Determination of atenolol in pharmaceutical formulations by diffuse reflectance spectroscopy

A simple analytical method for quantification of atenolol in pharmaceutical formulations by diffuse reflectance spectroscopy is described. The method is based on the reaction, on the filter paper surface, between the drug and p-chloranil producing a colored compound. The best reaction conditions were obtained with 20 μL of atenolol solution and 20 μL of p-chloranil. All reflectance measurements were carried out at 550 nm and the linear range was from 1.13×10-2 to 7.88×10-2 mol L-1 (r = 0.9992). The limit of detection was 2.80 × 10-3 mol L-1. The proposed method was successfully applied to analysis of different commercial brands of pharmaceutical formulations and the results obtained by the proposed method were in good agreement with those obtained using the British Pharmacopoeia method.

A simple spectrophotometry method for the determination of tetracycline and doxycycline in pharmaceutical formulations using chloramine-T

A simple, rapid, accurate and inexpensive spectrophotometric method for the determination of tetracycline and doxycycline has been developed. The method is based on the reaction between these drugs and chloramine-T in alkaline medium producing red color products with absorbance maximum at the λ=535 and 525 nm for the tetracycline and doxycycline, respectively. The best conditions for the reactions have been found using multivariate method. Beer's law is obeyed in a concentration ranges 1. 03 x 10 -5 to 3. 61 x 10 4mol L -1 and 1. 75 x 10 -5 to 3. 48 x 10 4mol L -1 for the tetracycline and doxycycline, respectively. The quantification limits were 5. 63 x 10 -6 mol L -1 and 7. 12 x 10 -7 mol L -1 for the tetracycline and doxycycline, respectively. The proposed method was successfully applied to the determination of these drugs in pharmaceutical formulations and the results obtained were in good agreement with those obtained by the comparative method at the 95% confidence level.

A simple and environmentally friendly reflectometric method for the rapid quantitative analysis of captopril in pharmaceutical formulations

This paper describes a simple, environmentally friendly and rapid quantitative spot test procedure for the determination of captopril (CPT) in bulk drug and in pharmaceutical formulations by using diffuse reflectance spectroscopy. The proposed method is based on the reflectance measurements of the orange compound (λ max 490 nm) produced by the spot test reaction between CPT and p-chloranil (CL). Under optimal conditions, calibration curves were obtained for CPT by plotting the optical density of the reflectance signal (A R) vs. the log of the mol L -1 concentration, from 6.91×10 -3 to 1.17×10 -1, with a good coefficient of determination (R 2 = 0.9992). The common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method was applied to determine CPT in commercial pharmaceutical formulations. The results obtained by the proposed method are compared favorably with those obtained by an official procedure at 95% confidence level. The method validation results showed that the sensitivity and selectivity of the methods were adequated for drug monitoring in industrial quality control laboratories. © 2011 Moment Publication.

Influence of natural polymer derived from starch as a sensory modifier in sunscreen formulations

Background: Nowadays, there has been increased incidence of skin cancer, which is mainly related to increased sun exposure. Although sunscreen products may prevent the appearing of this disease, consumers may not use them due to some factors, including the sensory properties. The Aluminum Starch Octenylsuccinate (Dry-Flo® Pure, Akzo Nobel), an aluminum salt produced by the reaction of anhydride octenylsuccinic with starch, is able to improve the spreadability on the skin and reduce the oiliness of the formulation. Objective: To verify volunteers' acceptance for sunscreen formulation with natural polymer, compared with a control formulation (without polymer). Methods: To carry out the sensory analysis a formulation with or without 2. 0% Aluminum Starch Octenylsuccinate was prepared. Formulations had FPS 15, with critical wavelength of 353 nm, determined by testing in silico using the BASF® Sunscreen Simulator. Sensory analysis was performed on 60 students of both sexes, aged between 18 and 25 years, regular users of sunscreen products. Results: The results suggested that the polymer was able to promote a very soft and velvety feel on the skin when used in a sunscreen formulation, and it was able to mitigate and noticeably reduce the oiliness of the skin. Of the 60 volunteers who participated in the study, 45 volunteers (75%) considered that the polymer formulation provides little brightness or did not notice the difference in brightness of the skin after application. Conclusions: It was able to improve the sensory of the product, contributing to greater volunteers' acceptance.

