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En Perú, al 2019, solo el 6,4 % de los distritos disponen sus residuos urbanos en rellenos sanitarios, los cuales, están en situación de colapso, lo que exige buscar alternativas para mejorar la gestión de estos residuos y, frente a ello, el compostaje se perfila como una tecnología simple y económica, empleada para el tratamiento del componente orgánico, para reducir daños a la salud y al ambiente, sin embargo, la falta de criterios técnicos en su aplicación está afectando la calidad del compost final. El objetivo de esta investigación fue evaluar los criterios técnicos de procesamiento y la calidad del compost, a través de residuos sólidos urbanos en los distritos de la provincia Leoncio Prado. La investigación identificó los distritos que aplican el compostaje a sus residuos y evaluó la técnica de procesamiento, indicadores fisicoquímicos y determinó la calidad con base en normas técnicas internacionales. Los resultados muestran que seis de diez distritos aplican el compostaje y los indicadores fisicoquímicos contrastados con los criterios de calidad de la norma técnica chilena (NCH 2880), colombiana 5167 y de la OMS, corresponden a compost de calidad intermedia (Clase B). Los compost evaluados no representan riesgo ambiental y pueden ser utilizados como enmienda en la mejora del suelo y los cultivos con algunas restricciones, por presentar valores elevados de humedad, pH y bajos niveles de P, Ca, Mg y K.
At 2019, in Peru, only 6.4 % of the districts dispose of their urban waste in sanitary landfills, which are in a situation of collapse, therefore is needed looking for alternatives to improve the management of this waste, facing this, composting is emerging as a simple and economical technology used for the treatment of the organic component, thus, reducing damage to health and the environment, however, the lack of technical criteria in its application is affecting the quality of the final compost. The objective of this research was to evaluate the technical criteria for processing and the quality of compost based on municipal solid waste in the districts of Leoncio Prado province. The research identified the districts that apply composting to their waste and evaluated the processing technique, physicochemical indicators and determined the quality based on international technical standards. The results show that six out of ten districts apply composting, and the physicochemical indicators contrasted with the quality criteria of the Chilean technical standard (NCH 2880), Colombian 5167 and WHO, correspond to intermediate quality compost (Class B). The evaluated compost does not represent an environmental risk and can be used as an amendment in soil and crop improvement with some restrictions, since it has high moisture, pH and low levels of P, Ca, Mg and K.
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ABSTRACT Several aspects of the development of the peach fruit under tropical conditions are unknown, this information allows agronomic practices to be carried out with technical criteria. Therefore, the objective was to determine the different changes and phenological changes of peach fruit depending on the Growing Degree Days (GDD) in the varieties 'Dorado' and 'Rubidoux', grown in the Colombian high tropics. This study randomly selected 51 trees and 100 flowers per plant that were in full flowering for sampling every 15 days until harvest to determine physical variables such as firmness, color index of the epidermis and pulp, and chemical properties such as soluble solids, titratable acidity, and respiratory rate. From full bloom to harvest, the Dorado and Rubidoux varieties took 1081.8 GDD (153 days) and 1667.1 GDD (205 days) respectively. The firmness increased in the two cultivars during phase 1 of development, then decreased until harvest. The color index of the epidermis and pulp increased during ripening, indicating yellow tones in the two varieties. The soluble solids increased continuously, with final values of 15.9 ± 0.9 and 15.5 ± 0.3 °Brix. The acidity increased during phase 2 and then decreased during ripening. The respiratory rate decreased between phase 1 and 3, with an increase in phase 2, which is related to the lignification of the endocarp in the two cultivars. These results contribute to the understanding of the development of the two peach cultivars under tropical conditions.
RESUMEN Se desconocen varios aspectos del desarrollo del fruto de duraznero en condiciones tropicales, información que permite realizar labores agronómicas con criterio técnico, por tanto, el objetivo fue determinar los diferentes cambios fisicoquímicos y fenológicos del fruto de durazno, en función del tiempo térmico, de las variedades 'Dorado' y 'Rubidoux', cultivados en zonas de trópico alto colombiano. Se seleccionaron al azar 51 árboles y 100 flores/planta, en estado de plena floración. Cada 15 días y hasta la cosecha, se hicieron mediciones de la firmeza, el índice de color de epidermis y pulpa, los sólidos solubles, la acidez titulable y la tasa respiratoria. De plena floración a cosecha, las variedades Dorado y Rubidoux tardaron 1081,8 GDC (153 días) y 1667,1 GDC (205 días), respectivamente. La firmeza presentó un incremento en los dos cultivares durante la fase 1 de desarrollo, luego disminuyó hasta la cosecha. El índice de color de epidermis y pulpa aumentó durante la maduración, con tonalidades amarillas, en las dos variedades. Los sólidos solubles incrementaron de forma continua y en los dos cultivares, con valores finales de 15,9 ± 0,9 y 15,5 ± 0,3 °Brix. La acidez mostró un incremento durante la fase 2 y luego disminuyó durante la maduración. La tasa respiratoria decreció entre la fase 1 y 3, con un incremento en la fase 2, relacionado con la lignificación del endocarpio, en los dos cultivares. Estos resultados contribuyen al entendimiento del desarrollo de los dos cultivares de durazno, bajo condiciones tropicales.
