Determination of lomefloxacin in tablet preparations by liquid chromatography

A sensitive, precise, and specific high-performance liquid chromatography (HPLC) method was developed for the assay of lomefloxacin (LFLX) in raw material and tablet preparations. The method validation parameters yielded good results and included the range, linearity, precision, accuracy, specificity, and recovery. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay. The HPLC separation was performed on a reversed-phase Phenomenex C18 column (150 x 4.6 mm id, 5 pm particle size) with a mobile phase composed of 1% acetic acid-acetonitrile-methanol (70 + 15 + 15, v/v/v), pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 280 nm. The calibration graph for LFLX was linear from 2.0 to 7.0 mg/mL. The interday and intraday precisions (relative standard deviation) were less than 1.0%. The method was applied for the quality control of commercial LFLX tablets to quantitate the drug.

High-performance liquid chromatographic determination of amfepramone hydrochloride, mazindol, and diazepam in tablets

Simple and rapid procedures were developed for the quantification of amfepramone hydrochloride and diazepam and mazindol and diazepam in tablets using high performance liquid chromatography (HPLC) with UV detection. These techniques provided conditions for the separation of each active ingredient from the complex matrices of the dosage forms by dilution or extraction in methanol. Isocratic reversed phase chromatography was performed using acetonitrile, methanol, and aqueous 0,1% ammonium carbonate (70:10:20, v/v/v) as a mobile phase, Radial-Pak C-18 column (100 x 8 mm id, 4 mu m), a column temperature of 25+/-1 degrees C and detection at 255 nm. The calibration curves were linear over a wide concentration range (100-1000 mu g.mL(-1) to amfepramone hydrochloride and mazindol and 10-100 mu g.mL(-1) to diazepam) with good correlation factors of 0.9978, 0.9956 and 0.9997 for amfepramone hydrochloride, mazindol, and diazepam, respectively.Mean recoveries obtained from the two kinds of samples ranged from 83.2 to 102.5%, with coefficients of variation ranging from 1.0 to 6.1.These results demonstrated the efficiency of the proposed methods, as well as advantages such as simplicity and short duration of analysis.

Spectrophotometric determination of sparfloxacin in pharmaceutical formulations using bromothymol blue

A visible light spectrophotometric method is described for them determination of sparfloxacin in tablets. The procedure is based on the complexation of bromothymol blue 0.5% and sparfloxacin to form a compound of yellow colour with maximum absorption at 385 nm. The Lambert-Beer law was obeyed in the concentration range of 2-12 mg/l. The present study describes a sensitive and accurate method for the determination of the concentration of sparfloxacin in tablets. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay.

Development of a Validated Stability-Indicating LC Assay and Stress Degradation Studies of Linezolid in Tablets

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development and validation of a stability-indicative agar diffusion assay to determine the potency of linezolid in tablets in the presence of photodegradation products

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development and Validation of an UV-Derivative Spectrophotometric Method for Determination of Glimepiride in Tablets

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

A new approach to the granulation of beta-cyclodextrin inclusion complexes

Cyclodextrins (CDs) are annular oligosaccharides containing 6-12 glucose unities joined together by alpha-1,4 bonds. They have a conical-truncated shape with a lipophilic cavity in which different molecules can be included resulting in a stable inclusion complex. The cyclodextrins have been widely applied in pharmaceutical technology with the objective of increasing the solubility, stability and bioavailability of drugs in different pharmaceutical dosage forms, such as tablets. In order to obtain beta-CD tablets, liquid dispersions of drug/beta-CD are usually submitted to different drying processes, like spray-drying, freeze-drying or slow evaporation, being this dry material added to a number of excipients. However, such drying processes can generate particulate materials showing problems of flow and compressibility, needing their conversion into granulates by means of wetting with granulation liquid followed by additional drying. In this work, the main objective was to evaluate the preparation of tablets without the need of this additional drying step. For this purpose an aqueous dispersion containing acetaminophen/beta-CD complex and cornstarch was dried using a spouted bed and the obtained granules were compressed in tablets. Acetaminophen was used as model drug due to its low water solubility and the inexpensive and widely available cornstarch was chosen as excipient. Acetaminophen powder was added into a beta-cyclodextrin solution prepared in distilled water at 70 degrees C. Stirring was kept until this dispersion cooled to room temperature. Then cornstarch was added and the resulting dispersion was dried in spouted bed equipment. This material was compressed into tablets using an Erweka Korsh EKO tablet machine. This innovative approach allowed the tablets preparation process to be carried out with fewer steps and represents a technological reliable strategy to produce beta-cyclodextrin inclusion complexes tablets. (C) 2010 Elsevier By. All rights reserved.