Chemical composition and antioxidant activity of dried powder formulations of Agaricus blazei and Lentinus edodes

Several mushroom species have been pointed out as sources of antioxidant compounds, in addition to their important nutritional value. Agaricus blazei and Lentinus edodes are among the most studied species all over the world, but those studies focused on their fruiting bodies instead of other presentations, such as powdered preparations, used as supplements. In the present work the chemical composition (nutrients and bioactive compounds) and antioxidant activity (free radical scavenging activity, reducing power and lipid peroxidation inhibition) of dried powder formulations of the mentioned mushroom species (APF and LPF, respectively) were evaluated. Powder formulations of both species revealed the presence of essential nutrients, such as proteins, carbohydrates and unsaturated fatty acids. Furthermore, they present a low fat content (<2 g/100 g) and can be used in low-calorie diets, just like the mushrooms fruiting bodies. APF showed higher antioxidant activity and higher content of tocopherols and phenolic compounds (124 and 770 μg/100 g, respectively) than LPF (32 and 690 μg/100 g). Both formulations could be used as antioxidant sources to prevent diseases related to oxidative stress. © 2012 Elsevier Ltd. All rights reserved.

Square-wave voltammetric determination of rutin in pharmaceutical formulations using a carbon composite electrode modified with copper (II) phosphate immobilized in polyester resin

Descreve-se um eletrodo de carbono modificado com fosfato de cobre (II) imobilizado em uma resina de poliéster (Cu₃(PO₄)₂-Poly) para a determinação de rutina em amostras farmacêuticas por voltametria de onda quadrada. O eletrodo modificado permite a determinação de rutina em potencial (0.20 V vs Ag / AgCl (3,0 mol L^-1 KCl)) menor que o observado em um eletrodo não modificado. Verificou-se que a corrente de pico foi linear com a concentração de rutina na faixa de 9,9 × 10^-8 a 2,5 × 10^-6 mol L^-1, com um limite de detecção de 1,2 × 10^-8 mol L^-1. A resposta do eletrodo foi estável, sem variação significativa dentro de várias horas de operação contínua. A morfologia da superfície do eletrodo modificado foi caracterizada por microscopia eletrônica de varredura (MEV) e pelo sistema de energia dispersiva de raios-X (EDX). Os resultados obtidos foram precisos e exatos. Ademais, estes resultados estão de acordo com aqueles obtidos pelo método cromatográfico a um nível de confiança de 95%.

Minimum Evaporation Model of Dermatological Delivery Systems. Lamellar Liquid Crystal Formulations Containing Brazilian Nut (Bertholletia excelsa HBK) Vegetable Oil and Guarana Glycolic Extract

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Evaluation of Three Formulations of Culture Media for Isolation of Brucella spp. regarding Their Ability to Inhibit the Growth of Contaminating Organisms

Three culture media (Brucella agar, Farrell medium, and CITA) were compared for their effectiveness in inhibiting contamination and for isolating Brucella spp. One hundred lymph nodes from pigs (n = 50) and wild boars (n = 50) with lymphadenitis were collected in slaughterhouses in the State of Sao Paulo and were assessed on these three selective media for Brucella spp. All of the samples were negative for Brucella spp. on the three culture media. On the agar medium, fungal (70 plates) and Gram-positive bacterial (59 plates) contaminants were observed; in the CITA medium, the absence of fungal and Gram-positive bacteria on 15 plates was observed; no bacterial or fungal growth was observed on the Farrell media. The results demonstrated that the CITA and Farrell media inhibited the growth of contaminants better than the Brucella agar.

