esmeraldina da Pani. Os difratogramas de raios X destes compostos apresentaram deslocamento dos picos (003) e (006) do ZnAlHDL para menores valores de 2θ, indicando a presença das duas fases nos compósitos. Além disso, foi constatado também que os surfactantes aniônicos também exercem influência nas características estruturais dos compósitos. Os espectros de FTIR corroboram os resultados do DRX. Os compósitos obtidos com os surfactantes foram submetidos à testes de sensor colorimétrico para HCl. Após 5 minutos apenas de exposição aos vapores do HCl, os materiais apresentaram mudança na sua coloração de azul para verde, indicando a formação da fase da Pani, sal esmeraldina. Esse indício foi confirmado por espectroscopia na região do UV-Vis, uma vez que os espectros após interação com ácido, apresentaram novas bandas, nas regiões de 400 nm e 820 nm, que são características do sal esmeraldina, forma estrutural da Pani de coloração verde. Esses resultados mostram a viabilidade da utilização destes materiais no sensoriamento de ambientes ácidos, apresentando resposta rápida e eficaz. Pani/ZnAlHDL PaniZnAlHDL (Pani/ZnAlHDL (Pani 003 (003 006 (006 2θ θ disso DRX HCl verde UVVis, UVVis UV Vis, Vis UV-Vis ácido bandas 40 82 ácidos eficaz 00 (00 4 8 0 (0 (

This is an initial study using infrared (IR) in silico data as a standard database in preliminary method for new synthetic seized drugs. For this purpose, ten of the most common synthetic illicit seized substances on the Brazilian market were compared and computational chemistry was used as a tool for theoretical standard database. Infrared data from standard electronic library, experimental data from seized samples and data simulated by Density Functional Theory (DFT) were evaluated. The feasibility of the method was based on the degree of correlation of evaluated data. The results suggest that the computational methodology can be a viable way to analyze the structures of new synthetic drugs and obtain preliminary infrared profiles. Correlations data indicated a presumptive identification of the analyzed samples and it was also possible to observe a preliminary identification of drugs in five classes. However, it was observed that some synthetic cathinones and phenylethylamines were confused with amphetamines. Therefore, new studies must be developed to optimize the use of these data, because the simulated IR spectra can be advantageous to evaluate the profile of possible substances that may be synthesized in the future. (IR purpose library DFT (DFT profiles classes However amphetamines Therefore future

Abstract Maize (Zea mays L.) is of socioeconomic importance as an essential food for human and animal nutrition. However, cereals are susceptible to attack by mycotoxin-producing fungi, which can damage health. The methods most commonly used to detect and quantify mycotoxins are expensive and time-consuming. Therefore, alternative non-destructive methods are required urgently. The present study aimed to use near-infrared spectroscopy with hyperspectral imaging (NIR-HSI) and multivariate image analysis to develop a rapid and accurate method for quantifying fumonisins in whole grains of six naturally contaminated maize cultivars. Fifty-eight samples, each containing 40 grains, were subjected to NIR-HSI. These were subsequently divided into calibration (38 samples) and prediction sets (20 samples) based on the multispectral data obtained. The averaged spectra were subjected to various pre-processing techniques (standard normal variate (SNV), first derivative, or second derivative). The most effective pre-treatment performed on the spectra was SNV. Partial least squares (PLS) models were developed to quantify the fumonisin content. The final model presented a correlation coefficient (R2) of 0.98 and root mean square error of calibration (RMSEC) of 508 µg.kg-1 for the calibration set, an R2 of 0.95 and root mean square error of prediction (RMSEP) of 508 µg.kg-1 for the test validation set and a ratio of performance to deviation of 4.7. It was concluded that NIR-HSI with partial least square regression is a rapid, effective, and non-destructive method to determine the fumonisin content in whole maize grains. Zea L. L nutrition However mycotoxinproducing mycotoxin producing fungi health timeconsuming. timeconsuming time consuming. consuming time-consuming Therefore nondestructive non destructive urgently nearinfrared near infrared NIRHSI NIR HSI (NIR-HSI cultivars Fiftyeight Fifty eight samples 4 NIRHSI. HSI. 38 (3 20 (2 obtained preprocessing pre processing standard SNV, SNV , (SNV) derivative derivative. . derivative) pretreatment treatment PLS (PLS R (R2 098 0 98 0.9 RMSEC (RMSEC 50 µg.kg1 µgkg1 µgkg µg.kg 1 µg kg µg.kg- 095 95 RMSEP (RMSEP 47 7 4.7 3 ( 2 (SNV (R 09 9 0. 5 kg1 4.

