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This study aimed to obtain and characterize an oil-in-water nanoemulsion (NE) loaded with an in vitro optimized bactericidal essential oil blend of 50% oregano, 40% thyme, and 10% lemongrass and to evaluate its potential at three different concentrations (0.5%, 1%, and 2%) in the inactivation of Escherichia coli, Staphylococcus aureus, and Salmonella enterica serotype Enteritidis inoculated in rainbow trout fillets stored at 4 °C for 9 days. Regarding the NE, the nanometric size (<100 nm) with low polydispersion (0.17 ± 0.02) was successfully obtained through ultrasound at 2.09 W/cm2. Considering the three concentrations used, S. Enteritidis was the most susceptible. On the other hand, comparing the concentrations used, the NE at 2% showed better activity, reducing S. Enteritidis, E. coli, and S. aureus by 0.33, 0.20, and 0.73 log CFU/g, respectively, in the trout fillets. Thus, this data indicates that this is a promising eco-friendly alternative to produce safe fish for consumption and reduce public health risks.
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This study aimed to obtain optimized mixture with three essential oils (EOs) for maximum antioxidant activity through the augmented simplex-centroid mixture design and evaluate the effect of this optimized blend on total aerobic psychrotrophic count (TAPC), lipid and protein oxidation, instrumental color parameters and texture profile in rainbow trout fillets at refrigerated storage for nine days. Considering the DPPH and FRAP assays, the ideal EO blend was 66% lemongrass and 34% oregano. During refrigerated storage, this blend at 2000 ppm was equally effective as BHT (100 ppm) (p > 0.05), mitigating the discoloration (a* and b*), lipid, and protein oxidation in 38.83%, 12.95%, 76.13%, and 35.13%, respectively, besides shows greater effectiveness for preserving texture changes (p < 0.05) and extending the shelf life in 13 h. The lemongrass + oregano EO blend reveals a promising natural alternative to enhance the quality of rainbow trout fillets under refrigerated storage. Furthermore, the multiresponse optimization showed to be a strong ally in enabling the use of these EOs by food industries.
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Óleos Voláteis , Oncorhynchus mykiss , Animais , Antioxidantes/farmacologia , Emulsões , ÁguaRESUMO
This study aims to investigate the effects of canning variables (cooking time, storage time, volume of vinegar, salt and sugar) on the mineral composition of canned cowpea (Vigna unguiculata (L.) Walp) and which conditions provide optimised preservation of the mineral content of the grains. Different formulations of canned cowpeas were produced following two levels factorial experimental design using five variables. A set of 11 different formulations were evaluated using the desirability function with essential minerals (Ca, Cu, Fe, Mn, Mg, P and Zn) as the response. The optimal multi-response conditions for higher mineral retention were: 360 days of storage at 30 ± 5 °C (ST2), 30 ml of vinegar, 9.0â g of NaCl, 18 min of cooking time, and 9.0â g, 19.5â g or 30 g of sugar (the effect of the sugar content at the evaluated range was not significant at 95% confidence level).
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Vigna , Ácido Acético , Carboidratos , Minerais/análise , AçúcaresRESUMO
Plant-based materials are an important source of bioactive compounds (BC) with interesting industrial applications. Therefore, adequate experimental strategies for maximizing their recovery yield are required. Among all procedures for extracting BC (maceration, Soxhlet, hydro-distillation, pulsed-electric field, enzyme, microwave, high hydrostatic pressure, and supercritical fluids), the ultrasound-assisted extraction (UAE) highlighted as an advanced, cost-efficient, eco-friendly, and sustainable alternative for recovering BC (polyphenols, flavonoids, anthocyanins, and carotenoids) from plant sources with higher yields. However, the UAE efficiency is influenced by several factors, including operational variables and extraction process (frequency, amplitude, ultrasonic power, pulse cycle, type of solvent, extraction time, solvent-to-solid ratio, pH, particle size, and temperature) that exert an impact on the molecular structures of targeted molecules, leading to variations in their biological properties. In this context, a diverse design of experiments (DOEs), including full or fractional factorial, Plackett-Burman, Box-Behnken, Central composite, Taguchi, Mixture, D-optimal, and Doehlert have been investigated alone and in combination to optimize the UAE of BC from plant-based materials, using the response surface methodology and mathematical models in a simple or multi-factorial/multi-response approach. The present review summarizes the advantages and limitations of the most common DOEs investigated to optimize the UAE of bioactive compounds from plant-based materials.