Evaluation of the Interaction Between Sodium Hypochlorite and Several Formulations Containing Chlorhexidine and its Effect on the Radicular Dentin-SEM and Push-Out Bond Strength Analysis

The aim of the current study was to evaluate the presence of debris and smear layer after endodontic irrigation with different formulations of 2% chlorhexidine gluconate (CHX) and its effects on the push-out bond strength of an epoxy-based sealer on the radicular dentin. One hundred extracted human canines were prepared to F5 instrument and irrigated with 2.5% sodium hypochlorite and 17% ethylenediaminetetraacetic acid. Fifty teeth were divided into five groups (n=10), according to the final irrigation protocol with different 2% CHX formulations: G1 (control, no final rinse irrigation), G2 (CHX solution), G3 (CHX gel), G4 (Concepsis), and G5 (CHX Plus). In sequence, the specimens were submitted to scanning electron microscopy (SEM) analysis, in the cervical-medium and medium-apical segments, to evaluate the presence of debris and smear layer. The other 50 teeth were treated equally to a SEM study, but with the root canals filled with an epoxy-based endodontic sealer and submitted to a push-out bond strength test, in the cervical, middle, and apical thirds. G2, G3, G4, and G5 provided higher precipitation of the debris and smear layer than G1 (P<0.05), but these groups were similar to each other (P>0.05), in both segments. The values obtained in the push out test did not differ between groups, independent of the radicular third (P>0.05). The CHXs formulations caused precipitation of the debris and smear layer on the radicular dentin, but these residues did not interfere in the push-out bond strength of the epoxy-based sealer. Microsc. Res. Tech. 77:17-22, 2014. (c) 2013 Wiley Periodicals, Inc.

Effects of different formulations of neem oil-based products on control Zabrotes subfasciatus (Boheman, 1833) (Coleoptera: Bruchidae) on beans

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Atenolol characterization in solid formulations available in Brazilian market

Atenolol is the most used drug in Brazil to hypertension treatment. Two crystal structures are known for this molecule: a racemic form (R,S)-atenolol and a pure form S-atenolol. The racemic form is found in commercial tablets. X-ray powder diffraction (XRD) is an adequate tool to study crystalline structures including drugs. Using the Rietveld Method with XRD data it is possible to quantify the crystalline structures existing in the raw material. Other methods like Le Bail and Pawley can be used to the profile fit and phases identification. For this work we analyzed three tablets of atenolol, two generics and the reference (materials were purchased from a drugstore at the city of Araraquara). These tablets were analyzed by Rietveld, Le Bail and Pawley methods. All tablets exhibited the racemic mixture API (R,S)-atenolol. Some crystalline excipients could be characterized: magnesium carbonate hydrate, lactose monohydrate and talc. The conclusion is that the three methods can be efficiently used to characterize the three atenolol tablets.

A simple and portable instrument for determination of captopril in pharmaceutical formulations

Objective: This article describes the application and the performance of a cheap, simple and portable device that can be used for colorimetric quantitative determination of captopril (CPT) in pharmaceutical preparations. Methods: The sensor is a light detector resistor (LDR) placed into a black PTFE cell and coupled to a low cost multimeter (Ohmmeter). The instrument has been tested and is easy and fast to use. The quantitative study is based mainly on reduction of ammonium molybdate by captopril, in the presence of sulphuric acid, producing a green-yellow compound (max 407 nm). The calibration curves were obtained by plotting the electric resistance of the LDR against the CPT concentration on the range of 4.60 x 10-4 to 1.84 x 10-3 mol l-1 with a good coefficient of determination (R2 = 0.9962). Results: Statistical analysis of the obtained results showed no significant difference between the proposed methodology and the official reported method as evident from the t-test and variance ratio at 95% confidence level. Conclusion: The results of this study demonstrate that the instrument can be used for simple, accurate, precise, fast, in situ and low-cost colorimetric analysis of captopril in pharmaceuticals products.