Performance characteristics of bioassay UV-spectrophotometry and high perfomance liquid chromatographic determination of gatifloxacin in tablets

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Aplicação da termogravimetria na determinação do teor de ferro em comprimidos: um estudo comparativo com a espectrofotometria

This study used the Thermogravimetry (TG) and molecular absorption spectroscopy in UV-visible region to determine the iron content in herbal medicinal ferrous sulfate used in the treatment of iron deficiency anemia. The samples were characterized by IR, UV, TG / DTG, DTA, DSC and XRD. The thermoanalytical techniques evaluated the thermal stability and physicochemical events and showed that the excipients interfere in the decomposition of the active ingredients. The results of thermogravimetry showed that the decomposition temperature of the active principle Fe2(SO4)3 (T = 602 °C) is higher as compared to samples of tablets (566 586 °C). In the DTA and DSC curves were observed exothermic and endo events for samples of medicines and active analysis. The infrared spectra identified key functional groups exist in all samples of active ingredients, excipients and compressed studied, such as symmetric and asymmetric stretching of OH, CH, S=O. The analysis by X-ray diffraction showed that all samples had crystallinity and the final residue showed peaks indicating the presence of silicon dioxide, titanium dioxide and talc that are excipients contained in pharmaceutical formulations in addition to iron oxide. The results obtained by TG to determine the iron content of the studied drugs showed a variance when compared with those obtained by theoretical and UV-visible, probably due to formation of a mixture of Fe2O3 and Fe2(SO4)3. In one tablet was obtained FE content of 15.7 % and 20.6 % for TG by UV-visible, the sample EF 2 was obtained as a percentage of 15.4 % and 21.0 % for TG by UV-visible . In the third SF samples were obtained a content of 16.1 % and 25.5 % in TG by UV-visible, and SF 4 in the percentage of TG was 16.7 % and 14.3 % UV-visible

Magnetic images of the disintegration process of tablets in the human stomach by ac biosusceptometry

Oral administration of solid dosage forms is usually preferred in drug therapy. Conventional imaging methods are essential tools to investigate the in vivo performance of these formulations. The non-invasive technique of ac biosusceptometry has been introduced as an alternative in studies focusing on gastrointestinal motility and, more recently, to evaluate the behaviour of magnetic tablets in vivo. The aim of this work was to employ a multisensor ac biosusceptometer system to obtain magnetic images of disintegration of tablets in vitro and in the human stomach. The results showed that the transition between the magnetic marker and the magnetic tracer characterized the onset of disintegration (t(50)) and occurred in a short time interval (1.1 +/- 0.4 min). The multisensor ac biosusceptometer was reliable to monitor and analyse the in vivo performance of magnetic tablets showing accuracy to quantify disintegration through the magnetic images and to characterize the profile of this process.