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Antocianinas , Polifenóis , Flavonoides , Extratos Vegetais/química , Solventes/químicaRESUMO
Abstract In this study, orodispersible films formed from hydroxypropyl methylcellulose (HPMC) E6 (2, 2.5, and 3%) and plasticizers ((glycerin (Gly), propylene glycol (PP), or polyethylene glycol (PEG)), containing doxazosin mesylate, were prepared by the solvent casting method and characterized. Design of experiments (DoE) was used as a statistical tool to facilitate the interpretation of the experimental data and allow the identification of optimal levels of factors for maximum formulation performance. Differential scanning calorimetry (DSC) curves and X-ray powder diffraction (XRPD) diffractograms showed doxazosin mesylate amorphization, probably due to complexation with the polymer (HPMC E6), and the glass transition temperature of the polymer was reduced by adding a plasticizer. Fourier transformed infrared (FTIR) spectroscopy results showed that the chemical structure of doxazosin mesylate was preserved when introduced into the polymer matrix, and the plasticizers, glycerin and PEG, affected the polymer matrix with high intensity. The addition of plasticizers increased the elongation at break and adhesiveness (Gly > PEG > PP), confirming the greater plasticizer effect of Gly observed in DSC and FTIR studies. Greater transparency was observed for the orodispersible films prepared using PP. The addition of citric acid as a pH modifier was fundamental for the release of doxazosin mesylate, and the desirability formulation had a release profile similar to that of the reference product
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Testes Mecânicos/instrumentação , Filmes Cinematográficos/classificação , Plastificantes/classificação , Análise Espectral/métodos , Varredura Diferencial de Calorimetria/instrumentação , Adesividade , Doxazossina/efeitos adversos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Derivados da Hipromelose/efeitos adversosRESUMO
(1) Background: This study aimed to use the simplex-centroid mixture design methodology coupled with a microdilution assay to predict optimal essential oil (EO) formulations against three potential foodborne pathogens simultaneously through the desirability (D) function. (2) Methods: Oregano (ORE; Origanum vulgare), thyme (THY; Thymus vulgaris), and lemongrass (LG; Cymbopogon citratus) and their blends were evaluated concerning minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) for Salmonella enterica serotype Enteritidis, Escherichia coli and Staphylococcus aureus. (3) Results: THY combined with ORE or LG were the most promising EO formulations in inhibiting and killing each bacterium separately. Regarding the simultaneous effect, the optimal proportion for maximum inhibition was composed of 75% ORE, 15% THY, and 10% LG, while for maximum inactivation was 50% ORE, 40% THY, and 10% LG. (4) Conclusion: The multiresponse optimization allowed identifying an EO blend to simultaneously control three potential foodborne pathogens. This first report could be a helpful natural and green alternative for the industry to produce safer food products and mitigate public health risks.
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Abstract Thiazolidinedione, often shortened to TZD or glitazone, helps lower insulin resistance, which is the underlying problem for many people with type 2 diabetes. The two most known glitazones are pioglitazone (PGZ), with the brand name medicine Actos®, and rosiglitazone (RSG), which is Avandia®. This study presented a multivariate optimization in the microextraction procedure employing Fractional Factorial Design (FFD) combined with Desirability Function (DF) to determine TZD and metabolites in biological samples. Microextraction requires several parameters to be optimized; however, most of them still use univariate optimization. Finding optimum conditions by simple response is relatively simple, but the problems, in case of microextractions, are often more complex when it has more responses. For example, changing one factor that promotes one response may suppress the effect of the others. Thus, this multivariate optimization was applied for two bioanalytical methods for determination of TZD and metabolites, one by HPLC and other by CE, both using Hollow Fiber Liquid-Phase Microextraction (HF-LPME). The results establish the optimal values and elucidate how the factors that affect HF-LPME procedure perform in extraction efficiency for TZDs. Additionally, this study demonstrates that DF can be an important tool to optimize microextraction procedures.