Effect of calcium chloride on the pH values of several formulations of calcium hydroxide mixed with chlorhexidine digluconate

This study evaluated the effect of the addition of 5% calcium chlorite (CaCl2) on pH values in calcium hydroxide pastes (CH), with or without 2% chlorhexidine digluconate (CHX) used as vehicle, in several periods analysis. Polyethylene tubes were filled with CH mixed with water (G1), 2% CHX solution (G2) or gel (G3), or CHX solution or gel with 5% CaCl2 (G4 and G5, respectively). All tubes were individually immersed in distilled water. After 12, 24 hours, 7, 14 and 28 days, pH value was evaluated directly in water which the tubes were stored. Data were submitted to ANOVA and Tukey tests (α=0.05). In 24 hs and 14 days, pH values were similar to all groups. In 12 hs, the G1 presented lower pH value than other groups except to G4 (p < 0.05), and G4 presented lower pH value than G5 (p < 0.05). In 7 days, G1 presented lower pH value than G4 and G5 (p < 0.05). In 28 days, G1 and G5 presented lower pH values than G2 and G4 (p < 0.05) and among other groups there are no statistical differences (p > 0.05). The pH values increased in long-term analysis to all CH pastes. The association of 5% calcium chloride with 2% CHX solution as vehicle of CH paste provided a pH value increase in relation to CH mixed with distilled water. The CHX gel interfered negatively on pH value in comparison to CHX solution when mixed with CaCl2.

Effect of two formulations of 10% sodium ascorbate on fracture resistance of endodontically treated tooth submitted to dental bleaching with hydrogen peroxide associated titanium dioxide nanoparticles

Purpose: This study evaluated the effect of 10% sodium ascorbate (10SA), in gel (10SAg) or aqueous solution (10SAs) formulations, on fracture resistance of endodontically treated tooth submitted to dental bleaching procedures with 15% hydrogen peroxide associated with titanium dioxide (15HP-TiO2) nanoparticles and photoactivated by LED-laser. Material and methods: Forty maxillary premolars were endodontically-treated and embedded in acrylic resin up to the cement-enamel junction. The specimens were divided into four groups (n=10): G1 (negative control): no bleaching, coronal access restored with composite resin; G2 (positive control): three dental bleaching sessions using 15HP-TiO2 and LED-laser photoactivation and restored with composite resin (positive control); G3 (10SAg): similar procedures to G2, but applied 10SA, in gel formulation, for 24 hours before restoration; G4 (10SAs): similar procedures to G3, but applied 10SA, in aqueous solution formulation. The 15HP-TiO2 was applied on buccal and lingual surfaces of the crown tooth and inside the pulp chamber and photoactivated by LED-laser. Between each bleaching session, the teeth were maintained in artificial saliva, at 37oC, for 7 days. In sequence, the teeth were submitted to fracture resistance testing using an eletromechanical machine test. The data was analyzed using Kruskal Wallis test (p = 0.05) Results: There are no differences significant among the groups in relation to fracture resistance of endodontically treated teeth (p>0.05). Conclusions: The use of 10% sodium ascorbate, in gel or aqueous solution formulations, did not interfered on the fracture resistance teeth after dental bleaching using 15HP-TiO2 and LED-laser photoactivation.

Hydrogen ion and calcium releasing of MTA Fillapex® and MTA-based formulations

MTA is composed of various metal oxides, calcium oxide and bismuth. It has good biological properties and is indicated in cases of endodontic complications. Several commercial formulations are available and further studies are necessary to evaluate these materials. Objective: To evaluate pH and calcium releasing of MTA Fillapex® compared with gray and white MTA. Material and methods: Gray and white MTA (Angelus) and MTA Fillapex® (Angelus) were manipulated and placed into polyethylene tubes and immersed in distilled water. The pH of these solutions was measured at 24 hours, 7 days and 14 days. Simultaneously, at these same aforementioned periods, these materials' calcium releasing was quantified, through atomic absorption spectrophotometry. The results were submitted to ANOVA, with level of significance at 5%. Results: Concerning to pH, the materials present similar behaviors among each other at 24 hours (p > 0.05). At 7 and 14 days, MTA Fillapex® provided significantly lower pH values than the other materials (p < 0.05). Regarding to calcium releasing, at 24 hours and 7 days, MTA Fillapex® provided lower releasing than the other materials (p < 0.05). After 14 days, differences were found between MTA Fillapex® and gray MTA (p < 0.05). Conclusion: All materials showed alkaline pH and calcium releasing, with significantly lower values for MTA Fillapex® sealer.