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BACKGROUND The inappropriate use of antibiotics has led to the accelerated growth of resistance to antibiotics. The search for new therapeutic strategies (i.e., antimicrobial peptides-AMPs) has thus become a pressing need. OBJECTIVE Characterising and evaluating Sarconesiopsis magellanica larval fat body-derived AMPs. METHODS Fat body extracts were analysed by reversed-phase high-performance liquid chromatography (RP-HPLC); mass spectrometry was used for characterising the primary structure of the AMPs so found. ProtParam (Expasy) was used for analysing the AMPs' physico-chemical properties. Synthetic AMPs' antibacterial activity was evaluated. FINDINGS Four new AMPs were obtained and called sarconesin III, IV, V and VI. Sarconesin III had an α-helix structure and sarconesins IV, V and VI had linear formations. Oligomer prediction highlighted peptide-peptide interactions, suggesting that sarconesins III, V and VI could form self-aggregations when in contact with the microbial membrane. AMPs synthesised from their native molecules' sequences had potent activity against Gram-positive bacteria and, to a lesser extent, against Gram-negative and drug-resistant bacteria. Sarconesin VI was the most efficient AMP. None of the four synthetic AMPs had a cytotoxic effect. MAIN CONCLUSIONS S. magellanica larval fat body-derived antimicrobial peptides are an important source of AMPs and could be used in different antimicrobial therapies and overcoming bacterial resistance.
Subject(s)
Animals , Diptera , Fat Body , Microbial Sensitivity Tests , Pore Forming Cytotoxic Proteins , Calliphoridae , Larva , Anti-Bacterial Agents/pharmacologyABSTRACT
SUMMARY The purpose of this study was to evaluate physicochemical properties and dissolution studies of furosemide (FUR), hydrochlorothiazide (HCTZ) and nifedipine (NIF), low water solubility drugs, in raw materials and pharmaceutical formulations. Surface and physicochemical characterization techniques -scanning electronic microscopy (SEM), thermogravimetry (TG), X-ray diffraction (XRD) and infrared (IR) spectrometry- as well as physical and physicochemical tests on tablets and capsules were applied as supporting information on drug quality control. Simple, rapid, and efficient UV-Vis methods were developed and validated for the determination of FUR, HCTZ and NIF samples. SEM exhibited considerable differences in the crystal morphological structures. Among the drugs studied, except for furosemide, more than one polymorph was present in the samples. Drug release profiles were satisfactory for all products. FUR and HCTZ tablets exhibited similar dissolution profiles, with very rapid release to the pharmaceutical specialties (reference, similar and generic). For HCTZ tablets, the similar drug (f2= 48.74) is not equivalent to the reference drug. NIF capsules (reference and compounded) showed a release >80% of stated on product labels, in 10 minutes. The results obtained in this study suggest that the quality parameters and drug dissolution profiles may have been influenced by the morphology and size of the crystals, excipients, and technological processes.
RESUMEN El propósito de este estudio fue evaluar las propiedades fisicoquímicas y los estudios de disolución de furosemida (FUR), hidroclorotiazida (HCTZ) y nifedipina (NIF), medicamentos de baja solubilidad en agua, en materias primas y formulaciones farmacéuticas. Técnicas de caracterización fisicoquímica y de superficie: microscopía electrónica de barrido (SEM), termogravimetría (TG), difracción de rayos X (XRD) y espectrometría infrarroja (IR), así como pruebas físicas y fisicoquímicas en tabletas y cápsulas que se aplicaron como información de apoyo sobre el control de calidad. Se desarrollaron y validaron métodos simples, rápidos y eficientes de UV-Vis para la determinación de muestras de FUR, HCTZ y NIF. SEM exhibió diferencias considerables en las estructuras morfológicas de cristal. Entre las drogas estudiadas, a excepción de la furosemida, más de un polimorfo estaba presente en las muestras. Los perfiles de liberación de fármacos fueron satisfactorios para todos los productos. Las tabletas FUR y HCTZ exhibieron perfiles de disolución similares, con una liberación muy rápida a las especialidades farmacéuticas (referencia, similares y genéricas). Para las tabletas de HCTZ, el medicamento similar (f2= 48,74) no es equivalente al medicamento de referencia. Las cápsulas NIF (de referencia y compuestas) mostraron una liberación >80% de la indicada en las etiquetas del producto, en 10 minutos. Los resultados obtenidos en este estudio sugieren que los parámetros de calidad y los perfiles de disolución del fármaco pueden haber sido influenciados por la morfología y el tamaño de los cristales, excipientes y procesos tecnológicos.