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Cromatografia Líquida de Alta Pressão/métodos , Tiazolidinedionas/efeitos adversos , Pioglitazona/análogos & derivados , Métodos , Resistência à Insulina , Diabetes Mellitus Tipo 2/patologia , Rosiglitazona/análogos & derivadosRESUMO
In this study, multivariate methodologies were applied in the optimization of a dispersive liquid-liquid microextraction (DLLME) method, aiming at the determination of Cu and Mn in coconut water samples by flame atomic absorption spectrometry. Some extractors (chloroform and CCl4), dispersants (ethanol, methanol and acetonitrile) and complexing agents (5-Br-PADAP and Dithzone) were previously tested in the extraction. A mixture design was used to optimize the component proportions formed by chloroform (10%), acetonitrile (76%), and 0.020% 5-Br-PADAP solution (14%). Doehlert design optimized the variables pH, NaCl, and buffer amounts for the extraction of both metals. The following analytical characteristics, respectively for Cu and Mn, were accessed: limit of quantification (4.83 and 3.32 µg L-1), enrichment factors (11 and 8 fold), and precision (6.6 and 6.0% RSD, n = 10). Addition/recovery tests of the analytes allowed to find values in the range of 96.5-120% for Cu and 99-107% for Mn.
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Microextração em Fase Líquida , Poluentes Químicos da Água , Cocos , Cobre/análise , Manganês , Espectrofotometria Atômica , Água , Poluentes Químicos da Água/análiseRESUMO
This work aims to produce bio-surfactant using a brewery waste (trub) as a strategy to reduce production costs related to the substrate, as well as to provide an eco-friendly destination for this residue. Trub is obtained during the boiling of the wort, being mainly composed of proteins and reducing sugars. To evaluate important process parameters on bio-surfactant production, a full factorial design (24) was elaborated, having agitation rate and concentrations of trub, yeast extract, and peptone as independent variables. The highest bio-surfactant concentration achieved was 100.76 mg L-1, where FTIR and Maldi-ToF-MS confirmed functional groups characteristic of peptides and isomers of surfactin in the bio-surfactant extract. Trub, agitation and yeast extract showed statistically significant effects on the response variable (surface tension), where an increase in the agitation rate and in the concentration of yeast extract demonstrated a positive impact on the production of bio-surfactant.
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Cerveja , Carbono/metabolismo , Resíduos Industriais , Tensoativos/metabolismo , Fermentação , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz , Espectroscopia de Infravermelho com Transformada de Fourier , Tensão SuperficialRESUMO
Multi-response optimization of hot pressurized liquid extraction (HPLE) was applied for the first time to obtain maqui (Aristotelia chilensis [Mol.] Stuntz) leaf extracts. The total polyphenol content (TPC), the antioxidant capacity (AC) as well as the total polyphenol purity of the maqui leaf extracts were accurately predicted (RSD < 8%) at the evaluated extraction scales. The optimum HPLE conditions that prioritized TPC and AC equally (OPT1) recovered ~3 times more TPC (205.14 mg GAE/g leaves) than maqui leaf extracts obtained by maceration, while the extract that prioritized purity over TPC and AC presented the highest purity (36.29%) and an EC50 ~3 times lower than currently reported values. It was found by multi-response optimization that maqui leaves and HPLE are among the best natural sources and extraction techniques, respectively, to recover protocatechuic acid, quercetin, and catechin.
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An optimization of the composition of polymer inclusion membrane (PIM)-based optodes, and their exposure times to metal ion solutions (Hg(II), Cd(II), and Pb(II)) was performed using two different chromophores, diphenylthiocarbazone (dithizone) and 1-(2-pyridylazo)-2-naphthol (PAN). Four factors were evaluated (chromophore (0.06-1 mg), cellulose triacetate (25-100 mg) and plasticizer amounts (25-100 mg), and exposure time (20-80 min)). Derringer's desirability functions values were employed as response variables to perform the optimization obtained from the results of three different processes of spectral data treatment: two full-spectrum methods (M1 and M3) and one band-based method (M2). The three different methods were compared using a heatmap of the coefficients and dendrograms of the Principal Component Analysis (PCA)reductions of their desirability functions. The final recommended M3 processing method, i.e., using the scores values of the first two principal components in PCA after subtraction of the normalized spectra of the membranes before and after complexation, gave more discernable differences between the PIMs in the Design of Experiments (DoE), as the nodes among samples appeared at longer distances and varyingly distributed in the dendrogram analysis. The optimal values were time of 35-65 min, 0.53 mg-1.0 mg of chromophores, plasticizers 34.4-71.9 of chromophores, and 62.5-100 mg of CTA, depending on the metal ion. In addition, the method yielded the best outcomes in terms of interpretability and an easily discernable color change so that it is recommended as a novel optimization method for this kind of PIM optode.
