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1.
Rev. chil. nutr ; 47(2): 171-180, abr. 2020. tab, graf
Article in Spanish | LILACS | ID: biblio-1115486

ABSTRACT

La bioaccesibilidad de un nutriente en un alimento sirve para determinar la calidad nutricional de éste para el consumo humano. El arroz es uno de los alimentos más importantes en la dieta por su gran aporte calórico y nutricional. El objetivo de este estudio fue analizar la bioaccesibilidad in vitro del zinc en arroz mediante espectrofotometría ultravioleta-visible y espectrometría de absorción atómica de llama y su relación con el contenido de ácido fítico. El porcentaje de bioaccesibilidad del zinc, respecto al porcentaje de ácido fítico, presentó una relación logarítmica inversamente proporcional (r= −0,669; p<0,05). Los valores porcentuales de bioaccesibilidad del zinc y ácido fítico en las líneas de arroz evaluadas se hallaron en un rango de 1,98,7% y 0,039-0,946% respectivamente. Se encontró que el ácido fítico afecta la bioaccesibilidad del zinc y que ésta no estuvo ligada a la concentración total del zinc presente en las líneas de arroz evaluadas. Las técnicas implementadas para cuantificar el zinc dializado presentaron diferencias significativas y se mostró que la técnica ultravioleta-visible no fue apta para este tipo de ensayos.


The bioavailability of a nutrient in a food serves to determine the nutritional quality for human consumption. Rice is one of the most important foods in diet due to its caloric and nutritional contribution. The objective of this study was to analyze the in vitro bioavailability of zinc in rice by ultraviolet-visible spectrophotometry and flame atomic absorption spectrometry and its relationship with phytic acid content. The percentage of zinc bioaccessibility with respect to phytic acid percentage, showed an inverse proportional logarithmic relationship (r= −0.669; p<0.05). The percentage values of zinc bioavailability and phytic acid in the evaluated rice varieties had a range of 1.9-8.7% and 0.039-0.946%, respectively. Phytic acid affected the bioaccessibility of zinc and was not linked to the total concentration of zinc present in the rice lines evaluated. The techniques implemented to quantify zinc dialyzed presented significant differences. It was shown that the ultraviolet-visible technique was not suitable for this type of assay.


Subject(s)
Phytic Acid/analysis , Oryza , Spectrophotometry, Ultraviolet , Zinc/analysis , In Vitro Techniques , Biological Availability , Atomic Absorption Spectroscopy , Absorption , Minerals/analysis , Nutritive Value
2.
Bol. latinoam. Caribe plantas med. aromát ; 19(2): 188-206, mar. 2020. ilus, tab
Article in English | LILACS | ID: biblio-1104201

ABSTRACT

The present study aimed to screen the Rhazya stricta Decne root for its antihyperglycemic and antioxidants potential through invitro assays along with phytochemical and elemental analyses. The crude extract was prepared through maceration and fractionated using solvent-solvent extraction technique. The spectroscopic studies indicated the presence of various phytochemical classes in the extract and its fractions. The antioxidant assays showed notable results along with a good concentration of phenolic and flavonoid contents. Enzyme inhibition assays demonstrated glucose-lowering effects by inhibiting the enzyme activity which could reduce post-prandial blood glucose level. The Dipeptidyl peptidase-IV (DPP-IV) inhibition assay results showed the novel DPP-IV inhibition activity of the plant extract and all fractions showed noteworthy enzyme inhibition and antihyperglycemic activity. Conclusively, the Rhazya stricta root extract displayed its antioxidant and antihyperglycemic potential due to the presence of various classes of phytochemicals and micro-nutrients.


El presente estudio tuvo como objetivo examinar la raíz de Rhazya stricta Decne por su potencial antihiperglicémico y antioxidante a través de ensayos in vitro junto con análisis fitoquímicos y elementales. El extracto crudo se preparó por maceración y se fraccionó usando una técnica de extracción solvente-solvente. Los estudios espectroscópicos indicaron la presencia de varias clases fitoquímicas en el extracto y sus fracciones. Los ensayos antioxidantes mostraron resultados notables junto con una importante concentración de contenido fenólico y flavonoide. Los ensayos de inhibición enzimática demostraron efectos reductores de la glucosa al inhibir la actividad enzimática que podría reducir el nivel de glucosa posprandial en sangre. Los resultados del ensayo de inhibición de Dipeptidyl peptidase-IV (DPP-IV) mostraron la nueva actividad de inhibición de DPP-IV del extracto de la planta y todas las fracciones mostraron una notable inhibición enzimática y actividad antihiperglicémica. En conclusión, el extracto de raíz de Rhazya stricta Decne mostró su potencial antioxidante y antihiperglicémico debido a la presencia de varias clases de fitoquímicos y micronutrientes.


Subject(s)
Plant Extracts/pharmacology , Apocynaceae/chemistry , Hypoglycemic Agents/pharmacology , Antioxidants/pharmacology , Phenols/analysis , Spectrophotometry, Ultraviolet , Flavonoids/analysis , Blood Glucose/drug effects , In Vitro Techniques , Plant Extracts/chemistry , Spectroscopy, Fourier Transform Infrared , Plant Roots/chemistry , Dipeptidyl-Peptidases and Tripeptidyl-Peptidases/antagonists & inhibitors , Phytochemicals , Hypoglycemic Agents/chemistry , Antioxidants/chemistry
3.
Bol. latinoam. Caribe plantas med. aromát ; 18(3): 277-288, mayo 2019. ilus
Article in English | LILACS | ID: biblio-1007989

ABSTRACT

Neurolaena lobata (L.) R.Br. ex Cass. (Asteraceae)Is a popular folk remedy for in Central America. The plant is of commercial value in Guatemala but so far there is not any monograph to guide regional laboratories on ensuring identity and chemical tests for this species. As identity test we here run macro and micro morphoanatomical studies of the characters of the vegetative organs. We also developed standard chemical tests for quality by both TLC and HPLC for infusions and tinctures of varying alcoholic strength. Their radical scavenging activities in DPPH and NO were also measured. Macro and micro morphoanatomical characters of the vegetative organs present a set of characteristics to facilitate the identification of dry powdered samples of this species. We developed optimal conditions for the TLC and HPLC phytochemical fingerprints of the 4 most common pharmacopoeial liquid herbal preparations from this herbal drug, namely infusion, 70%, 45% and 20% hydroalcoholic tinctures. Our work provides the Latin-American industry with a set of analyses to establish the identity and chemistry of N. lobata samples for quality control purposes.