Resumo O milho (Zea mays L.) possui importância socioeconômica por constituir um dos alimentos básicos na nutrição humana e animal. Porém, o cereal é suscetível ao ataque de fungos produtores de micotoxinas que podem causar danos à saúde. Os métodos mais utilizados para detectar e quantificar micotoxinas são caros e demorados e métodos alternativos para a detecção das micotoxinas são uma necessidade. O presente trabalho tem como objetivo utilizar espectroscopia no infravermelho próximo com imagem hiperespectral (NIR-HSI) e análise multivariada de imagens para desenvolver um método rápido e preciso para quantificação de fumonisinas em grãos inteiros de seis cultivares de milho naturalmente contaminadas. Cinquenta e oito amostras, cada uma contendo 40 grãos, foram submetidas ao NIR-HSI e posteriormente divididas em um conjunto de calibração (38 amostras) e um conjunto de predição (20 amostras) com base nos dados multiespectrais obtidos. Os espectros médios foram submetidos a diversas técnicas de pré-processamento (variação normal padrão – SNV, primeira derivada ou segunda derivada). O melhor pré-processamento dos espectros foi SNV e um modelo de mínimos quadrados parciais (PLS) foi desenvolvido para quantificar o teor de fumonisinas. O modelo final apresentou coeficiente de correlação (R2) de 0,98 e raiz quadrada do erro médio quadrático de calibração (RMSEC) de 508 µg.kg-1 para o conjunto de calibração, R2 de 0,95 e raiz quadrada do erro médio quadrático de predição (RMSEP) de 508 µg.kg-1 para o conjunto de validação do teste e relação desempenho/desvio de 4,7. Conclui-se que o NIR-HSI com regressão parcial de mínimos quadrados pode ser um método rápido, eficaz e não destrutivo para determinar o teor de fumonisinas em grãos integrais de milho. Zea L. L animal Porém saúde necessidade NIRHSI NIR HSI (NIR-HSI contaminadas amostras 4 38 (3 20 (2 obtidos préprocessamento pré processamento variação derivada. . derivada) PLS (PLS R (R2 098 0 98 0,9 RMSEC (RMSEC 50 µg.kg1 µgkg1 µgkg µg.kg 1 µg kg µg.kg- 095 95 RMSEP (RMSEP desempenhodesvio desempenho desvio 47 7 4,7 Concluise Conclui se 3 ( 2 (R 09 9 0, 5 kg1 4,

ABSTRACT: Near-infrared (NIR) spectroscopy is a promising tool for optimizing seed analyses quickly and assertively. The aim of this study was to investigate the viability of NIR in association with chemometric methods in classification of soybean seed lots regarding their physiological potential. We evaluated 372 soybean seed lots for vigor and obtained NIR spectra from seed samples. The original spectra were pre-processed by the following methods: Standard Normal Variate (SNV), SNV + 1st and 2nd derivatives, Gap-segment derivative, and Savitzky-Golay for the first- and second-degree derivatives, as well as combinations of the methods. The lots were divided into Class I (≥ 85% germination after accelerated aging) and Class II (< 85% germination after accelerated aging); and the pre-processed spectra were used to build classification models through the following methods: K-nearest neighbors (KNN), Partial Least Squares - Discriminant Analysis (PLS-DA), Naive Bayes (NB), Random Forest (RF), and Support Vector Machine (SVM). The PLS-DA model showed greater classification accuracy and kappa, followed by SVM. The lowest accuracy values were obtained for the NB and RF models. The regions between the wavelengths 1,000-1,200 nm and 2,200-2,500 nm were the most important for distinguishing the quality levels of soybean seeds. ABSTRACT Nearinfrared Near infrared (NIR assertively potential 37 samples preprocessed pre processed SNV, , (SNV) st nd derivatives Gapsegment Gap segment derivative SavitzkyGolay Savitzky Golay first seconddegree second degree ≥ ( 85 aging < Knearest K nearest KNN, KNN (KNN) PLSDA, PLSDA PLS DA (PLS-DA) NB, (NB) RF, (RF) SVM . (SVM) kappa 1,0001,200 10001200 1,000 1,200 1 000 200 1,000-1,20 2,2002,500 22002500 2,200 2,500 2 500 2,200-2,50 seeds 3 (SNV 8 (KNN (PLS-DA (NB (RF (SVM 0001 1,0001,20 1000120 1000 1,00 1200 1,20 00 20 1,000-1,2 2002 2,2002,50 2200250 2200 2,20 2500 2,50 50 2,200-2,5 1,0001,2 100012 100 1,0 120 1,2 0 1,000-1, 2,2002,5 220025 220 2,2 250 2,5 5 2,200-2, 1,0001, 10001 10 1, 12 1,000-1 2,2002, 22002 22 2, 25 2,200-2 1,0001 1,000- 2,2002 2,200-