Gastrointestinal transit and disintegration of enteric coated magnetic tablets assessed by ac biosusceptometry

The oral administration is a common route in the drug therapy and the solid pharmaceutical forms are widely used. Although much about the performance of these formulations can be learned from in vitro studies using conventional methods, evaluation in vivo is essential in product development. The knowledge of the gastrointestinal transit and how the physiological variables can interfere with the disintegration and drug absorption is a prerequisite for development of dosage forms. The aim of this work was to employing the ac biosusceptometry (ACB) to monitoring magnetic tablets in the human gastrointestinal tract and to obtain the magnetic images of the disintegration process in the colonic region. The ac biosusceptometry showed accuracy in the quantification of the gastric residence time, the intestinal transit time and the disintegration time (DT) of the magnetic formulations in the human gastrointestinal tract. Moreover, ac biosusceptometry is a non-invasive technique, radiation-free and harmless to the volunteers, as well as an important research tool in the pharmaceutical, pharmacological and physiological investigations. (c) 2005 Elsevier B.V. All rights reserved.

Disintegration of magnetic tablets in human stomach evaluated by alternate current Biosusceptometry

Oral administration is the most convenient route for drug therapy. The knowledge of the gastrointestinal transit and specific site for drug delivery is a prerequisite for development of dosage forms. The aim of this work was to demonstrate that is possible to monitor the disintegration process of film-coated magnetic tablets by multi-sensor alternate current Biosusceptometry (ACB) in vivo and in vitro. This method is based on the recording of signals produced by the magnetic tablet using a seven sensors array and signal-processing techniques. The disintegration was confirmed by signals analysis in healthy human volunteers' measurements and in vitro experiments. Results showed that ACB is efficient to characterize the disintegration of dosage forms in the stomach, being a research tool for the development of new pharmaceutical dosage forms. (C) 2003 Elsevier B.V. All rights reserved.

Influence of compression forces on tablets disintegration by AC Biosusceptometry

Analysis of physical phenomena that occurs during tablet disintegration has been studied by several experimental approaches; however none of them satisfactorily describe this process. The aim of this study was to investigate the influence of compression force on the tablets by associating the AC Biosusceptometry with consolidated methods in order to validate the biomagnetic technique as a tool for quality control in pharmaceutical processes.Tablets obtained at five compression levels were submitted to mechanical properties tests. For uncoated tablets, water uptake and disintegration force measurements were performed in order to compare with magnetic data. For coated tablets, magnetic measurements were carried out to establish a relationship between physical parameters of the disintegration process. According to the results, differences between the compression levels were found for water uptake, force development and magnetic area variation measurements. ACB method was able to estimate the disintegration properties as well as the kinetics of disintegration process for uncoated and coated tablets. This study provided a new approach for in vitro investigation and validated this biomagnetic technique as a tool for quality control for pharmaceutical industry. Moreover, using ACB will also be possible to test these parameters in humans allowing to establish an in vitro/in vivo correlation (IVIVC). (C) 2007 Elsevier B.V. All rights reserved.

Spectrofluorimetric Determination of Coumarin in Commercial Tablets

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A new potentiometric ibuprofenate ion sensor immobilized in a graphite matrix for determination of ibuprofen in tablets

The characteristics, performance, and application of an electrode, namely, Pt vertical bar Hg vertical bar Hg-2(IBP)(2)vertical bar Graphite, where IBP stands for ibuprofenate ion, are described. This electrode responds to IBP with sensitivity of (58.6 +/- 0.9) mV decade 1 over the range 5.0 x 10(-5)-1.0 x 10(-1) mol L-1 at pH 6.0-9.0 and a detection limit of 3.8 x 10(-5) mol L-1. The electrode is easily constructed at a relatively low cost with fast response time (within 1530 s) and can be used for a period of 5 months without any considerable divergence in potentials. The proposed sensor displayed good selectivity for ibuprofen in the presence of several substances, especially concerning carboxylate and inorganic anions. It was used for the direct assay of ibuprofen in commercial tablets by means of the standard additions method. The analytical results obtained by using this electrode are in good agreement with those given by the United States Pharmacopeia procedure. (c) 2006 Elsevier B.V. All rights reserved.