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Abstract Formulations containing chitosan incorporated with methanolic fraction of Euphorbia umbellata (Pax) Bruyns, Euphorbiaceae, were studied aiming future applications of this new material as medicine. In order to investigate potential interactions between chitosan and the methanolic fraction (10, 50 and 100% in relation to the amount of chitosan) physicochemical characterization was performed by scanning electron microscopy, density, differential scanning calorimetry, thermogravimetry, X-ray diffraction, Fourier-transform infrared spectroscopy and colorimetry techniques. The phenolic compounds released from the chitosan membranes were evaluated using the Folin-Ciocalteau quantification method; antioxidant and antimicrobial activity were also studied. Increasing amounts of the methanolic fraction added to polymeric matrix produced different numbers of pores on the surface of the membranes, changes in the calorimetric, spectroscopic and crystalline properties as well as color changes, when compared to the inert membrane. These changes can be attributed to chemical interactions that occurred between the structure of the chitosan and the phenolic compounds present in the studied fraction. The matrix samples incorporated with 50 and 100% of the methanolic fraction presented different release profiles of phenolic compounds from the membranes (controlled manner) and promoted antioxidant and antimicrobial activity.
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This study aimed to show that the physicochemical proprieties obtained by Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG), and scanning electronic microscopy (SEM) can be useful tools for evaluating the quality of active pharmaceutical ingredients (APIs) and pharmaceutical products. In addition, a simple, sensitive, and efficient method employing HPLC-DAD was developed for simulta-neous determination of lidocaine (LID), ciprofloxacin (CFX) and enrofloxacin (EFX) in raw materials and in veterinary pharmaceutical formulations. Compounds were separated using a Gemini C18 (250 mm × 4.6 mm, 5 μm) Phenomenex ? column, at a temperature of 25 °C, with a mobile phase containing 10 mM of phosphoric acid (pH 3.29): acetonitrile (85.7:14.3, v/v) and a flow rate of 1.5 mL/min. Physicochemical characterization by TG, FTIR, and SEM of raw materials of LID, CFX, and EFX provided information useful for the evaluation, differentiation, and qualification of raw materials. Finally, the HPLC method was proved to be useful for evaluation of raw material and finished products, besides satisfying the need for an analytical method that allows simultaneous determination of EFX, CFX, and LID, which can also be extended to other matrices and applications.
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ABSTRACT Etodolac is a non-steroidal anti-inflammatory drug (NSAID) and approved by USFDA as a COX2 inhibitor. Although etodolac therapy provides clinical benefits, it is associated with upper gastrointestinal (GI) tract complications also. Etodolac loaded gum Katira microsphere (ELGKM) was prepared by W1/O/W2 emulsion solvent evaporation technique. The gastric irritation properties of orally administered pure etodolac, ELGKM and blank microspheres (without etodolac) were evaluated in experimental rats treated for 6 days. The stomach examination and biochemical investigation of stomach tissue of treated rats indicated that ELGKM formulation remarkably reduced ulcerogenecity as compared to pure etodolac. The anti-inflammatory activities of pure etodolac and ELGKMs were ascertained by the implantation of cotton pellets in rats for 6 days. Based on the results, ELGKMs showed significant anti-inflammatory activities (P<0.01) as compared to control group. The cotton pellets test suggested that ELGKM formulation retained more anti-inflammatory properties among the groups. The hematological changes, biochemical analysis and histopathological studies of subacute toxicity in rats revealed that ELGKM were the effective sustained release formulation in the treatment of chronic pain and inflammation. In conclusion, the physicochemical characterization, pharmacological and toxicological studies suggest that ELGKMs may represent as a potential candidate for sustained drug delivery (10-12 hours) in chronic joint pain related diseases with remarkably diminished gastrointestinal side effects.
Subject(s)
Animals , Male , Rabbits , Rats , Tragacanth/therapeutic use , Evaporation/methods , Etodolac/analysis , Etodolac/therapeutic use , Microspheres , Upper Gastrointestinal Tract/pathologyABSTRACT
ABSTRACT Free films of pullulan-polymethacrylate associations were produced by casting process to develop a novel target-specific material. For characterization, tests of water vapor permeability, swelling index, infrared absorption spectroscopy, thermogravimetric analysis, scanning electron microscopy and mechanical analysis were performed. The polysaccharide concentration directly influenced vapor permeability and swelling, increasing the values of the latter up to five times when added in a proportion of 20% (per weight). The individual properties of each polymer were maintained, and chemical interactions were not detected. The films were found to be thermally stable and they had unaltered mechanical properties with the addition of the polysaccharide. The microscopic analysis revealed rugosity that was proportional to pullulan and disorganization of the polymer network at pH 6.8. These results suggest that this novel material has potential for enteric drug release because of synergism between pH and enzyme dependence.