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This study presents the results obtained for the optimization of the mineralization of losartan (LOS) and hydrochlorothiazide (HCTZ) using the photo-Fenton process with a UV-Vis LED. Experimental design optimization employing a Doehlert matrix and a global desirability function enabled simultaneous evaluation of multiple responses, with factor fitting providing the best conditions that maximized the mineralization efficiency: Fe2+ at 10 mg L-1 and H2O2 at 100 mg L-1. High rates of mineralization of LOS and HCTZ were obtained, with dissolved organic carbon (DOC); removal of almost 75% after 90 min was observed for both pharmaceuticals. The kinetic model showed that the mineralization followed two regimes in the first minutes, with a fast progression followed by slower activity. The energy consumption calculated for mineralization of LOS and HCTZ at a concentration of 20 mg L-1 using the UV-Vis LED-assisted photo-Fenton process, at 60 min, was 130 kWh m-3. The desirability function provides a useful tool for finding optimal experimental conditions for the treatment of effluents with different characteristics. The UV-Vis LED was shown to be a good light source in the photo-Fenton process.
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Peróxido de Hidrogênio , Poluentes Químicos da Água , Hidroclorotiazida , Ferro , Cinética , Losartan , Oxirredução , Raios Ultravioleta , Poluentes Químicos da Água/análiseRESUMO
This study approaches the development of a method for the determination of Ca, Mg, Zn, and Fe in liquid and powdered cow milk. The method is based on sample dissolution assisted by ultrasound energy in tetramethylammonium hydroxide (TMAH) media and determination by flame atomic absorption spectrometry (FAAS). Central composite design (CCD) associated with response surface methodology and desirability function allowed the fast and efficient optimization of the variables involved in the performance of the dissolution. The developed dissolution method allowed Ca, Fe, Zn, and Mg determination in milk samples with adequate analytical characteristics for these determinations. Addition/recovery tests and analysis of a certified reference material of skimmed powdered milk (ERM-BD150) have shown that this method presents enough accuracy to carry out these analyses.
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Análise de Alimentos/métodos , Metais/análise , Leite/química , Compostos de Amônio Quaternário/química , Espectrofotometria Atômica/métodos , Animais , Bovinos , Feminino , Análise de Alimentos/estatística & dados numéricos , Análise Multivariada , Pós , SolubilidadeRESUMO
Food companies should comply with the requirements of a zero-waste concept to adapt to the circular economy requirements. In fruit companies, usually seeds are discarded without proper utilization and extraction of the bioactive compounds. Fruit seeds are sources of chemical compounds that can be extracted, studied, and applied in high value-added products. Thus, in this work the experimental conditions for the water extraction of phenolic compounds from camu-camu (Myrciaria dubia) seed coat were optimized using a central composite design and the desirability function. Total phenolic content (TPC), and condensed tannins (CT), DPPH radical scavenging activity, ferric reducing antioxidant capacity (FRAP), Folin-Ciocalteu reducing capacity (FCRC), and Cu2+ chelating ability were assessed. Seed coat extracted for 51.1 min using a 1:34.1 solid:liquid ratio was the optimal condition to extract 6,242 mg gallic acid equivalent (GAE)/100 g of TPC and 695 mg catechin equivalent (CE)/100 g of CT. The optimized extract displayed free-radical scavenging activity, reducing properties and ability to chelate Cu2+ , and inhibited the growth of Listeria monocytogenes, Pseudomonas aeruginosa, Salmonella Typhimurium, Salmonella Enteritidis, Bacillus cereus, and Staphylococcus aureus. Additionally, the lyophilized water extract inhibited the in vitro activity of α-amylase, α-glucosidase, and angiotensin converting enzyme and showed cytotoxic effects towards Caco-2, A549, and HepG2 cancer cells, but no cytotoxicity towards IMR90 cells. Vescalagin, castalagin, and 3,4-dihydroxybenzoic acid were the major phenolic compounds identified in the optimized extract. In conclusion, the optimized camu-camu seed coat water extract is a rich source of phenolic compounds with antioxidant, antidiabetic, antihypertensive, and antiproliferative effects. PRACTICAL APPLICATION: Camu-camu fruit pulp and seeds have been studied for their phenolic composition and bioactivity. However, seeds are usually discarded and represent an environmental problem in South American countries. We presented a methodological overview on the extraction optimization of the phenolic compounds from camu-camu seed coat and studied the bioactivity of the optimized extract using chemical, enzymatic, and cell-based experiments. Results can be used by camu-camu processors to obtain a phenolic-rich extract for industrial applications, without any further processing.