RESUMO: A espectroscopia no infravermelho próximo (NIR) consiste em uma ferramenta promissora para otimização das análises de sementes de forma rápida e assertiva. Este trabalho teve como objetivo investigar a viabilidade do NIR, associado a métodos quimiométricos, para classificar lotes de sementes de soja quanto ao potencial fisiológico. Foram utilizados 372 lotes de sementes de soja avaliados quanto ao vigor e obtidos espectros NIR das amostras de sementes. Os espectros originais foram submetidos aos métodos de pré-processamento Standard Normal Variate (SNV), SNV + 1ª e 2ª derivadas; Gap-segment derivative; e Savitzky-Golay, pelas derivadas de primeiro e segundo grau, e a combinação entre os métodos. Os lotes foram divididos em Classe I (≥ 85% de germinação após envelhecimento acelerado), Classe II (< 85% de germinação após envelhecimento acelerado) e os espectros pré-processados foram utilizados para a construção de modelos de classificação por meio dos métodos K-nearest neighbors (KNN), Partial Least Squares - Discriminant Analysis (PLS-DA), Naive Bayes (NB), Random Forest (RF) e Support Vector Machine (SVM). O modelo de classificação PLS-DA apresentou maior acurácia e kappa, seguido pelo SVM. Os menores valores de acurácia foram obtidos para os modelos NB e RF. As regiões entre os comprimentos de ondas 1.000-1.200 nm e 2.200-2.500 nm foram as mais importantes para distinguir os níveis de qualidade das sementes de soja. RESUMO (NIR assertiva quimiométricos fisiológico 37 préprocessamento pré processamento SNV, , (SNV) ª Gapsegment Gap segment derivative SavitzkyGolay, SavitzkyGolay Savitzky Golay, Golay Savitzky-Golay grau ≥ ( 85 acelerado, acelerado < préprocessados processados Knearest K nearest KNN, KNN (KNN) PLSDA, PLSDA PLS DA (PLS-DA) NB, (NB) RF (RF SVM . (SVM) kappa 1.0001.200 10001200 1.000 1.200 1 000 200 1.000-1.20 2.2002.500 22002500 2.200 2.500 2 500 2.200-2.50 3 (SNV 8 (KNN (PLS-DA (NB (SVM 0001 1.0001.20 1000120 1000 1.00 1200 1.20 00 20 1.000-1.2 2002 2.2002.50 2200250 2200 2.20 2500 2.50 50 2.200-2.5 1.0001.2 100012 100 1.0 120 1.2 0 1.000-1. 2.2002.5 220025 220 2.2 250 2.5 5 2.200-2. 1.0001. 10001 10 1. 12 1.000-1 2.2002. 22002 22 2. 25 2.200-2 1.0001 1.000- 2.2002 2.200-

We report a quantum chemical study of cryptolepine, an alkaloid that is of considerable pharmacological interest. We focus on solvent effects, spectroscopic properties and on chemical reactivity descriptors, such as electronegativity, hardness, and electrophilicity. On the density functional level, gas phase ¹H and 13C nuclear magnetic resonance chemical shifts and infrared spectra agree well with experiments, although the dipole moment increases significantly with an increasing polarity of the solvent. We characterize normal modes using a potential energy distribution scheme. In the gas phase and in solution, the UV-Vis spectra are computed using time-dependent density functional theory. Here, major discrepancies between experiment and theory can only be observed in the visible range.