Neurolaena lobata (L.) R.Br. ex cass. (Asteraceae) es un remedio popular popular en América Central. La planta tiene un valor comercial en Guatemala, pero hasta el momento no existe una monografía que guíe a los laboratorios regionales para garantizar la identidad y las pruebas químicas para esta especie. Como prueba de identidad proponemos estudios macro y micro morfoanatómicos de los caracteres de los órganos vegetativos. También desarrollamos pruebas químicas de calidad mediante CCF y CLAR para infusiones y tinturas de grado alcohólico variable. También se midieron sus actividades de captación de radicales en DPPH y NO. Los caracteres macro y micro morfoanatómicos de los órganos vegetativos presentan un conjunto de características para facilitar la identificación de muestras de polvo seco de esta especie. Desarrollamos condiciones óptimas para las huellas dactilares fitoquímicas de CCF y CLAR de las 4 preparaciones herbales líquidas farmacopéicas más comunes de esta droga herbal, a saber, infusión, 70%, 45% y 20% tinturas hidroalcohólicas. Nuestro trabajo proporciona a la industria latinoamericana un conjunto de análisis base para establecer la identidad y la química de las muestras de N. lobata con fines de control de calidad.


Subject(s)
Asteraceae/anatomy & histology , Asteraceae/chemistry , Phytochemicals/analysis , Quality Control , Spectrophotometry, Ultraviolet , Free Radical Scavengers , Chromatography, High Pressure Liquid , Chromatography, Thin Layer , Asteraceae/ultrastructure , Guatemala , Microscopy
4.
Rev. Soc. Bras. Med. Trop ; 50(4): 499-505, July-Aug. 2017. tab, graf
Article in English | LILACS | ID: biblio-897000

ABSTRACT

Abstract INTRODUCTION: Primaquine (PQ) diphosphate is an 8-aminoquinoline antimalarial drug with unique therapeutic properties. It is the only drug that prevents relapses of Plasmodium vivax or Plasmodium ovale infections. In this study, a fast, sensitive, cost-effective, and robust method for the extraction and high-performance liquid chromatography with diode array ultraviolet detection (HPLC-DAD-UV ) analysis of PQ in the blood plasma was developed and validated. METHODS: After plasma protein precipitation, PQ was obtained by liquid-liquid extraction and analyzed by HPLC-DAD-UV with a modified-silica cyanopropyl column (250mm × 4.6mm i.d. × 5μm) as the stationary phase and a mixture of acetonitrile and 10mM ammonium acetate buffer (pH = 3.80) (45:55) as the mobile phase. The flow rate was 1.0mL·min-1, the oven temperature was 50OC, and absorbance was measured at 264nm. The method was validated for linearity, intra-day and inter-day precision, accuracy, recovery, and robustness. The detection (LOD) and quantification (LOQ) limits were 1.0 and 3.5ng·mL-1, respectively. The method was used to analyze the plasma of female DBA-2 mice treated with 20mg.kg-1 (oral) PQ diphosphate. RESULTS: By combining a simple, low-cost extraction procedure with a sensitive, precise, accurate, and robust method, it was possible to analyze PQ in small volumes of plasma. The new method presents lower LOD and LOQ limits and requires a shorter analysis time and smaller plasma volumes than those of previously reported HPLC methods with DAD-UV detection. CONCLUSIONS: The new validated method is suitable for kinetic studies of PQ in small rodents, including mouse models for the study of malaria.


Subject(s)
Animals , Female , Primaquine/blood , Antimalarials/blood , Primaquine/pharmacokinetics , Spectrophotometry, Ultraviolet , Chromatography, High Pressure Liquid , Mice , Antimalarials/pharmacokinetics
5.
Braz. j. infect. dis ; 21(1): 57-62, Jan.-Feb. 2017. tab, graf
Article in English | LILACS | ID: biblio-839184

ABSTRACT

Abstract The mechanisms involved in the uncommon resistance phenotype, carbapenem resistance and broad-spectrum cephalosporin susceptibility, were investigated in 25 Pseudomonas aeruginosa clinical isolates that exhibited this phenotype, which were recovered from three different hospitals located in São Paulo, Brazil. The antimicrobial susceptibility profile was determined by CLSI broth microdilution. β-lactamase-encoding genes were investigated by PCR followed by DNA sequencing. Carbapenem hydrolysis activity was investigated by spectrophotometer and MALDI-TOF assays. The mRNA transcription level of oprD was assessed by qRT-PCR and the outer membrane proteins profile was evaluated by SDS-PAGE. Genetic relationship among P. aeruginosa isolates was assessed by PFGE. Carbapenems hydrolysis was not detected by carbapenemase assay in the carbapenem-resistant and cephalosporin-susceptible P. aueruginosa clinical isolates. OprD decreased expression was observed in all P. aeruginosa isolates by qRT-PCR. The outer membrane protein profile by SDS-PAGE suggested a change in the expression of the 46 kDa porin that could correspond to OprD porin. The isolates were clustered into 17 genotypes without predominance of a specific PFGE pattern. These results emphasize the involvement of multiple chromosomal mechanisms in carbapenem-resistance among clinical isolates of P. aeruginosa, alert for adaptation of P. aeruginosa clinical isolates under antimicrobial selective pressure and make aware of the emergence of an uncommon phenotype among P. aeruginosa clinical isolates.


