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OBJECTIVE: This study aimed to develop and validate a rapid, simple, accurate and precise analytical method for the quantification of L-AA in vitamin C serums. Moreover, the developed method was further applied to determine L-AA in eight different brands of vitamin C serums. A complementary study was also carried out to evaluate the stability of L-AA in the vitamin C serum samples after 15, 30, 45 and 60 days of storage at ambient temperature (15-35°C). METHODS: Ultra-high-performance liquid chromatography-tandem mass spectrometry was applied. RESULTS: Quantitative analyses were performed with a total chromatographic run time of 1.5 min by matrix-matched calibration, and the analytical curve was linear over the range of 1-1700 µg L-1 with a correlation coefficient of 0.9998. The limits of detection (LOD) and quantification (LOQ) were 0.3 and 1.0 µg L-1 , respectively. Intra- and inter-assay precisions, expressed in terms of relative standard deviation, ranged from 0.3% and 2.2%, respectively, and recoveries in concentration levels of 1 and 5 µg L-1 were 103.9% and 101.2%, respectively. The proposed analytical method was successfully applied to determine the L-AA content in eight commercial vitamin C serum samples. The stability of the target analyte in samples stored at ambient temperature (15-35°C) was evaluated throughout 60 days with a 15-day interval between analyses. At 0 days, L-AA content in samples ranged from 1.05 to 169.91 mg L-1 , which decreases over time. CONCLUSION: The proposed method could be powerful in routine analyses to ensure the quantification of L-AA in vitamin C serums since it proved to be a simple, reliable, fast, precise, accurate and sensitive analytical method.
OBJECTIF: Cette étude visait à développer et valider une méthode analytique rapide, simple, exacte et précise pour la quantification de l'acide L-ascorbique dans les sérums à la vitamine C. De plus, la méthode développée a été appliquée pour déterminer l'acide L-ascorbique dans huit différentes marques de sérums à la vitamine C. Une étude complémentaire a également été réalisée pour évaluer la stabilité de l'acide L-ascorbique dans les échantillons de sérum à la vitamine C après 15, 30, 45 et 60 jours de conservation à température ambiante (15 à 35 °C). MÉTHODES: La chromatographie en phase liquide à haute performance avec spectrométrie de masse en tandem a été employée. RÉSULTATS: Des analyses quantitatives ont été réalisées avec une durée totale d'exécution chromatographique de 1,5 minute par calibration matricielle appariée, et la courbe analytique était linéaire sur la plage de 1 à 1700 µg L-1 avec un coefficient de corrélation de 0,9998. La limite de détection (LD) et la limite de quantification (LQ) ont été déterminées à 0,3 et 1,0 µg L−1 , respectivement. Les précisions intra- et inter-essais, exprimées en termes d'écart-type relatif, étaient de 0,3 % et 2,2 %, respectivement, et les récupérations aux niveaux de concentration de 1 et 5 µg L-1 étaient de 103,9 % et 101,2 %, respectivement. La méthode analytique proposée a été employée avec succès pour déterminer la teneur en acide L-ascorbique de huit échantillons de sérum à la vitamine C commerciaux. La stabilité de l'analyte cible dans les échantillons conservés à température ambiante (15 à 35 °C) a été évaluée sur 60 jours avec un intervalle de 15 jours entre les analyses. À 0 jour, la teneur en acide L-ascorbique dans les échantillons était comprise entre 1,05 et 169,91 µg L-1 , ce qui diminue au fil du temps. CONCLUSION: La méthode proposée pourrait être puissante dans les analyses de routine pour assurer la quantification de l'acide L-ascorbique dans les sérums à la vitamine C puisqu'elle s'est avérée être une méthode analytique simple, fiable, rapide, précise, exacte et sensible.
Assuntos
Ácido Ascórbico , Espectrometria de Massas em Tandem , Cromatografia Líquida de Alta Pressão/métodos , Limite de DetecçãoRESUMO
This study evaluated the fatty acid composition and the nutritional profile of Brycon cephalus and Brycon microlepis, fish species from the central Amazon basin, by different methods of quantification. The methods applied were: area normalization (MAN), internal standard (MIS), alternative theoretical (MAT) and alternative experimental (MAE). Significant differences were observed between the methods applied and the species studied. MAN supplied poor information about fatty acids composition and diet formulation, presenting only fatty acid profiles. MIS, MAT and MAE supplied fatty acids composition information on a mass basis. MAT and MAE overestimated results, whereas MIS presented the most accurate results. B. cephalus and B. microlepis showed high contents of approximately 65 mg g-1 of n-3 fatty acids. Eicosapentaenoic acid (EPA; 20:5n-3) and docosahexaenoic acid (DHA; 22:6n-3) content totaled, 104.37 mg 100 g-1 and 117.89 mg 100 g-1 for B. cephalus and B. microlepis, respectively. The nutritional profile of both fish species showed favorable indices for nutritional quality of the lipid fraction, indicating that both Brycon species are healthy dietary choices.