Subject(s)
Tablets, Enteric-Coated/pharmacology , Drug Delivery Systems/adverse effects , GlucansABSTRACT
ABSTRACT Meloxicam (MLX) is a non-steroidal, anti-inflammatory drug that is prescribed in the treatment of rheumatoid arthritis and osteoarthritis. MLX is practically insoluble in water and exhibits a slow onset of action. In this study, MLX solid dispersions (MLX SDs) were prepared to improve the water solubility of this poorly water-soluble drug. Then orally disintegrating tablets (ODT) of MLX were developed using MLX SD to decrease the onset of action of this drug. MLX, poloxamer 188, and crospovidone of different ratios were melted in molten poloxamer 188 as a hydrophilic carrier. The optimum SD with the highest saturation solubility in water (13.09±0.34 microgram/mL) consisting of MLX: poloxamer 188: crospovidone in the ratio of 1:2:0 was used for the preparation of MLX ODTs. MLX ODTs were prepared by the direct compression method and optimized by the 23 factorial design. The effect of the superdisintegrant concentration, the mannitol-avicel ratio, and the level of compression force on the disintegration time, hardness, and percent of dissolved MLX from MLX ODTs after 30 min was evaluated. DSC and XRD analysis approved an amorphous form of MLX in SDs. The optimized ODT formulation containing 10% of superdisintegrant, and mannitol and avicel in the ratio of 4:1 respectively was compressed using a high level of compression force. The optimized ODT showed hardness (34.37±2.1 N) and friability (1.26±0.04%). This formulation showed a rapid disintegration in 12.66±2.5 seconds, which 82.66±5.1% of the MLX released within 30 min. MLX ODTs, prepared from MLX SD, could be introduced as a suitable dosage form of MLX with improved solubility and the onset of action.
Subject(s)
Solubility , Tablets/analysis , Pharmaceutical Preparations/chemical synthesis , Osteoarthritis/prevention & control , Arthritis, Rheumatoid/prevention & control , Dosage FormsABSTRACT
The objective of the present study was to improve the physicochemical properties of poorly water soluble cefixime by preparing its nanoparticles using a hydrophilic polymer polyvinylpyrrolidone K30 (PVP). The nanoparticles of cefixime were prepared by spray drying technique. A 32 factorial design approach was employed for the optimization of nanoparticle batches. The present model demonstrated significance of factors such as drug to polymer ratio (X1) and feed flow rate (X2) of spray dryer on the production yield (Y1), particle size (Y2) and % drug release at 15 min (Y3). The pure drug and prepared nanoparticles were characterized by Fourier transformation infrared spectroscopy (FTIR), Differential scanning calorimetry (DSC), X-ray powder diffraction (XPRD), Scanning electron microscopy (SEM), particle size, saturation solubility and in vitro drug release. The results of DSC and XPRD revealed transformation of the crystalline nature of cefixime into an amorphous form which was supported by SEM. A significant improvement in solubility and dissolution rate was noticed in case of prepared nanoparticles as compared to pure cefixime. These results suggested that preparation of polymeric nanoparticles by spray drying technique might be a promising approach for improving the physicochemical properties of cefixime.
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ABSTRACT This study aimed to obtain and characterize a microemulsion (ME) containing phenobarbital (PB). The PB was incorporated in the proportion of 5% and 10% in a microemulsion system containing Labrasol(r), ethanol, isopropyl myristate and purified water. The physicochemical characterization was performed and the primary stability of the ME was evaluated. An analytical method was developed using spectrophotometry in UV = 242 nm. The kinetics of the in vitro release (Franz model) of the ME and the emulsion (EM) containing PB was evaluated. The incorporation of PB into ME at concentrations of 5 and 10% did not change pH and resistance to centrifugation. There was an increase in particle size, a decrease of conductivity and a change in the refractive index in relation to placebo ME. The ME remained stable in preliminary stability tests. The analytical method proved to be specific, linear, precise, accurate and robust. Regarding the kinetics of the in vitro release, ME obtained an in vitro release profile greater than the EM containing PB. Thus, the obtained ME has a potential for future transdermal application, being able to compose a drug delivery system for the treatment of epilepsy.