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Myrtaceae/química , Fenóis/química , Fenóis/isolamento & purificação , Extratos Vegetais/química , Sementes/química , Antibacterianos/isolamento & purificação , Anti-Hipertensivos/isolamento & purificação , Antineoplásicos Fitogênicos/isolamento & purificação , Antioxidantes/isolamento & purificação , Células CACO-2 , Humanos , Hipoglicemiantes/isolamento & purificação , Resíduos Industriais/análise , Proantocianidinas/análise , alfa-Amilases/antagonistas & inibidoresRESUMO
Camu-camu (Myrciaria dubia) seeds are discarded without recovering the bioactive compounds. The main aim of the present work was to optimise the solvent mixture to extract higher total phenolic content and antioxidant capacity of camu-camu seeds. The optimised solvent system increased the extraction of phenolic compounds, in which vescalagin and castalagin were the main compounds. The optimised extract displayed antioxidant capacity measured by different chemical and biological assays, exerted antiproliferative and cytotoxic effects against A549 and HCT8 cancer cells, antimicrobial effects, protected human erythrocytes against hemolysis, inhibited α-amylase and α-glucosidase enzymes and presented in vitro antihypertensive effect. Additionally, the optimized extract inhibited human LDL copper-induced oxidation in vitro and reduced the TNF-α release and NF-κB activation in macrophages cell culture. Thus, the use of camu-camu seed showed to be a sustainable way to recover bioactive compounds with in vitro functional properties.
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Myrtaceae/química , Extratos Vegetais/química , Extratos Vegetais/farmacologia , Animais , Anti-Infecciosos/química , Anti-Infecciosos/farmacologia , Anti-Inflamatórios/química , Anti-Inflamatórios/farmacologia , Anti-Hipertensivos/química , Anti-Hipertensivos/farmacologia , Antioxidantes/química , Antioxidantes/farmacologia , Linhagem Celular , Avaliação Pré-Clínica de Medicamentos/métodos , Hemólise/efeitos dos fármacos , Humanos , Taninos Hidrolisáveis/análise , Hipoglicemiantes/química , Hipoglicemiantes/farmacologia , Fenóis/análise , Sementes/química , alfa-Amilases/antagonistas & inibidoresRESUMO
This work aimed to optimize an aqueous extract rich in phenolic compounds and potential functional properties made of Ilex paraguariensis, Melissa officinalis, and Cymbopogon citratus. The lyophilized extract was used for the development of an ice cream. Total phenolics, FRAP, DPPH, Folin-Ciocalteu's reducing capacity, and total reducing capacity of different combinations of herbal extracts were tested and modeled using response surface methodology. Simultaneous optimisation was employed to maximize the bioactive compounds in the extract and the lyophilized optimum combination was added to ice cream. The lyophilized extract contained quercetin-3-rutinoside, hesperidin, isoquercetin, caffeic acid, and 5,7-dihydroxyflavone. The optimised extract, which showed antihypertensive, antidiabetic, and antioxidant activity using in vitro protocols, increased total phenolics and antioxidant activity in comparison to the control ice cream. The ice cream presented a sensory acceptance index of 83%. After 72â¯days of storage (-18⯰C), total phenolics and antioxidant activity significantly decreased.
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Indústria de Processamento de Alimentos/métodos , Sorvetes , Extratos Vegetais/química , Extratos Vegetais/farmacologia , Adolescente , Adulto , Anti-Infecciosos/farmacologia , Anti-Hipertensivos/química , Anti-Hipertensivos/farmacologia , Antioxidantes/química , Antioxidantes/farmacologia , Linhagem Celular , Cymbopogon/química , Feminino , Flavonoides/análise , Flavonoides/química , Armazenamento de Alimentos , Humanos , Sorvetes/análise , Ilex paraguariensis/química , Masculino , Melissa/química , Pessoa de Meia-Idade , Oligossacarídeos/química , Fenóis/química , PaladarRESUMO
The process employed for the pulping and bleaching of sorghum straw was optimized prior to the synthesis of cellulose acetate. A 22 factorial central composite design was carried out. The variables considered were cooking time (1.5 to 2.5â¯h) and dilute alkali concentration (0.75 to 1.25%) for the pulping and bleaching time (30 to 35â¯min) and bleach volume (20 to 25â¯mL) for the bleaching. The sorghum straw was comprised of 49.43% α-cellulose, 19.18% hemicellulose and 30.42% lignin. The optimum conditions that maximize these processes were 2.5â¯h and 1.25% (dilute alkali concentration) at 90⯰C, and 35â¯min and 25â¯mL (bleach volume) at 80⯰C, respectively, providing pulps with a low Kappa number (<3) and lignin content, and cellulose with a high degree of crystallinity. The 1H NMR, XRD, FTIR spectroscopy, SEM and thermal analysis demonstrated that it is possible to synthetize cellulose acetate (with 2.62 degrees of substitution) by acetylating bleached pulp for 16â¯h at 25⯰C.