Subject(s)
Humans , Pseudomonas aeruginosa/drug effects , Carbapenems/pharmacology , Cephalosporins/pharmacology , beta-Lactam Resistance/genetics , Anti-Bacterial Agents/pharmacology , Phenotype , Pseudomonas aeruginosa/enzymology , Pseudomonas aeruginosa/genetics , Spectrophotometry, Ultraviolet , Bacterial Outer Membrane Proteins , Bacterial Proteins/metabolism , beta-Lactamases/metabolism , Brazil , DNA, Bacterial , Microbial Sensitivity Tests , Electrophoresis, Gel, Pulsed-Field , Sequence Analysis, DNA , Porins/metabolism , Reverse Transcriptase Polymerase Chain Reaction
6.
Braz. J. Pharm. Sci. (Online) ; 53(1): e15181, 2017. tab, graf
Article in English | LILACS | ID: biblio-839459

ABSTRACT

Sildenafil citrate (SILC) is a potent phosphodiesterase-5 inhibitor used for erectile dysfunction and pulmonary hypertension. This study shows two simple, fast and alternative analytical methods for SILC determination by non-aqueous titration and by derivative ultraviolet spectrophotometry (DUS) in active pharmaceutical ingredient and/or dosage forms. The quantitation method of SILC active pharmaceutical ingredient by non-aqueous acid-base titration was developed using methanol as solvent and 0.1 mol/L of perchloric acid in acetic acid as titrant. The endpoint was potentiometrically detected. The non-aqueous titration method shows satisfactory repeatability and intermediate precision (RSD 0.70-1.09%). The neutralization reaction occurred in the stoichiometric ratio 1:1 in methanol. The determination of SILC active pharmaceutical ingredient or dosage forms by DUS was developed in the linear range from 10 to 40 µg/mL, in 0.01 mol/L HCl, using the first order zero-peak method at λ 256 nm. The DUS method shows selectivity toward tablets excipients, appropriate linearity (R2 0.9996), trueness (recovery range 98.86-99.30%), repeatability and intermediate precision in three concentration levels (RSD 1.17-1.28%; 1.29-1.71%, respectively). Therefore, the methods developed are excellent alternatives to sophisticated instrumental methods and can be easily applied in any pharmaceutical laboratory routine due to simple and fast executions.


Subject(s)
Spectrophotometry, Ultraviolet/methods , Titrimetry/methods , Sildenafil Citrate/analysis , Tablets/pharmacology , Vasodilator Agents/classification
7.
Rev. Soc. Bras. Med. Trop ; 49(6): 693-697, Dec. 2016. tab, graf
Article in English | LILACS | ID: biblio-829668

ABSTRACT

Abstract: INTRODUCTION: Dengue fever is a viral disease transmitted by the Aedes aegypti Linn. (1792) (Diptera: Culicidae) mosquito, which is endemic in several regions of Brazil. Alternative methods for the control of the vector include botanical insecticides, which offer advantages such as lower environmental contamination levels and less likelihood of resistant populations. Thus, in this study, the ability of botanical insecticide formulations to inhibit the activity of the liver enzymes serum cholinesterase and malate dehydrogenase was evaluated. METHODS: Inhibition profiles were assessed using in vitro assays for cholinesterase and malate dehydrogenase activity and quantitated by ultraviolet-visible spectroscopy at 410nm to 340nm. RESULTS Insecticide products formulated from cashew nutshell liquid [A] and ricinoleic acid [B] showed cholinesterase activity levels of 6.26IU/mL and 6.61IU/mL, respectively, while the control level for cholinesterase was 5-12IU/mL. The products did not affect the level of 0.44IU/mL established for malate dehydrogenase, as the levels produced by [A] and [B] were 0.43IU/mL and 0.45IU/mL, respectively. CONCLUSIONS Our findings show that in vitro testing of the formulated products at concentrations lethal to A. aegypti did not affect the activity of cholinesterase and malate dehydrogenase, indicating the safety of these products.


Subject(s)
Humans , Animals , Ricinoleic Acids/pharmacology , Cholinesterase Inhibitors/pharmacology , Cholinesterases/drug effects , Anacardium/chemistry , Insecticides/pharmacology , Liver/enzymology , Malate Dehydrogenase/antagonists & inhibitors , Spectrophotometry, Ultraviolet , In Vitro Techniques , Ricinoleic Acids/isolation & purification , Aedes , Insect Vectors/drug effects , Insecticides/isolation & purification
8.
Electron. j. biotechnol ; 19(6): 70-78, Nov. 2016. ilus
Article in English | LILACS | ID: biblio-840316

ABSTRACT

Background: Many buildings in Egypt e.g. museums, mosques and churches, do not possess controlled environments for minimizing the risks of damage of wooden artifacts due to the growth of fungi. Fungal damage usually appears as change in wood color, appearance of stains, and sometimes deformation of wooden surfaces. In this study we focused on the effect that some fungi exert on the properties of wooden artifacts and evaluated the effectiveness of different concentrations of chitosan on their protection against damage by mold fungi. Results: Samples were collected from different monuments and environments, and fungi growing on them were isolated and identified. The isolated Penicillium chrysogenum, Aspergillus flavus and /Aspergillus niger strains were used for the infestation of new pitch pine samples. The results revealed that the lightness of samples infected with any of the tested fungi decreased with increasing incubation times. XRD analysis showed that the crystallinity of incubated samples treated individually with the different concentrations of chitosan was lower than the crystallinity of infected samples. The crystallinity index measured by the first and the second method decreased after the first and second months but increased after the third and fourth months. This may due to the reducing of amorphous part by enzymes or acids produced by fungi in wooden samples. Conclusions: The growth of fungi on the treated wood samples decreased with increasing the concentration of chitosan. Hence, it was demonstrated that chitosan prevented fungal growth, and its use could be recommended for the protection of archeological wooden artifacts.