RESUMO O objetivo deste trabalho foi obter e caracterizar uma microemulsão (ME) contendo fenobarbital (FEN). O FEN foi incorporado na proporção de 5% e 10% em um sistema microemulsionado composto por labrasol(r), etanol, miristato de isopropila e água purificada. Foi realizada a caracterização físico-química e avaliada a estabilidade preliminar da ME. Desenvolveu-se um método analítico por espectrofotometria em UV = 242 nm. Foi avaliada a cinética de liberação in vitro (em modelo de Franz) da ME e da emulsão (EM) contendo FEN. A incorporação do FEN em ME nas concentrações de 5 e 10% não alterou o pH e a resistência à centrifugação. Houve aumento do tamanho da partícula, redução da condutividade e alteração do índice de refração em relação à ME placebo. A ME manteve-se estável nos ensaios de estabilidade preliminar. O método analítico demonstrou ser específico, linear, preciso, exato e robusto. Na cinética de liberação in vitro, a ME obteve um perfil de liberação in vitro superior a EM contendo FEN. Desta forma, a ME obtida tem potencial para uma futura aplicação transdérmica, podendo compor um sistema de liberação de fármacos para tratamento da epilepsia.
Subject(s)
Phenobarbital/pharmacokinetics , Emulsions/analysis , Quality Control , Spectrophotometry, Ultraviolet/methods , Kinetics , Nanotechnology/methods , Drug Liberation/drug effectsABSTRACT
ABSTRACT The physicochemical attributes of emulsified systems are influenced by the characteristics of their internal phase droplets (concentration, size and morphology), which can be modified not only by the formulation components, but also by the analytical methodology employed. Thus, the aim of this work involved the physicochemical characterization of cosmetic emulsions obtained from different surfactants, as well as the introduction of the optical coherence tomography (OCT) as the analytical technique employed for the morphological characterization and particle size determination of the formulations. Three emulsions were prepared, differing at the type and concentration of the surfactant used, and their droplet sizes were evaluated through optical microscopy, laser diffraction and OCT. The microscopic analysis and the laser diffraction techniques provided an average particle size minor than 6.0 µm, not detected by the OCT technique, which could identify only bigger particles of the emulsified systems' internal phase. The results testify that OCT was suitable for the morphological characterization of cosmetic emulsions; however, the technique needs to be improved to ensure a better sensitivity in the analysis of smaller particles.
RESUMO Os atributos físico-químicos de sistemas emulsionados são influenciados pelas características de suas gotículas de fase interna (concentração, tamanho e morfologia), as quais podem ser modificadas não apenas pelos componentes da formulação, mas também pela metodologia analítica empregada. Desta forma, o objetivo deste trabalho envolveu a caracterização físico-química de emulsões cosméticas obtidas a partir de diferentes tensoativos, bem como a introdução da tomografia de coerência óptica (OCT) como a técnica analítica utilizada para a caracterização morfológica e determinação do tamanho de partícula das formulações. Três emulsões foram preparadas, diferindo no tipo e concentração do tensoativo empregado, e seus tamanhos de gotícula foram avaliados por meio das técnicas de microscopia óptica, difração a laser e OCT. As técnicas de microscopia óptica e difração a laser forneceram tamanhos de partícula médios menores de 6.0 µm, não detectados pela técnica de OCT, que permitiu apenas a identificação de partículas maiores pertencentes à fase interna dos sistemas emulsionados. Os resultados reforçam a introdução da OCT como metodologia promissora para a caracterização morfológica de emulsões cosméticas; no entanto, a técnica requer aprimoramento para garantir maior sensibilidade na análise de partículas de menor tamanho.
Subject(s)
Tomography, Optical Coherence/methods , Emulsions/analysis , Surface-Active Agents/analysisABSTRACT
Este estudo avaliou as características físico-químicas e a qualidade sanitária da carne ovina comercializada em supermercados e mercados públicos no semiárido potiguar. Foram adquiridas amostras de carne ovina em supermercados locais e em boxes de mercados públicos da região citada. Nos pontos de comercialização, foi aplicado um checklist referente às condições higiênico-sanitárias do ambiente, equipamentos e manipuladores. As amostras foram avaliadas quanto à presença de coliformes a 35 ºC e a 45 ºC, enterobactérias, Staphylococcus spp. e Salmonella sp., além dos parâmetros físico-químicos de pH, cor, perda de peso por cocção, capacidade de retenção de água e força de cisalhamento. Os mercados públicos analisados apresentaram 93,34 % de não conformidade na aplicação do checklist. Quanto aos aspectos microbiológicos, 5 % das amostras apresentaram-se impróprias para o consumo, com contaminação por Salmonella sp. Os resultados encontrados nas análises físico-químicas estavam dentro dos padrões estabelecidos para carne ovina. Não houve diferença significativa entre os espécimes dos dois grupos avaliados, exceto para o parâmetro a* da análise de cor nas amostras de mercado público que apresentaram maior teor de vermelho em relação às amostras de supermercados. Portanto, apesar de apresentarem características físico-químicas satisfatórias, esses produtos são vendidos em condições higiênico-sanitárias precárias, que podem representar risco ao consumidor.
