A simple and rapid spectrophotometric method for the determination of trans-chalcone in raw-materialand topical formulation / Método espectrofotométrico simples e rápido paradeterminação de trans-chalcona em matéria-primae em formulação tópica

Trans-chalcone (TC) is a flavonoid precursor characterized by a wide spectrum of action, with anti-inflammatory and antioxidant effects. However, no validated methods are available in official compendia for the analysis of this substance. Thus, the aim of this work was to develop and validate a simple, fast, and reproducible spectrophotometric method for the analysis of TC in raw material, and in topical pharmaceutical formulation containing TC. The established conditions were: methanol as extracting solvent, and detection wavelength of 309 nm by UV spectrophotometer. All tests followed the rules of Resolution RDC 166, 2017. The proposed method was selective. Linearity was demonstrated in the concentration range of 1 to 8 µg/mL (r = 0.999). Repeatability and intermediate precision were confirmed by low relative standard deviation values of 1.53% and 2.70% for TC, and of 1.73% and 2.91% for formulation containing TC. Accuracy, evaluated through recovery test, was adequate, with minimum of 98.24% and maximum of 100.23% of recovery. It was observed that the small deliberate modifications done did not interfere with the results, demonstrating the method is robust. The results showed that the method was considered suitable for the intended purpose, inexpensive, easy to apply, selective, linear, precise, accurate, and robust for the determination TC, and pharmaceutical formulation containing TC. Thus, the method developed satisfies the need for an analytical method for the determination of TC, and topical formulation containing TC, being effective, innovative and able to aid in the development of the pharmaceutical field.

Trans-chalcona (TC) é um precursor de flavonoides caracterizado por um amplo espectro de ação, como efeitos anti-inflamatórios e antioxidantes. No entanto, não há método validado disponível em compêndio oficial para análise deste composto. Então, o objetivo deste trabalho foi desenvolver e validar um método espectrofotométrico, simples, rápido e reprodutível para análise de TC em matéria-prima, e em formulação farmacêutica tópica contendo TC. As condições estabelecidas foram: metanol como o solvente de extração, e detecção no comprimento de onda de 309 nm por espectrofotometria no UV. Todos os testes seguiram as normas da RDC 166, 2017. O método proposto foi seletivo. A linearidade foi demonstrada na faixa de concentração de 1 a 8 µg/mL (r = 0.999). A repetibilidade e a precisão intermediária foram confirmadas pelos valores baixos de desvio padrão relativo de 1,53% e 2,70% para a TC, e de 1,73% e 2,91% para a formulação contendo TC. A exatidão, avaliada por meio de testes de recuperação, foi adequada, com mínimo de 98,24% e máximo de 100,04% de recuperação. Observou-se que pequenas modificações no método não interferiram nos resultados, demonstrando que o método é robusto. Os resultados demonstraram que o método foi adequado para a finalidade pretendida, barato, de fácil aplicação, seletivo, linear, preciso, exato e robusto para determinação de TC, e de formulação contendo TC. Então o método desenvolvido satisfaz as necessidades de um método analítico para determinação de TC, e de formulação tópica contendo TC, e é eficaz, inovador e pode contribuir para o desenvolvimento da área farmacêutica.

Analysis of docosanol using GC/MS:Method development,validation,and application to ex vivo human skin permeation studies / 药物分析学报

Docosanol is the only US Food and Drug Administration(FDA)approved over-the-counter topical product for treating recurrent oral-facial herpes simplex labialis.Validated analytical methods for docosanol are required to demonstrate the bioequivalence of docosanol topical products.A gas chromatography/selected ion monitoring mode mass spectrometry(GC/SIM-MS)method was developed and validated for docosanol determination in biological samples.Docosanol and isopropyl palmitate(internal standard)were separated on a high-polarity GC capillary column with(88％cyanopropy)aryl-polysiloxane employed as the stationary phase.The ions of m/z 83 and 256 were selected to monitor docosanol and isopropyl palmitate,respectively;the total run time was 20 min.The GC/SIM-MS method was validated in accordance with US FDA guidelines,and the results met the US FDA acceptance criteria.The docosanol calibration standards were linear in the 100-10000 ng/mL concentration range(R2＞0.994).The recoveries for docosanol from the receptor fluid and skin homogenates were＞93.2％and＞95.8％,respectively.The validated method was successfully applied to analyze ex vivo human cadaver skin permeation samples.On applying Abreva?cream tube and Abreva?cream pump,the amount of doco-sanol that penetrated human cadaver skin at 48 h was 21.5±7.01 and 24.0±6.95 ng/mg,respectively.Accordingly,we concluded that the validated GC/SIM-MS was sensitive,specific,and suitable for quantifying docosanol as a quality control tool.This method can be used for routine analysis as a cost-effective alternative to other techniques.