Summary: A retrospective-prospective research was carried out to establish a soil quality index (SQI) of Los Rios region (RR), Tabasco, Mexico, and its modeling with the near infrared technology (NIR) and chemometrics. The SQI was determined with the OM / (clay + silt) relationship to evaluate the Cambisol soils of RR. The OM percentage and the SQI were compared to define the best soil quality qualifier. Based on the SQI, 58% of the soils in RR exhibit degradation, while only 14% indicates a low concentration of OM. Therefore, we conclude that the SQI is more sensitive to quantify soil degradation compared to the evaluation based on OM. A sustainable soil management program and soil practices adapted to local environmental, social and economic conditions are recommended to increase OM and improve SQI. With the SQI, a classification model was established using near-infrared spectroscopy and chemometrics. The spectra of each soil sample were recorded and through chemometric interpretation, it was shown that it is possible to conduct a partial least squares discriminant analysis model (PLS-DA) to predict the SQI. The model meets all statistical qualifiers and correctly predicts the SQI in 100% of cases. We conclude that the NIR technology provides sufficient information to predict the SQI with the advantage of eliminating the consumption of reagents, no laboratory waste is generated, the analysis time is reduced to minutes, and the sample under study is not destroyed. In addition, the procedure is simple as it consists of drying, grinding and sieving the soil samples to assess the structural quality of the soil.

Resumen: Se realizó una investigación retrospectiva - prospectiva, para establecer un índice de calidad de los suelos (ICS) de la región de los Ríos (RR) en Tabasco, México y su modelación con la tecnología de infrarrojo cercano (NIR) y la quimiometría. Con la relación MO / (arcilla + limo) se estableció el ICS para evaluar los suelos Cambisoles de la RR. El porcentaje de MO y el ICS fueron comparados para definir el mejor calificador de la calidad de los suelos. Con base en el ICS, el 58% de los suelos de la RR presentan degradación, mientras que, solo el 14% de los suelos indican que presentan baja concentración de MO. Por lo que se concluye que el ICS es más sensible para cuantificar la degradación de los suelos cuando se comparó con la evaluación basada en la MO. Se recomienda un programa de manejo sostenible del suelo y prácticas edafológicas adaptadas a las condiciones locales, ambientales, sociales y económicas, para incrementar la MO y mejorar el ICS. Con el ICS se estableció un modelo de clasificación mediante espectroscopía de infrarrojo cercano y quimiometría. Se registraron los espectros de cada muestra de suelo y mediante interpretación quimiométrica se demostró que es posible establecer un modelo de análisis discriminante por mínimos cuadrados parciales (PLS-DA) para predecir el ICS. El modelo cumple con todos los calificadores estadísticos y predice correctamente el ICS en el 100% de los casos. Se concluye que la tecnología NIR genera información suficiente para predecir el ICS; con la ventaja de, eliminar el consumo de reactivos, no se generan residuos de laboratorio, se reduce el tiempo de análisis a minutos y no se destruye la muestra en estudio. Y solo se necesita secar, moler y tamizar las muestras de suelos para evaluar la calidad estructural de suelos.

Parkinson’s disease is a neurodegenerative disorder characterized by progressive loss of dopaminergic neurons. There is substantial evidence that the endocannabinoid system modulates the dopaminergic activity in the basal ganglia, a forebrain system that integrates cortical information to coordinate motor activity regulating signals. In this article, a fused-silica capillary with a molecularly imprinted polymer was developed for in-tube solid-phase microextraction of the endocannabinoid anandamide in plasma samples from Parkinson’s disease patients and further analysis by ultra-high-performance liquid chromatography with tandem mass spectrometry. The molecularly imprinted polymer capillary presented recognition sites with complementary shape, size, and functionality to anandamide. Scanning electron micrographs and Fourier transform infrared spectra illustrated the physical and chemical modification of the printed and non-printed capillary surface. The in-tube solid-phase microextraction ultra-high-performance liquid chromatography with tandem mass spectrometry method presented a linear range from 0.1 to 20 ng mL-1, precision with coefficient of variation values ranging from 1.2 to 13%, and relative standard deviation accuracy ranging from -3.6 to 7.5%. The method developed herein can adequately determine anandamide in plasma samples from Parkinson’s disease patients. By applying the standard addition approach, the anandamide plasmatic concentration in these samples was found to range from 0.2 to 0.4 ng mL-1. Parkinsons Parkinson s neurons ganglia signals article fusedsilica fused silica intube tube solidphase solid phase ultrahighperformance ultra high performance shape size nonprinted non surface 01 0 1 0. 2 mL1, mL1 mL 1, mL-1 12 1. 13 13% 3.6 36 3 6 -3. 75 7 5 7.5% approach 02 04 4 mL1. mL- 3. -3 7.5 - 7.