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Human milk (HM) is essential for newborns' food, but its low storage stability is a limiting factor so that microencapsulation may stabilize and protect compounds sensitive to degradation. This study investigated the action of maltodextrin and gum arabic on freeze-dried HM concerning its quality and solubility. Microencapsulation was evidenced by morphology, and all samples presented high encapsulation efficiency (>85 %), proving to be an efficient process. Furthermore, specific signals in the Fourier-Transform Infrared (FTIR) spectra indicate the interactions between the coating materials and the HM matrix. Gum arabic improved the reconstitution properties of freeze-dried HM (higher solubility, 3 % on average, and lower dissolution time, around 80 %), elucidating its high stabilization capacity, even at low concentrations (5 and 10 %). Despite the best results reached by gum arabic, the addition of maltodextrin proved effective; in other words, its low stabilization capacity enables combinations with gum arabic. A lower polidispersibility (difference of 20 % between samples: control and containing gum arabic) was also observed, which means that the encapsulated samples were more homogeneous. Therefore, through the analysis performed, we recommend using gum arabic alone or with maltodextrin to obtain HM microcapsules with a good quality of reconstitution.
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Goma Arábica , Leite Humano , Recém-Nascido , Humanos , Solubilidade , Cápsulas , PolissacarídeosRESUMO
Amoxicillin is a pharmaceutical compound that is not degraded in wastewater treatment plants, causing harm to the environment. In this work, an iron nanoparticle (IPP) was synthesized using pumpkin (Tetsukabuto) peel extract for the degradation of amoxicillin under UV light. The IPP was characterized using scanning electron microscopy/energy dispersive x-ray spectroscopy, transmission electron microscopy, X-ray diffraction, Fourier-transform infrared spectroscopy, thermogravimetric analysis, and Raman spectroscopy techniques. The photocatalytic efficiency of IPP was analyzed by investigating the effect of IPP dosage (1-3 g L-1), initial amoxicillin concentration (10-40 mg L-1), pH (3-9), reaction time (10-60 min), and the effect of inorganic ions (1 g L-1). The optimum conditions for the maximum photodegradation removal (≈60%) were IPP = 2.5 g L-1, initial amoxicillin concentration = 10 mg L-1, pH = 5.6, and irradiation time = 60 min. The results of this study showed that inorganic ions (Mg2+, Zn2+, and Ca2+) negatively affect the photodegradation of amoxicillin by IPP; the quenching test showed that hydroxyl radical (OHâ¢) is the primary reactive species of the reaction; NMR analysis revealed changes in amoxicillin molecules after photoreaction; the subproducts of photodegradation were identified by LC-MS; the proposed kinetic model demonstrated good applicability, predicting the behavior of OH⢠and determining the kinetic constant, and the cost analysis based on required energy (238.5 kWh m-3 order-1) indicated that the amoxicillin degradation method by IPP is economically viable. This study developed a new efficient iron nanocatalyst for the removal of antibiotics from aqueous environments and provided optimal conditions and relevant information in the area of advanced oxidative processes.
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Amoxicilina , Cucurbita , Ferro , Antibacterianos/química , Microscopia Eletrônica de Varredura , CatáliseRESUMO
BACKGROUND & AIMS: The present study evaluated the lipid profile of enteral nutrition formulas with added fish oil used in a public hospital, with an emphasis on the fatty acid (FA) composition. METHODS: FA composition was determined using gas chromatography coupled to a flame ionization detector (GC-FID). Nine enteral nutrition formulas were evaluated and the results obtained were compared with those reported on the formulas labels. RESULTS: The sample with the highest percentage of added fish oil according to the label information had the lowest total amounts of eicosapentaenoic acid and docosahexaenoic acid (EPA + DHA) (p < 0.05). In the evaluation of the total amount of polyunsaturated fatty acids/saturated fatty acids (ΣPUFA/ΣSFA) ratio, five samples were not within the values recommended by Brazilan and international health regulatory agencies. Regarding the n-6/n-3 fatty acids ratio, five samples showed values higher than the recommended ratio. It was observed that EPA + DHA content was positively correlated with the cost of the diet. Importantly, we also found that there was a significant difference between the results of our analysis and the descriptions found on the labels for fatty acids n-6, n-3, EPA, DHA, SFA, PUFA and MUFA. CONCLUSIONS: We conclude that the discrepancies for fatty acids between the values obtained in the analyses and the values reported on the labels highlight the need for more rigorous inspection when public hospitals purchase enteral nutrition formulas with added fish oil, since the administration of formulas with inadequate levels of FA in hospitalized patients can compromise clinical results during the hospitalization period.