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Celulose/análogos & derivados , Sorghum/química , Celulose/síntese química , Celulose/química , Fenômenos Químicos , Técnicas de Química Sintética , Peso Molecular , ResíduosRESUMO
Berries are among the nutritionally richest fruits and the mixing of these fruits can originate products with peculiar characteristics and added value, since the fruit mixture allows adding nutritional and sensory value to the final product. Thus, in this study we aimed to optimize a mixed berry jelly formulation of red fruit (blackberry, blueberry, and strawberry), through the mixture design, desirability function, and response surface methodology. The fruit mixture influenced the physical-chemical, sensory, and nutritional characteristics of mixed jelly, and it was observed that the mixture of two or more fruits may increase the acceptance of the product and even its nutritional value. According to the contour curve graph for the sensory and nutritional desirability function, the ideal mixed berry jelly should contain 55% to 100% blackberry, 0% to 20% blueberry, and 0% to 40% strawberry. The exact proportion of fruit may depend on seasonality or the commercial value of the fruit. PRACTICAL APPLICATION: In Brazil, there are many blackberry, blueberry, and strawberry cultivars grown in subtropical regions and high perishability hinders the fruit consumption in fresh form. In this context, through this study it was possible to verify which fruits are more suitable for processing in the form of jelly, as well as to optimize, based on sensory and nutritional characteristics, a mixed berry jelly formulation with greater attractiveness to consumers.
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Mirtilos Azuis (Planta)/química , Manipulação de Alimentos/métodos , Fragaria/química , Frutas/química , Rubus/química , Brasil , Humanos , Valor Nutritivo , PaladarRESUMO
This research focused on obtaining eicosapentaenoic acid (EPA, 20:5 n-3) and docosahexaenoic acid (DHA, 22:6 n-3) (EPA+DHA) concentrates from refined commercial salmon oil (RCSO). Independent variables of the complexation process were optimized by means of the application of response surface methodology (RSM) in order to obtain the maximum content of such fatty acids (FAs). As a result of employing the optimized conditions for all the variables (6.0, urea:FA content ratio; -18.0 °C, crystallization temperature; 14.80 h, crystallization time; 500 rpm, stirring speed), high contents of EPA and DHA could be obtained from RCSO, achieving increases of 4.1 and 7.9 times in the concentrate, with values of 31.20 and 49.31 g/100 g total FA, respectively. Furthermore, a 5.8-time increase was observed for the EPA + DHA content, which increased from 13.78 to 80.51 g/100 g total FA. It is concluded that RCSO can be transformed into a profitable source of EPA and DHA (EPA+DHA), thus leading to a product with higher commercial value.
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Ácidos Docosa-Hexaenoicos/análise , Ácido Eicosapentaenoico/análise , Ácidos Graxos/química , Óleos de Peixe/análise , Óleos de Peixe/química , Ureia/química , Valor NutritivoRESUMO
Honeydew honeys have been under-evaluated about their major phenolic compounds, especially Mimosa scabrella Bentham (bracatinga) honeydew honey. In this work, a fast and robust chromatographic method was optimized for simultaneous separation and quantification by HPLC/DAD of 18 phenolic compounds detected in bracatinga honeydew honey. A simplex-centroid design, central composite rotatable design and response surface-desirability function simultaneous optimization of Derringer and Suich were used, evaluating the mobile phase composition, flow rate and oven temperature to separate all the peaks. These multivariate procedures were efficient in determining the optimal separation conditions, using peak pair resolutions and run time as responses. The 18 peaks were separated in 25 min and the mobile phase gradient started with 1.6% MeOH, 3.3% ACN, 1.0% THF and 94.1% formic acid 0.1% changing to 10.0% MeOH, 33.3% ACN, 6.0% THF and 50.7% formic acid 0.1%, oven temperature of 33 °C and flow rate of 0.73 mL min-1. The method was validated according to Eurachem guidelines and considered accurate and robust. It was applied to 18 bracatinga honeydew honey samples in which 9 phenolic compounds were identified and quantified.