Subject(s)
Antifungal Agents/pharmacology , Chitosan/chemistry , Fungi/drug effects , Wood/microbiology , Archaeology , Aspergillus flavus/drug effects , Aspergillus flavus/isolation & purification , Aspergillus niger/drug effects , Aspergillus niger/isolation & purification , Chitosan/pharmacology , Crystallization , Penicillium chrysogenum/drug effects , Penicillium chrysogenum/isolation & purification , Spectrophotometry, Ultraviolet
9.
Braz. j. pharm. sci ; 52(2): 251-264, Apr.-June 2016. tab, graf
Article in English | LILACS | ID: lil-794999

ABSTRACT

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)
Emulsions/analysis , Phenobarbital/pharmacokinetics , Drug Liberation/drug effects , Kinetics , Nanotechnology/methods , Quality Control , Spectrophotometry, Ultraviolet/methods
10.
Rev. cuba. farm ; 50(1)ene.-mar. 2016. ilus, graf, tab
Article in Spanish | LILACS, CUMED | ID: biblio-844862

ABSTRACT

Introducción: la colchicina es una alternativa terapéutica indicada por vía oral para las crisis agudas de la gota. Se formula en tabletas de baja dosificación debido a su elevada toxicidad. Los Laboratorios Dr.A. Bjarner C.A producen las tabletas de Artrichine y se requiere de un método sencillo, pero a la vez confiable para realizar el control de calidad de este producto terminado, que considere la solubilidad en etanol, la presencia de cromóforos y la composición de la formulación de la colchicina. Objetivo: se propuso validar un método por espectrofotomería UV útil para el control de rutina. Métodos: se aplicó un método simple, que se modifica del método establecido en la Farmacopea Británica del 2009 para las tabletas, por espectrofotometría UV directa. Se basa en la extracción del analito en etanol absoluto y su posterior determinación a 350 nm. La validación del método se realizó a través de los parámetros linealidad, precisión, exactitud y especificidad frente a los componentes de la formulación. Resultados: se estableció una metodología analítica muy sencilla para obtener una solución transparente a partir de la forma terminada, de igual concentración a la solución de referencia. El cumplimiento satisfactorio de todos los criterios de aceptación establecidos para los parámetros evaluados permitió demostrar la validez del método en estudio para el control de calidad en el rango de 50 a 150 por ciento (5-15 µg/mL). Conclusiones: el método por espectrofotometría UV resultó específico, lineal, exacto y preciso para su aplicación al control de calidad de la colchicina en Artrichine tabletas(AU)


Introduction: colchicine is a therapeutic alternative orally prescribed for acute gout. It is formulated as low dose tables due to its high toxicity. Dr A. Bjarner C.A laboratories manufacture Artrichine tablets and it requires a simple and reliable method to conduct quality control of the finished product that will consider ethanol-soluble characteristics, presence of chromophores and composition of colchicine formulation. Objective: to validate an ultraviolet spectrophotometry-based method for the routine quality control. Methods: a simple method by direct UV spectrophotometry which is modified from the set method of the British Pharmacopeia 2009 for tablets. It is based on the analyte extraction in absolute ethanol and the estimation at 350 nm. The method was validated on account of linearity, precision, accuracy and specificity against the formulation components. Results: a very simple analytical methodology was established to obtain a transparent solution from the finished form, with the same concentration as that of the reference solution. The satisfactory compliance with all the acceptance criteria for the evaluated parameters allowed proving the validity of the study method for the quality control in the 50 to 150 percent range (5-15 ug/ml). Conclusions: the UV spectrophotometry-based method proved to be specific, linear, accurate and precise for the quality control of colchicine in Artrichine tablets(AU)


Subject(s)
Humans , Colchicine/therapeutic use , Reference Drugs , Validation Studies as Topic , Gout/therapy , Spectrophotometry, Ultraviolet/methods
11.
Braz. j. pharm. sci ; 51(4): 811-821, Oct.-Dec. 2015. tab, graf
Article in English | LILACS | ID: lil-778408

ABSTRACT

abstract Daptomycin is the first approved drug from a new class of antimicrobials, the cyclic lipopeptides, and is a very important antimicrobial agent in current clinical practice. Currently, there are no "green" analytical methods described in the literature to analyze the typical pharmaceutical dosage form of daptomycin. Thus, the aim of this work was to validate an environment-friendly spectrophotometric method in the UV region, for the analysis of daptomycin as a lyophilized powder. Water was used as diluent and the analyses were carried out on a spectrophotometer at 221 nm. The method met all validation requirements of the ICH guidelines, over a concentration range of 6-21 µg mL-1. A Student's t-test demonstrated that the proposed method was comparable to an HPLC method previously validated. Thus, the validated spectrophotometric method could quantify daptomycin in a powder form for injectable solutions, while being an economical, rapid, and "green" alternative for routine analysis in quality control.


resumo A daptomicina é o primeiro membro aprovado de uma nova classe de antimicrobianos, os lipopeptídeos cíclicos, e é muito importante para a prática clínica atualmente. Não existem métodos analíticos "verdes" descritos na literatura para a análise da daptomicina na forma farmacêutica. Desta forma, o objetivo deste trabalho foi a validação de método espectrofotométrico na região do UV ambientalmente favorável para análise da daptomicina em pó liofilizado. A água foi escolhida como diluente e as análises foram realizadas em 221 nm. O método atendeu a todas as exigências de validação dos guias do ICH, na faixa de 6-21 µg mL-1. Teste t de Student mostrou que o método proposto é intercambiável com método de HPLC previamente validado. Assim, o método espectrofotométrico validado é capaz de quantificar a daptomicina em pó para solução injetável e é uma opção econômica, rápida e "verde" para análises de rotina do controle de qualidade deste fármaco.