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Ácidos Graxos Ômega-3 , Óleos de Peixe , Humanos , Nutrição Enteral , Ácido Eicosapentaenoico , Ácidos Graxos , Ácidos Docosa-Hexaenoicos , Hospitais PúblicosRESUMO
The effect of the use of Nilo tilapia filleting residues in the production of pâtés with the addition of oregano essential oil stored for 90 days at 4 °C was evaluated. For that, 5 treatments were performed as follows: TSA-control treatment; TES with the addition of sodium erythorbate; and formulation TOE1 with 600 ppm oregano essential oil; TOE2 with 1000 ppm essential oil; and TOE3 with 1400 ppm essential oil. The pâtés showed adequate technological and physicochemical characteristics and microbiological counts within the legislation standards. No significant differences were observed in the luminosity of the pâté formulations during storage, and the addition of oil contributed to the increase in a* values and stability of b* values. Regarding the lipid and protein oxidation, TOE3 showed lower values at the end of the shelf-life. The addition of essential oil did not affect the hardness and cohesiveness of the products. The fatty acids in greater amounts in the samples were linoleic, oleic, palmitic, and stearic acids. The analysis of biogenic amines indicated that only the treatments with the highest amounts of sodium erythorbate (TES and TOE1) showed losses of spermidine. It was observed that decreasing the inclusion of sodium erythorbate and increasing the inclusion of oregano essential oil resulted in a drop in cadaverine values. A total of 46 volatile compounds were detected in the samples with the highest amount of free fatty acids and all the formulations were well accepted sensorially.
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Ciclídeos , Óleos Voláteis , Origanum , Animais , Origanum/química , Conservação de Alimentos/métodos , Embalagem de Alimentos/métodosRESUMO
Orange fruit is one of the most popular types of fruit in the world, and its juice is the main product of its processing. This study aimed to evaluate a simple, fast, and eco-friendly methodology, atmospheric solids analysis probe mass spectrometry (ASAP-MS), to assess the chemical profile of four oranges varieties (Valencia, Folha Murcha, Pera, and Iapar). The oranges' varieties were evaluated for the physicochemical composition (extraction yield, pH, total titratable acidity, total soluble solids [TSS], °Brix), ratio (TSS/TA), and bioactive compounds (ASAP-MS analysis). The characterization of oranges resulted in great values of oranges yield according to the varieties (44.00-48.10% [w/w], adequate and characteristic acidity [0.73-1.35%], soluble solids content (10.24-13.80°Brix), pH (3.30-3.96), and ratio (7.59-19.90) level for this fruit. This powerful method showed that all analysis procedures were simple, fast, and easy because there is no need to prepare the sample and the analysis time lasted 2 min. Besides, results obtained exhibited a vast array of chemical groups. Principal component analysis (PCA) defined and distinguished the varieties of the orange. Therefore, ASAP-MS and PCA showed that they are very attractive candidates for routine analysis to monitor the varieties of the orange with its pronounced advantages, besides being contributing to the environment because it does not use any quantities of organic solvents. This methodology was applied for the first time to this type of sample.
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Citrus sinensis , Citrus sinensis/química , Frutas/química , Sucos de Frutas e Vegetais , Espectrometria de Massas , Análise de Componente PrincipalRESUMO
The direct methylation method developed in this work for coffee samples allowed the determination of fatty acids using smaller sample amounts (100 mg), lower solvent volumes (5 mL) and shorter experimental run time (~12 min). Hence, the experiments are more economical and collaborate with green chemistry, besides favoring the health of the analyst who handles a smaller amount of solvents in a short period. Design Expert software was employed to determine the optimal concentration of the acid and base (0.7 e 1.75 molL-1) and evaluate the sonication time (5 min for both procedures). The experiments were carried out on different coffee samples in which the fat content ranging from 10.18% to 14.86%. The relative standard deviation values for intraday and interday were 2.78% and 7.8%, respectively, confirming the good precision of the proposed method for fatty acid derivatization.
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Café , Ácidos Graxos , Cromatografia Gasosa/métodos , Ácidos Graxos/química , Metilação , Solventes/químicaRESUMO
This work has proposed the application of optimized dispersive liquid-liquid microextraction (DLLME) in order to extract acrylamide from brewed coffee samples for its subsequent determination by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). DLLME achieved superior results employing 300⯵L of brewed coffee, 100⯵L of dichloromethane, 400⯵L of acetonitrile and without sodium chloride addition. Quantitative analyses were carried out by the standard addition method, and the limits of detection and quantification were 0.9 and 3.0⯵gâ¯L-1, respectively. Recoveries ranged from 97 to 106%, and the intra- and inter-assay precisions ranged from 6 to 9%. The proposed analytical method was applied to seventeen brewed coffee samples prepared in a filter coffee maker, and acrylamide amounts varied from 10.5 to 28.5⯵gâ¯L-1. Therefore, the suggested DLLME-UPLC-MS/MS method is promising for routine analysis in order to guarantee the quality control of acrylamide in brewed coffee.