Use of sisal industrial waste (Agave sisalana Perrine) in sustainable and multifunctional cosmetic products.

OBJECTIVE: Sisal is a common stiff fibre produced around the world, corresponding to approximately 70% of the commercial production of all fibres of this type. The fibres are extracted from the leaves of Agave sisalana, from which approximately 4% of their weight is obtained, with the remaining 96% considered to be residues from the process of the sisal industry. The objective of this work was to obtain a polyphenol-enriched extract from the A. sisalana residue by ultrasonically assisted extraction, characterize it chemically, evaluate in vitro antioxidant activity, and develop safe and stable photoprotective formulations for future application in cosmetic preparations. METHODS: Ultrasonic extraction of solid plant material was performed using 50% ethanol/water (v/v). The extract was chemically characterized by high-performance liquid chromatography equipment associated with classical molecular networking and evaluated for in vitro antioxidant activity by different methodologies. Ten formulations were prepared, varying the component concentrations and the shear time. The 1.0% sisal extract was incorporated into the most stable formulations, and preliminary and accelerated stability were evaluated. The emulsions were investigated for safety by assessment of primary accumulated dermal irritability and sensitization and a dermatological clinical study of phototoxicity and photosensitization. The photoprotective formulations containing or not containing the extract that were stable after 90 days had their in vivo sun protection factor (SPF), UVA protection factor, critical wavelength, and protection against visible and blue light determined. RESULTS: Ultrasound extraction using 50% ethanol/water (EH 50) as an extractor vehicle showed the best yield. The extract exhibited a concentration of phenolic compounds (77.93 mg of equivalent to the standard gallic acid/g) and showed in vitro antioxidant activity. Emulsions without and with 1.0% sisal extract remained stable and safe. The addition of the extract to the photoprotective formulation statistically increased the SPF when compared to the formulation without the extract and offered protection against UVA radiation, critical wavelengths, and absorption of visible and blue light. CONCLUSION: Based on the findings, the solid residue of A. sisalana may be indicated as a component of photoprotective and antioxidant cosmetic formulations.

OBJECTIF: Le sisal est une fibre rigide courante produite dans le monde entier, correspondant à environ 70 % de la production commerciale de toutes les fibres de ce type. Les fibres sont extraites des feuilles d'Agave sisalana dont environ 4 % du poids est obtenu, les 96 % restants étant considérés comme des résidus du procédé de l'industrie du sisal. L'objectif de ce projet était d'obtenir un extrait du résidu d'A. sisalana enrichi en polyphénols par extraction assistée par ultrasons (EAU), de le caractériser chimiquement, d'évaluer l'activité antioxydante in vitro et de développer des formulations photoprotectrices sûres et stables pour une application future dans des préparations cosmétiques. MÉTHODES: L'extraction ultrasonique de la matière végétale solide a été effectuée avec une solution à 50 % d'éthanol/eau (v/v). L'extrait a été chimiquement caractérisé avec un équipement de chromatographie en phase liquide à haute performance associé à un réseau moléculaire (RM) classique, puis évalué pour l'activité antioxydante in vitro par différentes méthodologies. Dix formulations ont été préparées en variant les concentrations des composants et le temps de cisaillement. L'extrait de sisal à 1,0 % a été incorporé dans les formulations les plus stables et la stabilité préliminaire et accélérée a été évaluée. La sécurité d'emploi des émulsions a été étudiée en évaluant l'irritabilité et la sensibilisation cutanées accumulées primaires et l'étude clinique dermatologique de la phototoxicité et de la photosensibilisation. Le facteur de protection solaire in vivo, le facteur de protection UVA, la longueur d'onde critique et la protection contre la lumière visible et bleue ont été déterminées pour les formulations photoprotectrices contenant ou non l'extrait qui étaient stables après 90 jours. RÉSULTATS: L'extraction par ultrasons utilisant une solution à 50 % d'éthanol/eau (EH 50) comme véhicule d'extraction a menée au meilleur rendement. L'extrait a présenté une concentration de composés phénoliques (77,93 mg d'EAG/g) et une activité antioxydante in vitro. Les émulsions sans et avec 1,0 % d'extrait de sisal sont restées stables et sans danger. L'ajout de l'extrait à la formulation photoprotectrice a statistiquement augmenté le SPF par rapport à la formulation sans extrait et a offert une protection contre les rayonnements UVA, la longueur d'onde critique et l'absorption de la lumière visible et bleue. CONCLUSION: D'après ces résultats, les résidus solides d'A. sisalana peuvent être indiqués comme composant des formulations cosmétiques photoprotectrices et antioxydantes.