Subject(s)
Chemistry, Pharmaceutical/classification , Daptomycin/analysis , Spectrophotometry, Ultraviolet/statistics & numerical data , Anti-Infective Agents/analysis , Quality Control
12.
Braz. j. pharm. sci ; 51(4): 833-837, Oct.-Dec. 2015. tab, graf
Article in English | LILACS | ID: lil-778419

ABSTRACT

abstract Ultraviolet spectrophotometric (UV) and Liquid Chromatographic (LC) methods for the determination of mianserin hydrochloride in pharmaceutical formulation were developed and validated. The various parameters, such as specificity, linearity, precision and accuracy were studied according to International Conference on Harmonization (ICH, 2005). For UV method, mianserin hydrochloride was determinate at 278 nm using HCl 0.1 M as the solvent. The response was linear in the concentration range of 20.0 - 140.0 µg/mL (r = 0.9998). Precision data evaluated by relative standard deviation was lower than 2%. The UV method was simple, rapid and low cost. Chromatographic analyses were performed in an Ace C18 column and the mobile phase was composed of methanol, 50 mM monobasic potassium phosphate buffer and 0.3% triethylamine solution adjusted to pH 7.0 with phosphoric acid 10% (85:15). LC method was specific, linear, precise, exact and robust. The results confirmed that the both methods are valid and useful to the routine quality control of mianserin hydrochloride in coated tablets. Statistical analysis by Student´s t-test showed no significant difference between the results obtained by UV and LC methods.


resumo Os métodos por espectrofotometria na região do ultravioleta (UV) e por cromatografia líquida (CL) para determinação do cloridrato de mianserina na forma farmacêutica foram desenvolvidos e validados. Os vários parâmetros, como especificidade, linearidade, precisão e exatidão foram avaliados de acordo com o International Conference on Harmonization (ICH, 2005). Para o método de UV, o cloridrato de mianserina foi determinado utilizando o comprimento de onda de 278 nm e HCl 0,1 M como solvente. A resposta foi linear na faixa de concentração de 20,0 a 140,0 µg/Ml (r = 0,9998). A precisão foi avaliada pelo valor de desvio padrão relativo (DPR) inferior a 2%. O método por UV é simples, rápido e de baixo custo. As análises cromatográficas foram realizadas em uma coluna Ace C18 e a fase móvel foi composta por metanol, tampão fosfato de potássio monobásico 50 mM com 0,3% de trietilamina com o pH ajustado para 7,0 com ácido fosfórico 10% (85:15). O método de CL foi específico, linear, preciso, exato e robusto. Os resultados confirmam que ambos os métodos são válidos e úteis para o controle de qualidade do cloridrato de mianserina em comprimidos revestidos. A análise estatística por teste t de Student não mostrou diferença significativa entre os resultados obtidos para os métodos de UV e CL.


Subject(s)
Mianserin/pharmacokinetics , Spectrophotometry, Ultraviolet/statistics & numerical data , Chromatography, Liquid/statistics & numerical data , Evaluation Studies as Topic/analysis , Tablets/pharmacokinetics
13.
Braz. j. pharm. sci ; 51(1): 221-231, Jan-Mar/2015. tab, graf
Article in English | LILACS | ID: lil-751366

ABSTRACT

This study describes the development and evaluation of stability-indicating liquid chromatographic (LC) and UV spectrophotometric methods for the quantification of ciprofibrate (CPF) in tablets and capsules. Isocratic LC separation was achieved on a RP18 column using a mobile phase of o-phosphoric acid (0.1% v/v), adjusted to pH 3.0 with triethylamine (10% v/v) and acetonitrile (35:65 v/v), with a flow rate of 1.0 mL min-1. Detection was achieved with a photodiode array detector at 233 nm. For the spectrophotometric analysis, ethanol and water were used as the solvent and a wavelength of 233 nm was selected for the detection. The methods were validated according to International Conference on Harmonization (ICH) guidelines for validating analytical procedures. Statistical analysis showed no significant difference between the results obtained by the two methods. The proposed methods were successfully applied to the CPF quality-control analysis of tablets and capsules.


Este estudo descreve o desenvolvimento e avaliação de método indicativo da estabilidade por cromatografia líquida (LC) e método por espectrofotometria UV para quantificação de ciprofibrato (CPF) em comprimidos e cápsulas. No método por cromatografia líquida as análises foram realizadas isocraticamente em coluna de fase reversa C18, utilizando fase móvel composta por ácido o-fosfórico (0.1% v/v) pH 3.0, ajustado com trietilamina (10% v/v), e acetonitrila (35:65 v/v), com fluxo de 1,0 mL min-1. A detecção foi realizada em detector de arranjo de diodos a 233 nm. Na análise espectrofotométrica, etanol e água foram utilizados como solventes e o comprimento de onda de 233 nm foi selecionado para a detecção do fármaco. Os métodos foram validados de acordo com as diretrizes do International Conference on Harmonization (ICH). A análise estatística não mostrou diferença significativa entre os resultados obtidos pelos dois métodos. Os métodos foram aplicados com sucesso para análises de controle de qualidade do ciprofibrato em comprimidos e cápsulas.


Subject(s)
Chromatography, Liquid/methods , Tablets/pharmacokinetics , Capsules/pharmacokinetics , Drug Stability , Evaluation Studies as Topic/analysis , Spectrophotometry, Ultraviolet/classification
14.
Braz. j. pharm. sci ; 51(1): 183-191, Jan-Mar/2015. tab, graf
Article in English | LILACS | ID: lil-751370

ABSTRACT

The aim of this study was to develop and validate a UV spectrophotometric method for determination of LPSF/AC04 from inclusion complex and encapsulated into liposomes. The validation parameters were determined according to the International Conference on Harmonisation (ICH) and National Health Surveillance Agency (ANVISA) guidelines. LPSF/AC04 was determined at 250 nm in methanol by a UV spectrophotometric method, exhibiting linearity in the range from 0.3 to 2 µg.mL−1 (Absorbance=0.18068 x [LPSF/AC04 µg.mL-1] + 0.00348), (r2=0.9995). The limits of detection and quantification were 0.047µg.mL−1 and 0.143µg.mL−1, respectively. The method was accurate, precise, reproducible and robust since all the samples analyzed had coefficient of variation of less than 5% and no statistically significant difference between theoretical and practical concentrations was detected. Thus, a rapid, simple, low cost and sensitive spectrophotometric method was developed and validated for determining the content of inclusion complex and liposomes containing LPSF/AC04.