This study evaluated the sanitary and the physicochemical qualities of lamb meat sold in supermarkets and public markets in the semiarid Rio Grande do Norte. Ten samples of lamb meat were obtained in the local supermarketsand ten specimens in the public market food-stalls. These sale points were evaluated by using a checklist concerning the hygiene and sanitary conditions of environment, equipment and handlers. The collected samples were analyzed for detecting coliforms at 35 °C and 45 °C, enterobacteria, Staphylococcus and Salmonella spp., and the physicochemical parameters (pH, color, weight loss by cooking, water retention capacity and shear strength) were assessed. The food-stalls of public market showed 93.34 % of non-compliance to the checklist items. Concerningthe microbiological aspects, 5 % of the samples were unsuitable for consumption, being contaminated with Salmonella spp. The results found in the physicochemical analyzes complied with the standards established forlamb meat. No significant difference among the samples of the both groups was found, except for the a* color parameter in specimens from the public market food-stalls, which showed a higher red color contents.Despite evidencing satisfactory physicochemical characteristics, these products are sold under poor sanitary conditions, which might pose a risk to the consumer.
Subject(s)
Chemical Phenomena , Meat , Food Hygiene , Food Inspection , Sheep , Food QualityABSTRACT
Ischemic brain injury is a major disease which threatens human health and safety. (3, 5, 6-trimethylpyrazin-2-yl) methyl 3-methoxy-4-[(3, 5, 6-trimethylpyrazin-2-yl) methoxy] benzoate (VA-T), a newly discovered lead compound, is effective for the treatment of ischemic brain injury and its sequelae. But the poor solubility of VA-T leads to poor dissolution and limited clinical application. In order to improve the dissolution of VA-T, the pharmaceutical technology of solid dispersions was used in the present study. VA-T/polyvinylpyrrolidone (PVP) solid dispersion was prepared by the solvent method. The dissolution studies were carried out and solid state characterization was evaluated by differential scanning calorimetry (DSC), infrared spectroscopy (IR), x-ray diffraction (XRD) and scanning electron microscopy (SEM). The dissolution rate of VA-T was significantly improved by solid dispersion compared to that of the pure drug and physical mixture. The results of DSC and XRD indicated that the VA-T solid dispersion was amorphous. The IR spectra showed the possible interaction between VA-T and PVP was the formulation of hydrogen bonding. The SEM analysis demonstrated that there was no VA-T crystal observed in the solid dispersions. The ideal drug-to-PVP ratio was 1:5. In conclusion, the solid dispersion technique can be successfully used for the improvement of the dissolution profile of VA-T.
Subject(s)
Benzoates , Chemistry , Brain Ischemia , Drug Therapy , Chemistry, Pharmaceutical , Methods , Drug Delivery Systems , Povidone , Chemistry , SolubilityABSTRACT
The inclusion complexes of poorly water-soluble cephalosporin, cefuroxime axetil (CFA), were prepared withβ-cyclodextrin (βCD) with or without addition of L-arginine (ARG) to improve its physicochemical properties. We also investigated the effect of ARG on complexation efficiency (CE) ofβCD towards CFA in an aqueous medium through phase solubility behaviour according to Higuchi and Connors. Although phase solubility studies showed AL (linear) type of solubility curve in presence and absence of ARG, the CE and association constant (Ks) ofβCD towards CFA were significantly promoted in presence of ARG, justifying its use as a ternary component. The solid systems of CFA withβCD were obtained by spray drying technique with or without incorporation of ARG and characterized by differential scanning ca-lorimetry (DSC), X-ray powder diffractometry (XRPD), scanning electron microscopy (SEM), and sa-turation solubility and dissolution studies. The molecular modeling studies provided a better insight into geometry and inclusion mode of CFA insideβCD cavity. The solubility and dissolution rate of CFA were significantly improved upon complexation withβCD as compared to CFA alone. However, ternary system incorporated with ARG performed better than binary system in physicochemical evaluation. In conclu-sion, ARG could be exploited as a ternary component to improve the physicochemical properties of CFA viaβCD complexation.
ABSTRACT
The aim of this study was to evaluate the physicochemical characteristics of 3 mineralized bovine inorganic biomaterials and correlate them with the dissolution rate. Bio-Oss(r), GenoxInorgânico(r), and Bonefill(r) were examined using field emission gun scanning electron microscopy (FEG-SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), specific surface area (BET), calcium/phosphorous molar ratio and a dissolution assay. Bio-Oss(r) showed a micro- and nanoporous structure consisting of 15-nm hydroxyapatite (HA) crystallites; Genox(r), a microporous structure composed of 39-nm HA crystallites; and Bonefill(r), micro- and nanoporous structure of indeterminable crystallite size. FTIR analysis showed that Bio-Oss(r) and Genox(r) were composed of calcium phosphate. The absorption bands of phosphate were poorly defined in Bonefill(r). By XRD, Bio-Oss(r) was shown to contain peaks related to the carbonated HA, whereas Genox(r) only contained peaks corresponding to HA. The broad bands in Bonefill(r) indicated low crystallinity. Bio-Oss(r) showed a greater surface area and calcium release rate than that of Genox(r). Although all biomaterials were of bovine origin, the different manufacturing processes result in materials with different physicochemical properties and may influence the biological and clinical response.