Vegetable moisturizing raw material from "Caatinga" Brazilian biome: safety and efficacy evaluations of O/W cosmetic emulsions containing Kalanchoe brasiliensis extract

The purpose of this study was to evaluate the safety of Kalanchoe brasiliensis extract, followed by the development of an oil in water emulsion containing the K. brasiliensis leaves extract and evaluating its clinical moisturizing efficacy. The formulations containing sodium acrylates/ Beheneth-25 methacrylate Crosspolymer (and) hydrogenated polydecene (and) lauryl glucoside and 0.5% of extract were prepared. The extract was considered as non-irritating through skin irritant tests. The stability testing was carried out in different conditions for 90 days. The skin hydration was measured by capacitance measurement and transepidermal water loss using biophysical techniques. The results indicate that the formulation containing 0.5% of extract increased the hydration of the stratum corneum up to 5 h after application on the forearm. The transepidermal water loss was reduced when compared to the untreated area and placebo area. Therefore, we can conclude that the increased skin hydration and protection of barrier function can be attributed to the K. brasiliensis extract. This research presents a new raw material from the Brazilian Caatinga biome and shows its possible application in the development of cosmetic products.

Use of Opuntia ficus-indica (L. ) Mill extracts from Brazilian Caatinga as an alternative of natural moisturizer in cosmetic formulations

ABSTRACT The aim of this work was the obtainment of Opuntia fícus-indica (L.) Mill extract for the development of cosmetic formulations and in vivo evaluation of its moisturizing effects. The formulations were tested for preliminary and accelerated stability. Organoleptic characteristics, pH values and rheological behavior were assessed. The evaluation of moisturizing efficacy of the emulsions formulated with 3.0% of Polyacrylamide (and) C13-14 Isoparaffin (and) Laureth-7 containing 1.0 and 3.0% of O. ficus-indica hydroglycolic extract (EHG001) was performed using the capacitance method (Corneometer(r)) and the transepidermal water loss - TEWL evaluation (Tewameter(r)). The emulsions formulated were stable, exhibiting pseudoplastic and thixotropic behavior. The results of evaluation of moisturizing efficacy showed increased skin hydration after five hours by mainly increasing the skin barrier effect. The formulations containing 1.0 and 3.0% of EHG001 enhanced the skin barrier effect by reducing TEWL up to four hours after application. The results observed suggest that O. ficus-indica hydroglycolic extract may act through a humectant and occlusion mechanism.

Desenvolvimento e validação de método analítico para determinação do 4-nerolidilcatecol (4-NRC) em solução de proteína plasmática para aplicação em estudos de microdiálise cutânea / Development and validation of analytical method to determine 4-nerolidylcatechol (4-NRC) in plasma protein solution used for cutaneous microdialysis studies

Este artigo aborda a validação de um método analítico para determinação, em amostras de microdiálise, de 4-nerolidilcatecol (4-NRC), uma substância natural extraída da Piper umbellata (Piperaceae) com comprovada atividade antioxidante. O sistema de cromatografia líquida (CLAE-PDA Shimadzu LC 20AT, bomba LC–20AT, injetor com autosampler SIL– 20A) foi acoplado a uma coluna C18 (Phenomenex® Synergi Fusion 4μ RP-80ª, 150 x 4,6 mm). A fase móvel constituiu-se de acetonitrila, metanol e água (54:20:26, v:v:v), sob fluxo de 1,0 mL min-1, com detecção a 280 nm, volume de injeção 30 μL e tempo de corrida 15 minutos. O método foi linear para concentrações de 5,0-200,0 μg mL -1 (r = 0,9996). Os limites de detecção e de quantificação foram, respectivamente, 1,35 e 4,5 μg mL-1. A precisão (DPR <5,0%) e exatidão (99,0 – 112,0%) ficaram dentro dos valores recomendados pela ANVISA. A robustez foi garantida medindo-se a influência da variação do fluxo e da proporção de acetonitrila da fase móvel. As amostras de albumina enriquecidas com 4-NRC e submetidas ao processo de extração apresentaram recuperação de 69 a 95%. O método desenvolvido pode ser aplicado à análise de 4-NRC, com finalidade de estudos de microdiálise cutânea, devido aos adequados parâmetros de validação obtidos.