O objetivo deste estudo foi desenvolver e validar um método espectrofotométrico para determinação do LPSF/AC04 em complexo de inclusão e encapsulado em lipossomas. Os parâmetros de validação foram determinados de acordo com o International Conference on Harmonisation (ICH) e Agência Nacional de Vigilância Sanitária (ANVISA). OLPSF/AC04 foi determinado a 250 nm em metanol pelo método espectrofotométrico UV, que apresenta linearidade na faixa de 0,3 a 2 µg/mL (Absorbância = 0,18068 x [LPSF/AC04 µg/mL] + 0,00348), (r2 = 0,9995). Os limites de detecção e quantificação foi 0,047 µg/mL e 0,143 µg/mL, respectivamente. O método foi exato, preciso, reprodutível e robusto e todas as amostras analisadas apresentaram coeficiente de variação menor que 5% e não houve diferença estatisticamente significante entre a concentração teórica e a prática. Assim, um método espectrofotométrico rápido, simples, sensível e de baixo custo foi desenvolvido e validado para determinar o conteúdo do LPSF/AC04 em complexos de inclusão e encapsulados em lipossomas.


Subject(s)
Liposomes/pharmacokinetics , Spectrophotometry, Ultraviolet/methods , Validation Study , Evaluation Studies as Topic/analysis
15.
São Paulo; s.n; s.n; fev. 2015. 96 p. tab, graf, ilus.
Thesis in Portuguese | LILACS | ID: biblio-836741

ABSTRACT

A hipertensão é uma doença crônica não transmissível e mais freqüente na população sendo o principal fator de risco para complicações cardiovasculares, tais como acidente vascular cerebral e infarto agudo do miocárdio. Na presente pesquisa estão sendo estudados os fármacos utilizados no tratamento da hipertensão mais especificamente, os bloqueadores do canal de cálcio do grupo diidropiridínicos: besilato de anlodipino, nifedipino e nimodipino. O objetivo desse trabalho foi verificar a estabilidade intrínseca dos fármacos besilato de anlodipino, nifedipino e nimodipino, para isto foram utilizadas as seguintes técnicas: testes indicativos de estabilidade utilizando as técnicas de espectrofotometria na região do Ultravioleta/Visível (UV/VIS) e Cromatografia em fase Líquida de Alta Eficiência (CLAE). Termogravimetria/ Termogravimetria Derivada (TG/DTG), Calorimetria Exploratória Diferencial (DSC), Difração de Raios X (DRX), Espectroscopia de absorção na região do Infravermelho com Transformada de Fourier (FTIR) e Microscopia Eletrônica de Varredura (MEV). Para o fármaco besilato de anlodipino (AB) pelo método de degradação forçada, analisado por espectrofotometria no UV/VIS, as condições para a análise espectrofotométrica foram metanol e água a uma proporção de (5:45 v/v) e a segunda diluição com água. A leitura foi efetuada a 364,4nm. A linearidade foi estabelecida na faixa de 40,0-65,0 µg/mL e o coeficiente de correlação foi (r) 0,9992. O método cromatográfico, mostrou o diferente comportamento das substâncias nifedipino e nimodipino diante dos meios básicos, ácido, neutro e oxidativo. As condições para a substância nifedipino foram coluna LiChrospher®100 RP-18 (5µm) Merck® fase móvel constituída por metanol e água (45:55v/v), fluxo 1.0 mL/min, tempo de retenção 5,1min, detecção UV a 234nm e vazão de 1.0 mL/min. Foi obtida uma linearidade no intervalo de 5.0-55.0 µg/mL coeficiente de correlação (r) =0,9964. E para a substância nimodipino foram coluna LiChrospher®100 RP-18 (5µm) Merck® fase móvel constituída por acetonitrila e água (55:45v/v), fluxo 1.0mL/min, tempo de retenção 5,8 min, detecção UV a 235 nm e vazão de 1.0mL/min. Foi obtida uma linearidade no intervalo de 5.0-55.0 µg/mL coeficiente de correlação (r) =0,9964. Os resultados obtidos das curvas TG/DTG e DSC mostraram o perfil da decomposição térmica das substâncias estudadas pela Calorimetria Exploratória Diferencial. A análise dos resultados de DRX e DSC mostraram que não há evidências de polimorfismo nessas substâncias. No entanto nas análises de Espectroscopia de absorção na região do infravermelho com Transformada de Fourier (FTIR) não foram encontradas diferenças significativas na matéria-prima e no padrão de referência. As análises de MEV permitiram observar a cristalinidade das substâncias estudadas