O objetivo deste estudo foi avaliar as características físico-químicas de 3 biomateriais bovinos inorgânicos mineralizados e correlacioná-los com a taxa de dissolução. Bio-Oss(r), Genox Inorgânico(r) e Bonefill(r) foram caracterizados por microscopia eletrônica de varredura com fonte de emissão por efeito de campo (MEV-FEG), espectroscopia de infravermelho com transformada de Fourier (FTIR), difração de raios-X (DRX), área superficial específica (BET), razão molar cálcio/fósforo e análise da dissolução. Bio-Oss(r) mostrou uma estrutura micro e nanoporosa consistindo de cristalitos de hidroxiapatita (HA) de 15 nm; Genox(r), uma estrutura microporosa composta de cristalitos de HA de 39 nm e Bonefill(r), estrutura micro e nanoporosa com tamanho indeterminável de cristalito. Análises de FTIR mostraram que Bio-Oss(r) e Genox(r) eram compostos por fosfato de cálcio. As bandas de absorção de fosfato encontraram-se pouco definidas no Bonefill(r). Por DRX, Bio-Oss(r) mostrou picos relacionados à HA carbonatada, enquanto Genox(r) somente apresentou picos correspondentes à HA; as bandas alargadas no Bonefill(r) indicaram baixa cristalinidade. Bio-Oss(r) apresentou maior área de superfície e taxa de liberação de cálcio quando comparado ao Genox(r). Embora todos os biomateriais fossem de origem bovina, os diferentes processos de manufatura resultam em materiais com diferentes propriedades físico-químicas e podem influenciar a resposta biológica e clínica.
Subject(s)
Animals , Cattle , Bone Transplantation , Crystallography, X-Ray , Microscopy, Electron, Scanning , Spectroscopy, Fourier Transform InfraredABSTRACT
The aim of this study was to evaluate two important aspects of patent applications of crystalline forms of drugs: (i) the physicochemical characterization of the crystalline forms; and (ii) the procedure for preparing crystals of the blockbuster drug clopidogrel. To this end, searches were conducted using online patent databases. The results showed that: (i) the majority of patent applications for clopidogrel crystalline forms failed to comply with proposed Brazilian Patent Office guidelines. This was primarily due to insufficient number of analytical techniques evaluating the crystalline phase. In addition, some patent applications lacked assessment of chemical/crystallography purity; (ii) use of more than two analytical techniques is important; and (iii) the crystallization procedure for clopidogrel bisulfate form II were irreproducible based on the procedure given in the patent application.
Este trabalho tem como objetivo avaliar dois aspectos importantes em um pedido de patente de formas cristalinas de fármacos: (i) caracterização físico-química das formas cristalinas e (ii)o procedimento de preparo da forma II do fármaco clopidogrel, um blockbuster de vendas. Realizaram-se buscas em bancos de dados patentários on line. Os resultados mostraram que (i) a maioria dos pedidos de patente de formas cristalinas do clopidogrel não se adequam com proposta do INPI devido ao número insuficiente de técnicas analíticas utilizadas na caracterização da fase cristalina. Ainda, em alguns pedidos de patente não há a presença da avaliação da pureza química/cristalográfica; (ii) a importância de se utilizar mais de duas técnicas de avaliação e (iii) que não foi possível a reprodução da cristalização com o procedimento apresentado no pedido de patente.
Subject(s)
Chemistry Techniques, Analytical , Crystallins/classification , Polymorphism, Genetic , Platelet Aggregation Inhibitors/classification , PatentABSTRACT
Mucilage was isolated from the seeds of Diospyros melonoxylon Roxb., a plant growing naturally in the forests of India. Various physico-chemical methods like particle analysis, scanning electron microscopy, differential scanning calorimetry, differential thermal analysis, thermogravimetry analysis, molecular weight by gel permeation chromatography, rheometry, elemental analysis, x-ray diffraction spectrometry, zeta potential, fourier transform infrared spectroscopy, 1D(1H and 13C) (NMR) have been employed to characterize this gum in the present study. Particle analyses suggest that mucilage had particle size in nanometer. SEM analysis suggested that the mucilage had irregular particle size. The glass transition temperature of the gum observed was 78 °C and 74 °C by DSC and DTA respectively. The Thermogravimetry analysis suggested that mucilage had good thermal stability with two stage decomposition. The molecular weight of mucilage was determined to be 8760, by gel permeation chromatography, while the viscosity of mucilage was observed to be 219.1 cP. The XRD pattern of the mucilage indicated a complete amorphous nature. Elemental analysis of the gum revealed specific contents of carbon, hydrogen, nitrogen and sulfur. The major functional groups identified from FT-IR spectrum include 3441 cm-1 (-OH), 1632 cm-1 (-COO-), 1414 cm-1 (-COO-) and 1219 cm-1 (-CH3CO). Analysis of mucilage by paper chromatography and 1D NMR indicated the presence of sugars.