This paper reports the validation of an analytical method for the determination, in skin microdialysis samples, of 4-nerolidylcatechol (4-NRC), a natural substance extracted from Piper (Pothomorphe) umbellata (Piperaceae) with recognized antioxidant activity. The liquid chromatographic system (HPLC-PDA Shimadzu LC20AT, pump LC-20AT, injector with autosampler SIL-20A) was coupled to a C18 column (Phenomenex® Synergi Fusion 4 μm RP-80 Å, 150 x 4.6 mm), with acetonitrile:methanol:water (54:20:26, v:v:v) as the mobile phase, flowing at 1.0 mL min-1, with detection by absorbance at 280 nm, injection volume 30 μL and running time 15 min. The method was linear for concentrations from 5.0 to 200.0 μg mL-1 (r=0.9996). Detection and quantitation limits were, respectively, 1.35 and 4.5 μg mL-1, precision (RSD < 5.0%) and accuracy (99.0-112.0%) within values recommended by ANVISA. The robustness was tested by measuring the effect of arying the flow-rate and the proportion of acetonitrile in the mobile phase. Microdialysis perfusion solution of albumin (BSA) spiked with 4-NRC and subjected to liquid-liquid extraction showed recovery from 69 to 95%. This method is applicable to the analysis of 4-NRC for the purpose of cutaneous microdialysis studies, in view of the acceptable validation parameters obtained.

Rubus rosaefolius extract as a natural preservative candidate in topical formulations.

Even though the synthetic preservatives may offer a high antimicrobial efficacy, they are commonly related to adverse reactions and regarded as having potentially harmful effects caused by chronic consumption. The development of natural preservatives provides a way of reducing the amount of synthetic preservatives normally used in pharmaceutical and cosmetic preparations. In addition, these agents have less toxic effects and represent a possible natural and safer alternative of the preservatives. The purpose of this research was to evaluate the Rubus rosaefolius Smith extract efficiency as a natural preservative in base formulations. Of the extract, 0.2% (w/w) was assayed for its effectiveness of antimicrobial protection in two different base formulations (emulsion and gel). The microbial challenge test was performed following the standard procedures proposed by The United States Pharmacopoeia 33nd, European Pharmacopoeia 6th, Japanese Pharmacopoeia 15th, and the Cosmetics, Toiletries, and Fragrance Association using standardized microorganisms. The results demonstrated that R. rosaefolius extract at the studied concentration reduced the bacterial inocula, satisfying the criterion in all formulations, even though it was not able to present an effective preservative behavior against fungi. Thus, the investigation of new natural substances with preservative properties that could be applied in pharmaceutical and cosmetic products is relevant due to the possibility of substituting or decreasing the concentration of synthetic preservatives, providing a way for the development of safer formulas for the use of consumers.

Avaliação da eficácia e segurança do extrato de folhas de Rubus rosaefolius Sm. visando a aplicação como conservante em produtos cosméticos / Effectiveness and safety evaluation of Rubus rosaefolius Sm. leaves, regarding to the preservative use in cosmetic products