Hypertension is the most frequent non-communicable chronic disease in the population being the main factor of risk for cardiovascular complications, such as stroke and acute myocardial infarction. In this work, active pharmaceutical ingredients used to treat hypertension were studied, more specifically the blockers calcium channel dihydropyridine group: amlodipine besylate, nifedipine and nimodipine. The aim of this study was to determine the intrinsic stability of amlodipine besylate, nifedipine and nimodipine. For this purpose the following stability test techniques were used: UV/VIS spectrophotometry and chromatography Net phase High Performance. Thermogravimetry/Derivative Thermogravimetry (TG/ DTG), Differential Scanning Calorimetry (DSC), X-Ray Diffraction (XRD), Fourier Transformed Infrared absorption (FTIR) and Scanning Electron Microscopy (MEV). For drug amlodipine besylate (AB) by forced degradation method analyzed by spectrophotometry UV/VIS spectrophotometric conditions for the analysis were methanol and water at a ratio (5:45v/v) and the second dilution with water. The reading was made at 364,4nm. The linearity was established in the range of 40.0 to 65.0 mg/mL and the correlation coefficient was (r) 0.9992. The chromatographic method showed different behavior of nifedipine and nimodipine substances on the basic means, acid, neutral and oxidative. The conditions for nifedipine were LiChrospher®100 RP-18 column (5µm) Merck® mobile phase consisting of methanol and water (45:55v/v), flow 1.0 mL/min, retention time 5,1min, UV detection at 234 nm and flow of 1.0 mL/min. Linearity was obtained within the range of 5.0-55.0 mg/mL correlation coefficient (r) = 0.9964. And for nimodipine the parameters were: LiChrospher®100 RP-18 column (5µm) Merck® mobile phase consisted of acetonitrile: water (55:45v/v), flow 1.0 mL/min, retention time 5,8min, UV detection at 235nm and flow of 1.0 mL/min. The linearity was obtained within the range of 5.0- 55.0 mg/mL correlation coefficient (r) = 0.9964. The results of TG/DTG and DSC curves presented the profile of the thermal decomposition of the substances studied by DSC. The results of XRD and DSC presented no evidence of polymorphism in these analyzes, however, according to analyzes of absorption spectroscopy in the infrared (FTIR) there were no significant differences in the raw materials and standard reference. SEM analyzes allowed to observe the crystallinity of the studied substances


Subject(s)
Amlodipine/analysis , Calcium , Nifedipine/analysis , Nimodipine/analysis , Pharmaceutical Preparations/analysis , Spectrophotometry, Ultraviolet/instrumentation , Analytical Methods/analysis , Chromatography , Differential Thermal Analysis , Differential Thermal Analysis/instrumentation , Hypertension/prevention & control , Infarction , Polymorphism, Genetic/physiology , Stroke , Thermogravimetry/methods
16.
Article in Chinese | WPRIM | ID: wpr-246098

ABSTRACT

This study is to develop a sensitive method by using reversed-phase high performance liquid chromatography coupled with UV detector (HPLC-UV) to simultaneously determine four bioactive compounds, iriflophenone 3-C-beta-D-glucoside, iriflophenone 3,5-C-beta-D-diglucoside, mangiferin, and iriflophenone 2-O-alpha-L-rhamnoside in the leaves of Aquilaria sinensis. An Agilent Zorbax SB-C, column (4, 6 mm x 250 mm, 5 microm) was used, and the gradient elution was performed with mobile phase of 0.1% aqueous phosphoric acid and acetonitrile at a flow rate of 1 mL x min(-1). The detection wavelength was 280 nm, and the column temperature was 25 degrees C. The four marker compounds were well separated with good linearity (R2 > 0.9990), precision, stability and repeatabili y. The-recovery rates were in the range of 98.80%-101.39%. For 15 branch of the leaves, the contents of iriflophenone 3-C-beta-D-gluoside, iriflophenone 3,5-C-beta-D-diglucoside, mangiferin, and iriflophenone 2-O-alpha-L-rhamnoside were between 0.41-14.48, 0.72-3.85, 4.30-29.07, 0.24-5.06 mg, respectivley. This method is precise, accurate and reliable, which provides an efficient way for the quality control of the leaves of A. sinensis. This will promote the comprehensive usage of this plant.


Subject(s)
Benzophenones , Chromatography, High Pressure Liquid , Methods , Drugs, Chinese Herbal , Plant Leaves , Chemistry , Spectrophotometry, Ultraviolet , Methods , Thymelaeaceae , Chemistry , Xanthones
17.
IJPR-Iranian Journal of Pharmaceutical Research. 2015; 14 (2): 473-478
in English | IMEMR | ID: emr-167952

ABSTRACT

The method has been developed and validated for the determination of hydroquinone in liposomal formulation. The samples were dissolved in methanol and evaluated in 293 nm. The validation parameters such as linearity, accuracy, precision, specificity, limit of detection [LOD] and limit of quantitation [LOQ] were determined. The calibration curve was linear in 1-50 microg/mL range of hydroquinone analyte with a regression coefficient of 0.9998. This study showed that the liposomal hydroquinone composed of phospholipid [7.8%], cholesterol [1.5%], alpha ketopherol [0.17%] and hydroquinone [0.5%] did not absorb wavelength of 293 nm if it diluted 500 times by methanol. The concentration of hydroquinone reached 10 microg/mL after 500 times of dilution. Furthermore, various validation parameters as per ICH Q2B guideline were tested and found accordingly. The recovery percentages of liposomal hydroquinone were found 102 +/- 0.8, 99 +/- 0.2 and 98 +/- 0.4 for 80%, 100% and 120% respectively. The relative standard deviation values of inter and intra-day precisions were <%2. LOD and LOQ were 0.24 and 0.72 microg/mL respectively


Subject(s)
Liposomes , Spectrophotometry, Ultraviolet , Validation Studies as Topic
18.
Article in Chinese | WPRIM | ID: wpr-815239

ABSTRACT

OBJECTIVE@#To explore the interaction between cefdinir (CE) and bovine serum albumin (BSA) by fluorescence and ultraviolet-visible absorption spectrometry.
@*METHODS@#Under the optimal conditions, the interaction between CE and BSA was investigated by fluorescence and ultraviolet-visible absorption spectrometry.
@*RESULTS@#CE could quench (static quenching) the intrinsic fluorescence of BSA by forming the CE-BSA complex. The main binding forces were considered as hydrogen bonds and Van der Waals forces based on the calculated values of the thermodynamic parameter. The process of binding was spontaneous because Gibbs free energy change was negative. The primary binding site for CE was located at sub-domain II of BSA. The values of Hill's coefficients were less than 1, indicating a negative cooperative effect. Synchronous fluorescence spectra showed that the conjugation reaction between CE and BSA did not affect the conformation of BSA, and the binding site was close to the tyrosine residue.
@*CONCLUSION@#This test provides a theoretical basis for revealing the pharmacokinetic issue and the development for new drugs.