Mucilagem foi isolada de sementes de Diospyros melanoxylon Roxb, uma planta que cresce naturalmente nas florestas da Índia. Vários métodos físico-químicos, como análise de partículas, microscopia electrônica, calorimetria diferencial de varredura, análise térmica diferencial, análise termogravimétrica, massa molecular por cromatografia de permeação em gel, viscosidade, análise elementar, espectrometria de difração de raios-x, potencial zeta, espectroscopia no infravermelho com transformada de Fourier, 1D (1H e 13C) (NMR) foram utilizados no presente estudo para caracterizar essa goma. A análise de partículas sugere que a mucilagem tem tamanho de partícula em nm. A análise SEM sugere que a mucilagem tem tamanho de partícula irregular. Observou-se temperatura de transição vítrea da goma de 78 °C e 74 °C por DSC e DTA, respectivamente. A análise termogravimétrica sugeriu que a mucilagem possuía boa estabilidade térmica, com duas fases de decomposição. A massa molecular da mucilagem foi 8760, por meio de cromatografia de permeação em gel, enquanto que a viscosidade foi 219,1 cP. O padrão de DRX da mucilagem indicou natureza completamente amorfa. Os principais grupos funcionais identificados a partir do espectro de FT-IR foram: 3441 cm-1 (-OH), 1632 cm-1 (-COO-), 1414 cm-1 (-COO-) e 1.219 cm-1 (CH3CO-). As análises de mucilagem por cromatografia em papel e 1D RMN indicaram a presença de açúcares.
Subject(s)
/analysis , Diospyros , Plant Mucilage/analysis , zeta Potential/classification , Spectroscopy, Fourier Transform Infrared , Diospyros/classificationABSTRACT
Karpoora Cinthamani Mathirai (KCM) is a traditional Siddha medicinal preparation using to treat Arthritis associated with fever narrated in the text Anubhoga Vaithiya Navaneetham. This formulation has the detoxified ingredients such as Hydrargyrum subchloride and Croton tiglium seeds. The aim was to establish a fingerprint to ensure the quality and safety of KCM. Physicochemical characterization of KCM was carried out using qualitative biochemical analysis and modern techniques such as Fourier transform infra-red spectroscopy, inductively coupled plasma analysis and scanning electron microscopy. Physical evaluation revealed that KCM is a light green colour pill, neutral nature and having solubility in water and HCl with stabilized particle size distribution of 3μ. A clearly identifiable fraction of KCM particles were below 50 nm. The presence of nano sized particles and functional groups carboxylic acids and nitrocompounds in KCM might impart the therapeutic property. Trace elemental analysis of KCM revealed that heavy metals like arsenic, cadmium, mercury and lead were below the deduction limit. Further, elemental analysis of KCM revealed the presence of minerals like calcium, iron, potassium, sodium, and phosphorus under acceptable limits at the prescribed dose of KCM.
ABSTRACT
Objective:To isolate and identify Bacillus subtilis (B. subtilis) from soil and to characterize and partially purify the bacteriocin. To evaluate the antimicrobial activity against four diabetic foot ulcer bacterial pathogens. Methods:Genotypic identification was done based on Bergey’s manual of systemic bacteriology. Antimicrobial susceptibility test was done by Kirby-Bauer disc diffusion method. Colonies were identified by colony morphology and biochemical characterization and also compared with MTCC 121 strain. Further identification was done by 16S rRNA sequencing. Inhibitory activities of partially purified bacteriocin on all the DFU isolates were done by agar well diffusion method. The strain was identified to produce bacteriocin by stab overlay assay. Bacteriocin was extracted by organic solvent extraction using chloroform, further purified by HPLC and physical, and chemical characterization was performed. Results: The four isolates showed high level of resistance to amoxyclav and sensitivity to ciprofloxacin. HPLC purification revealed that the extracts are bacteriocin. The phylogenetic tree analysis results showed that the isolate was 99%related to B. subtilis BSF01. The results reveled activity to all the four isolates and high level of activity was seen in case of Klebsiella sp. Conclusions:Partially purified bacteriocin was found to have antimicrobial activity against the four diabetic foot ulcer bacterial pathogens, which can thus be applied as a better drug molecule on further studies. The strain B. subtilis are found to be safe for use and these antimicrobial peptides can be used as an antimicrobial in humans to treat DFU bacterial pathogens.