ABSTRACT Generally, the taxonomic classification of cocoa beans is based on the theobromine/caffeine ratio determined using high-performance liquid chromatography (HPLC). However, this technique involves laborious and time-consuming calculations. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy is a valuable, effective, and rapid tool for analyzing the chemical composition of food products. The objective of this study was to examine the potential of ATR-FTIR combined with chemometric tools such as principal component analysis (PCA), linear discriminant analysis (LDA), and partial least squares regression-discriminant analysis (PLS-DA) to discriminate between the Trinitario and Forastero dry bean cocoa varieties defined by theobromine and caffeine measurements via HPLC. The cocoa varieties were evaluated using HPLC analysis of 36 dry cocoa bean samples to determine the theobromine/caffeine ratio. Moreover, ATR-FTIR spectra were analyzed in the mid-infrared (MIR) region, and signals associated with theobromine and caffeine were identified and analyzed using the LDA and PLS-DA models. The LDA and PLS-DA models allowed the satisfactory differentiation between cocoa varieties, providing overall prediction capacity values of 98.2 ± 1.8% and 96.1 ± 2.4%, respectively. The results show the potential of ATR-FTIR spectroscopy for the reliable, fast, and easy differentiation of dried cocoa beans. Generally theobrominecaffeine highperformance high performance . (HPLC) However timeconsuming time consuming calculations ATRFTIR ATR FTIR (ATR-FTIR valuable effective products PCA, PCA , (PCA) LDA, (LDA) regressiondiscriminant regression PLSDA PLS DA (PLS-DA 3 Moreover midinfrared mid MIR (MIR region 982 98 2 98. 18 1 8 1.8 961 96 96. 24 4 2.4% respectively reliable fast (HPLC (PCA (LDA 9 1. 2.4 2.

RESUMO Geralmente, a classificação taxonômica das sementes de cacau foi feita pela relação teobromina/cafeína por cromatografia líquida de alto desempenho (HPLC). No entanto, esta técnica envolve determinações laboriosas e demoradas; assim, a espectroscopia atenuada de infravermelho de reflexão total (ATR-FTIR) é uma ferramenta valiosa, eficaz e rápida para analisar a composição química dos produtos alimentares. Neste estudo, o objetivo era examinar o potencial da ATR-FTIR combinado com ferramentas quimiométricas como a análise de componentes principais (PCA), a análise discriminante linear (LDA), e a análise menos regressiva quadrada parcial (PLS-DA) examinada para a discriminação entre as variedades de cacau Trinitario e Forastero definidas pelas medições de teobromina e cafeína via HPLC. As variedades de cacau foram avaliadas pela análise por HPLC de 36 amostras de grãos de cacau secos para a relação teobromina/cafeína. Além disso, os espectros ATR-FTIR foram analisados em regiões de infravermelhos médios (MIR), e os sinais associados à teobromina e à cafeína foram identificados e analisados através dos modelos LDA e PLS-DA. Os modelos LDA e PLS-DA proporcionaram uma discriminação satisfatória do cacau, fornecendo valores de capacidade de previsão global de 98.2 ± 1.8% e 96.1 ± 2.4%, respectivamente. Os resultados mostram o potencial da técnica de espectroscopia ATR-FTIR para uma diferenciação fiável, rápida e fácil das amêndoas de cacau secas. Geralmente teobrominacafeína . (HPLC) entanto demoradas assim ATRFTIR ATR FTIR (ATR-FTIR valiosa alimentares estudo PCA, PCA , (PCA) LDA, (LDA) PLSDA PLS DA (PLS-DA 3 disso MIR, MIR (MIR) PLSDA. DA. 982 98 2 98. 18 1 8 1.8 961 96 96. 24 4 2.4% respectivamente fiável secas (HPLC (PCA (LDA (MIR 9 1. 2.4 2.

5-Hydroxymethylfurfural (HMF) can be obtained from the dehydration of monosaccharides present in biomass, which helps add value to the raw material. The present work sought to study the relationship between the parameters of biomass characterization, including the content of reducing sugars, total soluble solids and the mid-infrared (MIR) and near-infrared (NIR) spectra, and the formation of HMF after synthesis. A thorough analysis was conducted in order to evaluate the residual agricultural biomass samples from sugarcane bagasse, corn stover, cassava branch, banana pseudostem and mango fruits after the drying (45 °C maximum) and ball mill grinding pre-processing procedure. HMF synthesis was performed using 0.50 mol L-1 HCl and n-butanol as extracting solvent. The analytical quantification of HMF and furfural (co-product of synthesis) was performed using high-performance liquid chromatography coupled to diode-array detector (HPLC-DAD). The highest efficiency of the synthesis of HMF was observed for the mango fruits (55.0 kg ton-1) and sugarcane bagasse biomass (47.5 kg ton-1) samples. The application of data fusion and principal component analysis (PCA) allowed us to identify the samples with greater potential for HMF synthesis. 5Hydroxymethylfurfural Hydroxymethylfurfural 5 (HMF material characterization sugars midinfrared mid infrared MIR (MIR nearinfrared near NIR (NIR spectra stover branch 45 (4 C maximum preprocessing pre processing procedure 050 0 50 0.5 L1 L 1 L- nbutanol n butanol solvent coproduct co product highperformance high performance diodearray diode array HPLCDAD. HPLCDAD HPLC DAD . (HPLC-DAD) 55.0 550 55 (55. ton1 ton ton-1 47.5 475 47 (47. PCA (PCA 4 ( 05 0. (HPLC-DAD 55. (55 ton- 47. (47 (5