Subject(s)
Binding Sites , Cefdinir , Cephalosporins , Chemistry , Serum Albumin, Bovine , Chemistry , Spectrophotometry, Ultraviolet , Thermodynamics
19.
Article in Chinese | WPRIM | ID: wpr-359562

ABSTRACT

This article explores the possible influencing factor and regular pattern of temperature rise induced by photo-thermal effect of gold nanorods when irradiated with near infrared region (NIR) laser. We used transmission electron microscope and UV-Vis-NIR spectrometer to characterize gold nanorods, then used 808 nm NIR laser with different power to irradiate the gold nanorods in different conditions and measured the temperature of the above solution. The higher the concentration of gold nanorods, the faster the temperature rose and the bigger its amplitude was. When the concentration of gold nanorods was fixed, the relation between power of laser and amplitude of temperature rise was linear. Temperature rise was also related to the shape of container. It could be concluded that amplitude of temperature rise of gold nanorods reaction system was related with concentration of the particles, irradiated power and shape of the container, so that we could control the temperature easily by regulating the irradiated power size of NIR laser in the experiments.


Subject(s)
Gold , Lasers , Light , Microscopy, Electron, Transmission , Nanotubes , Spectrophotometry, Ultraviolet , Spectroscopy, Near-Infrared , Temperature
20.
Rev. latinoam. enferm ; 22(6): 926-933, 16/12/2014. tab
Article in English | LILACS, BDENF | ID: lil-732950

ABSTRACT

OBJECTIVES: to assess how nurses perceive autonomy, control over the environment, the professional relationship between nurses and physicians and the organizational support and correlate them with burnout, satisfaction at work, quality of work and the intention to quit work in primary healthcare. METHOD: cross-sectional and correlation study, using a sample of 198 nurses. The tools used were the Nursing Work Index Revised, Maslach Burnout Inventory and a form to characterize the nurses. To analyze the data, descriptive statistics were applied and Spearman's correlation coefficient was used. RESULTS: the nurses assessed that the environment is partially favorable for: autonomy, professional relationship and organizational support and that the control over this environment is limited. Significant correlations were evidenced between the Nursing Work Index Revised, Maslach Burnout Inventory and the variables: satisfaction at work, quality of care and the intent to quit the job. CONCLUSION: the nurses' perceptions regarding the environment of practice are correlated with burnout, satisfaction at work, quality of care and the intent to quit the job. This study provides support for the restructuring of work processes in the primary health care environment and for communication among the health service management, human resources and occupational health areas. .


OBJETIVOS: avaliar percepções dos enfermeiros sobre autonomia, controle sobre o ambiente, relação profissional entre enfermeiro e médico e suporte organizacional e correlacioná-las com Burnout, satisfação no trabalho, qualidade do cuidado e intenção de deixar o trabalho, na atenção básica. MÉTODO: estudo transversal e correlacional, com amostra de 198 enfermeiros. Foram utilizados o Nursing Work Index Revised, o Inventário de Burnout de Maslach e uma ficha de caracterização do enfermeiro. Para análise dos dados, foi realizada estatística descritiva e utilizado o coeficiente de correlação de Spearman. RESULTADOS: os enfermeiros avaliaram que o ambiente é parcialmente favorável para: autonomia, relação profissional e suporte organizacional e que há pouco controle sobre o mesmo. Evidenciaram-se correlações significativas entre o Nursing Work Index Revised, o Inventário de Burnout de Maslach e as variáveis: satisfação no trabalho, qualidade de cuidado e intenção de deixar o trabalho. CONCLUSÃO: percepções dos enfermeiros acerca do ambiente da prática correlacionam-se com Burnout, satisfação no trabalho, qualidade do cuidado e intenção de deixar o trabalho. Este estudo fornece subsídios para reestruturação de processos de trabalho no ambiente da atenção básica e para comunicação entre as áreas de gestão de serviços de saúde, recursos humanos e saúde do trabalhador. .


OBJETIVOS: evaluar percepciones de los enfermeros sobre autonomía, control sobre el ambiente, relación profesional entre enfermero y médico y soporte organizacional y correlacionarlas con el síndrome de burnout, la satisfacción en el trabajo, la calidad del cuidado y la intención de dejar el trabajo, en la atención básica. MÉTODO: estudio transversal y de correlación, con muestra de 198 enfermeros. Fueron utilizados el Nursing Work Index Revised, el Inventario de Burnout de Maslach y una ficha de caracterización del enfermero. El análisis de los datos fue realizado con estadística descriptiva y se utilizó el coeficiente de correlación de Spearman. RESULTADOS: los enfermeros evaluaron que el ambiente es parcialmente favorable para: autonomía, relación profesional y soporte organizacional y que existe poco control sobre el mismo. Se evidenciaron correlaciones significativas entre el Nursing Work Index Revised, el Inventario de Burnout de Maslach y las variables: satisfacción en el trabajo, calidad del cuidado e intención de dejar el trabajo. CONCLUSIÓN: las percepciones de los enfermeros acerca del ambiente de la práctica se correlacionan con burnout, satisfacción en el trabajo, calidad del cuidado e intención de dejar el trabajo. Este estudio ofrece subsidios para la reestructuración de procesos de trabajo en el ambiente de la atención básica y para comunicación entre las áreas de administración de servicios de salud, recursos humanos y salud del trabajador. .


Subject(s)
Oxytetracycline/analysis , Capsules , Hydrogen-Ion Concentration , Indicators and Reagents , Molybdenum/chemistry , Oxytetracycline/chemistry , Solutions , Spectrophotometry, Ultraviolet
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