A review of the potential therapeutic and cosmetic use of propolis in topical formulations

A good deal of research has been carried out on the establishment and characterization of antioxidants and antibacterialproducts from natural sources for topical use. Recently, investors mainly from the cosmetics industry have becomeinterested in products from different species, not only for their individual active principles but also in the crudeextract itself. Propolis is one of such products. Several previous reports have demonstrated the antimicrobial, antiinflammatory, and wound healing effects of propolis. Additionally, what has drawn attention of the pharmaceuticalindustry to propolis and its derivatives, such as throat spray, is related to its antioxidant properties, having the potentialfor treatment and prevention of oxidative stress-mediated diseases, such as those developed on the skin, as well asaging. This literature review will focus on propolis composition and related potential uses in topical pharmaceuticaland cosmetic formulations.

Prevention of UVB radiation-induced oxidative stress in mice by topical administration of Azadirachta indica(neem) extract

Neem tree (Azadirachta indica A. Juss. fam. Meliaceae) has been extensively employed to combat diverse pathologies. Moreover, it has been described that its leaf extract present anticarcinogenic action. Thus, the neem extract (NE) chemical and antioxidant properties was evaluated, and also, the capacity of two dermatological formulations incorporated with neem extract (F1 and F2) to avoid oxidative UVB-induced skin injury in hairless mice. NE constituents were investigated and free radical scavenging ability were determined by different methods in vitro. Skin from mice treated with F1 and F2 and submitted to UVB radiation were tested for different parameters of inflammation and oxidative injury. Results show that the NE polyphenol and flavonoid content were 135.30 and 37.12mg/g, respectively. High performance liquid chromatography (HPLC) results demonstrated the existence of azarachtin, rutin, ursolic acid and tannic acid. NE presented scavenging ability by ABTS radical, ferric-reducing antioxidant power (FRAP), inhibition of lipid peroxidation and iron chelation. In vivo, it was observed that mice treated with F1 and F2 showed amelioration of the inflammation by reducing UVB induced skin edema. However, only samples from animals treated with F1 had lower neutrophil recruitment (measured by myeloperoxidase activity), and returning the oxidative status to baseline levels in parameters such as reduced glutathione level, ferric reducing ability (FRAP), and scavenging of free radical (ABTS). Concluding, NE demonstrated a good antioxidant property in vitro, and the data suggest the use of NE added F1 to prevent skin damage caused by UVB irradiation.(AU)

Development of a new propolis microemulsion system for topical applications / Desenvolvimento de um novo sistema microemulsionado de própolis para aplicação tópica

Microemulsion systems (MES) offer advantages as drug delivery systems, among them favour drug absorption, being in most case more efficient than other methods in delivering of drug. In this work a new MES was obtained in order to be applied as a pressurized aerosol formulation containing bee propolis ethanolic extract (PEE). For that, pseudoternary phase diagrams were used to characterize the microemulsions boundaries and also to define the Winsor IV microemulsion region of the PEE-MES system containing Tween 80 as surfactant and the cosurfactant ethyl alcohol in small percentage. The obtained results indicated that the best MES was composed by Tween 80 and ethyl alcohol with C/S (cosurfactant/surfactant) ratio equal to 1.0, since it provided a large boundaries in the obtained O/W microemulsion region. This PEE-MES formulation, in which bee propolis consisting as oil phase, is herein designed for topical uses (PEE-MES spraying) in order to treat mouth and throat inflammatory infections. Considering the very large uses of bee propolis in conventional vehicles, MES type of delivery system has to be compatible with achieving the highest drug aim loadings, determined substantially by the specific MES application (drug solubilization in water systems) improving in this case, propolis farmacological aplications. Additionally, PEE-MES antibacterial effect was evidenced and the microemulsion system PEE-MES was also used as newest chemical approach for extraction of bee propolis material from resinous hive.

Sistemas microemulsionados (MES) oferecem inúmeras vantagens como liberadores de fármacos já que favorecem a absorção do princípio ativo e são, em muitos casos, mais eficientes do que outros métodos de liberação de substâncias bioativas. Neste trabalho, um MES foi obtido visando uma formulação para uso tópico, contendo extrato etanólico de própolis (PEE). Neste estudo, Diagramas de fase pseudoternários foram utilizados para caracterização das regiões de microemulsão, bem como para definição da região de Winsor IV do sistema PEE-MES (Tween 80 como tensoativo e álcool etílico como co-tensoativo, em baixo percentual). Os resultados obtidos indicaram que o melhor sistema microemulsionado contém C/S (cotensoativo/tensoativo) na razão 1,0, fornecendo uma microemulsão do tipo O/A com ampla região de Winsor IV. A formulação PEE-MES poderá vir a ser utilizada comercialmente para uso tópico no combate a inflamações de boca e garganta. Considerando o amplo uso de própolis em formulações convencionais, onde sua solubilidade representa um dos maiores problemas, o sistema PEE-MES disponibiliza este produto natural para aplicações farmacológicas, com boa solubilidade em um sistema microemulsionado do tipo O/A. Adicionalmente, o efeito bactericida do sistema PEE-MES foi comprovado e uma nova metodologia de extração de própolis é apresentada.