The aim of this study was to produce and to characterize dietary fiber concentrates (DFCs) obtained from the peach palm by-product (PPB). Subcritical water extraction (SWE) and aqueous extractions at low pressure in magnetic (LPMS) and orbital (LPOS) stirring were carried out to DFCs production. DFCs and the untreated PPB were analyzed for composition, functional properties, scanning electron microscopy and infrared spectroscopy. The aqueous extraction treatments increased the total dietary fiber content, due to the removal of sugars (88.7-99.6%) and the partial leaching of proteins and ashes. The DFC obtained by SWE had the highest content of soluble and insoluble dietary fiber. The methods of aqueous extraction changed the structure of fiber components, that becomes more porous and fragmented, improving the functional properties, as water and oil absorption. Cellulose was the most abundant component of the samples and the alteration in its conformation was observed in the infrared spectra. The principal component analysis showed that the changes on the composition and functional properties were associated with the treatments applied. DFCs produced in this work, specially by SWE, are considered interesting alternatives to promote the utilization of peach palm by-product as a fiber-rich component. (DFCs byproduct product PPB. . (PPB) (SWE LPMS (LPMS LPOS (LPOS production spectroscopy 88.799.6% 887996 88.7 99.6% 88 7 99 6 (88.7-99.6% ashes components fragmented absorption spectra applied work fiberrich rich (PPB 799 88.799.6 88799 887 88. 996 99.6 8 9 (88.7-99.6 79 88.799. 8879 99. (88.7-99. 88.799 (88.7-99 88.79 (88.7-9 (88.7- (88.7 (88. (88 (8 (

Resumen: Se prepararon mezclas ácido poliláctico (PLA) - almidón de achira empleando polivinil alcohol (PVA) y glicerol como compatibilizante y plastificante, respectivamente. Las mezclas fueron caracterizadas en términos de espectroscopia infrarroja por transformadas de Fourier (FTIR), calorimetría diferencial de barrido (DSC), y propiedades mecánicas. Las superficies de fractura obtenidas del ensayo de tensión fueron evaluadas por medio de microscopía electrónica de barrido (SEM). Adicionalmente, se determinó la biodegradabilidad de las mezclas por medio de ensayos en suelo natural, vermicomposteo, así como también en condiciones aerobias y anaerobias. De acuerdo con los resultados, el PVA incrementó la resistencia a la tensión, elongación a la rotura y produjo una disminución en el módulo de Young. Las imágenes SEM exhibieron superficies rugosas con gránulos de almidón. Adicionalmente, los resultados de DSC evidenciaron un solo valor de Tg, muy cercana a la Tg de los componentes solos; en tanto que los espectros FTIR sugirieron la presencia de enlace hidrógeno entre PLA y almidón. Finalmente, los resultados de vermicomposteo revelaron un alto nivel de degradación de las mezclas PLA - almidón de achira.

Abstract: Polylactic acid (PLA) - achira starch blends were prepared using polyvinyl alcohol (PVA) and glycerol as compatibilizer and plasticizer, respectively. Blends were characterized through Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and mechanical behavior. Fracture surfaces obtained from tensile test were evaluated by scanning electron microscopy (SEM). In addition, biodegradability of blends was determined in natural soil, vermicomposting method, aerobic and anaerobic conditions. According to results, PVA increased tensile strength, elongation at break and decreased Young´s modulus. SEM images showed rugged surfaces with starch granules in the samples. Moreover, DSC results showed a single Tg value close to Tg of neat components whereas, FTIR spectra suggested the presence of hydrogen bonds between PLA and starch. Finally, vermicomposting results revealed a high degradation level of PLA - achira starch blends.