Os produtos cosméticos e farmacêuticos contendo componentes de origem natural têm aumentado significativamente nos últimos anos. Com o objetivo de utilizar esses componentes como conservante em formulações cosméticas, determinou-se a atividade antimicrobiana do extrato bruto de folhas de Rubus rosaefolius Sm. e suas frações. Aquele de melhor desempenho foi avaliado quanto à toxicidade in vitro e seu comportamento em formulações cosméticas (creme, gel e xampu), relacionado à estabilidade, eficácia do sistema conservante e compatibilidade epidérmica. A atividade antimicrobiana foi determinada pelo método de microdiluição e a concentração de 0,2% (p/v) do extrato bruto apresentou melhor desempenho. O teste de toxicidade do extrato bruto foi realizado por meio do método colorimétrico Cell Titer 96®, MTS, em cultura de queratinócitos humanos, constatando-se índice de citotoxicidade (IC50) de 1,0 mg/mL. As formulações cosméticas contendo o extrato foram analisadas quanto à estabilidade e as de melhor desempenho foram submetidas ao teste de eficácia do sistema conservante, de acordo com os procedimentos descritos na CTFA. O sistema conservante mostrou-se efetivo frente à Escherichia coli IAL 2393 (ATCC 10536), a Pseudomonas aeruginosa IAL 1874 (ATCC 9027), ao Staphylococcus aureus IAL 1875 (ATCC 6548), a Burkholderia cepacia IAL 1834 ATCC (17759) e a Candida albicans IAL 1611 (ATCC 10231). Avaliouse a compatibilidade epidérmica das formulações em equivalentes dermo-epidérmicos, sistema tridimensional cultivados na superfície ar-líquido. Os resultados mostraram que houve diferenças na compatibilidade epidérmica dependendo das características dos componentes das formulações. Concluiu-se que o extrato bruto de folhas de Rubus rosaefolius Sm. a 0,2% (p/v) pode ser utilizado como candidato a conservante em formulações cosméticas, sendo estável e apresentar compatibilidade epidérmica.

Cosmetic and pharmaceuticals products contained natural compounds have increased in the last few years. To verify the use of these compounds as preservative in formulations, the antimicrobial activity from the raw extract of the Rubus rosaefolius Sm. leaves and its fractions was determined. The toxicity in vitro and the behavior in cosmetic formulations (gel, emulsion and shampoo), regarding to the stability, effectiveness of the preservative system, and epidermal compatibility were evaluated in the extract, which had the best preservative action. The antimicrobial activity was determined by the micro dilution method, and the 0.2% concentration (w/v) of the raw extract had the best performance. The toxicity of the extract was analyzed by Cell Titer 96® colorimetric; MTS method in human keratinocytes culture, and the index of cytotoxicity (IC 50) found was 1.0 mg/mL. The cosmetic formulations with the raw extract were analyzed regarding to the stability and the best formulations were submitted to preservative challenge test, according to CTFA procedures. The preservative system was effective against Escherichia coli IAL 2393 (ATCC 10536), Pseudomonas aeruginosa IAL 1874 (ATCC 9027), Staphylococcus aureus IAL 1875 (ATCC 6548), Burkholderia cepacia IAL 1834 ATCC (17759), and Candida albicans IAL 1611 (ATCC 10231). The epidermal compatibility of the formulations was verified by skin (dermo-epidermal) equivalent, three-dimensional system, cultivated in the air-liquid surface. The results showed there were differences in the epidermal compatibility depended on the ingredient of formulation. In conclusion, the raw extract from the Rubus rosaefolius Sm leaves 0.2% (w/v) can be used as preservative candidate in the cosmetic formulations analyzed due to stability and it presented epidermal compatibility.

Validação de metodologias analíticas para determinação quantitativa de α-tocoferol e 4-nerolidilcatecol / Validation of α-tocopherol and 4-nerolidylcathecol quantitative assessment methodologies

O objetivo do nosso trabalho foi desenvolver um método para avaliação da concentração do `alfaï-tocoferol, considerado o antioxidante lipofilico de maior importância, e do 4-nerolidilcatecol (4-NC), uma substância natural com comprovada ação antioxidante in vitro e in vivo, em matriz biológica (homogeneizado de pele). Utilizamos a cromatografia de alta eficiência acoplada a um detector eletroquímico, sendo que o método apresentou linearidade para as concentrações de 0,025 µg/mL para o `alfaï-T (tempo de retenção 3,4 min) e de 0,15 µg/mL a 2,5 µg/mL para o 4-NC (tempo de retenção 2,06 min), dissolvidos em etanol e etanol:água (1:1)...