Development Of Uv-Spectrophotometric Method And Its Validation For Estimating Contents Of Prulifloxacin In Simulated Intestinal Fluid

This study was performed with an objective of developing and validating an UV-spectroscopic method for estimating contents of prulifloxacin in simulated intestinal fluid (SIF) i.e. phosphate- buffer media with a pH of 6.8 as per ICH guidelines. The λmax for prulifloxacin in phosphate- buffer media pH 6.8 was found to be 272 nanometer. The calibration curve of drug followed linearity in-between 1-9 μg/ml concentration range and correlation co-efficient value was found equal to 0.9995. We tested this proposed method onto the bulk and marketed pharmaceutical formulation (tablets) also in order to find out contents of drug. Using developed method for estimation of prulifloxacin in SIF, drug was found to be in-between 101.91 and 104.02 % in marketed tablets which shows a good agreement with that of the claimed level. Accuracy of developed method was established through recovery experimentation, performed for three spiked percent concentrations- 75%, 100%, and 125%. The % recovery was found to be in between 97.27 and 101.82%. Low values of % RSD supported accuracy as well as the reproducibility of developed method. Precision of developed method was established by good in-limit intraday and interday experimental variations and through repeatability tests. Values of % RSD less than 2 confirmed about precision of developed method. The ruggedness of the developed method was validated by performing drug estimation by two different performers. This proposed spectroscopic method has proved to be a rapid and successful method for routine analysis of prulifloxacin in simulated intestinal fluid.

The Newly Developed Highly Sensitive Method For The Determination Of Capecitabine By Using Uv-Spectroscopy

Capecitabine is a fluoropyrimidine carbamate, designed as 'pro-drug' to the cytotoxic agent 5-fluorouracil (5-FU) meant to be administered orally. Capecitabine is used as first line monotherapy for metastatic colorectal cancer. In the present study simple, rapid, accurate UV spectrophotometric methods were developed and validated for the estimation of capecitabine in bulk and its formulations as per ICH guidelines. Three solvent systems viz., 0.1N NaOH, 0.1N HCl and Methanol: Water (1:3) were tried. The results suggest that the developed methods shows linearity over the concentration range of 2-24μg/ml with a correlation coefficient of 0.9999. All the developed methods were statistically validated for accuracy, precision, linearity, robustness, and ruggedness as per ICH guidelines. The % RSD values for validated methods were found to be less than 1.5 and methods will find application in routine analysis of drug formulations containing capecitabine.

Development And Validation Of Uv-Visible Spectrophotometric Method For Determination Of Duloxetine

Objective: The aim of the present work was to develop and validate a simple UV spectroscopic method for the determination of duloxetine, which is a thiophene derivative and a selective neurotransmitter reuptake inhibitor for serotonin, norepinephrine, and to lesser degree dopamine. Methods: The UV Spectrophotometric analysis was performed using Shimadzu UV-1800 and Shimadzu UV-1700 spectrophotometer by using solvent system acetonitrile and water in the ratio of 8:2. Detection was performed at a wavelength of 290 nm. Method validation was carried out according to ICH Q2R1 guidelines by taking the parameters linearity, accuracy, precision, ruggedness, and robustness, LOD and LOQ. Results: The UV Spectrophotometric method was found linear in the range of 10-50 μg/ml. The method was rugged and robust with % relative standard deviation less than 2. The extraction recoveries were found to be higher than 99% in all experimental conditions. Conclusion: Based upon the performance characteristics, the proposed method was found accurate, precise and rapid and suitable for the determination of Duloxetine for routine analysis.

Development of alternative methods for the determination of raloxifene hydrochloride in tablet dosage form / O desenvolvimento de métodos alternativos para a determinação do cloridrato de raloxifeno na forma de dosagem em comprimidos

Three methods are proposed for the quantitative determination of raloxifene hydrochloride in pharmaceutical dosage form: ultraviolet method (UV) high performance liquid chromatography (HPLC) and micellar capillary electrophoresis (MEKC). These methods were developed and validated and showed good linearity, precision and accuracy. Also they demonstrated to be specific and robust. The HPLC and MEKC methods were tested in regards to be stability indicating methods and they showed to have this attribute. The UV method used methanol as solvent and optimal wavelength at 284 nm, obeying Lambert-Beer law in these conditions. The chromatographic conditions for the HPLC method included: NST column C18 (250 x 4.6 mm x 5 µm), mobile phase water:acetonitrile:triethylamine (67:33:0,3 v/v), pH 3.5, flow rate 1.0 mL min^-1, injection volume 20.0 µl, UV detection 287 nm and analysis temperature 30 °C. The MEKC method was performed on a fused-silica capillary (40 cm effective length x 50 µm i.d.) using as background electrolyte 35.0 mmol L^-1 borate buffer and 50.0 mmol L^-1 anionic detergent sodium dodecyl sulfate (SDS) at pH 8.8. The capillary temperature was 32°C, applied voltage 25 kV, UV detection at 280 nm and injection was perfomed at 45 mBar for 4 s, hydrodimanic mode. In this MEKC method, potassium diclofenac (200.0 µg mL^-1) was used as internal standard. All these methods were statistically analyzed and demonstrated to be equivalent for quantitative analysis of RLX in tablets and were successfully applied for the determination of the drug...

Três métodos são propostos para a quantificação de cloridrato de raloxifeno em sua forma farmacêutica de comprimidos: espectrofotometria no ultravioleta (UV), cromatografia líquida de alta eficiência (HPLC) e eletroforese capilar micelar (MEKC). Estes métodos desenvolvidos e validados demonstraram linearidade, precisão e exatidão. Também foram específicos e robustos. Os métodos HPLC e MEKC foram desenvolvidos para indicar a estabilidade do fármaco e demonstraram ter este atributo. O método UV usou metanol como solvente e comprimento de onda de 284nm, obedecendo a Lei de Lambert-Beer nestas condições. Os parâmetros cromatográficos para o método HPLC foram: coluna NST C18 (250 x 4,6 mm x 5 µm), fase móvel composta de água:acetonitrila:trietilamina (67:33:0,3 v/v), pH 3,5, vazão da fase móvel de 1,0 mL min^-1, volume de injeção de 20 µl, detecção no comprimento de onda de 287 nm e temperatura de análise de 30°C. O método MEKC foi realizado utilizando capilar de sílica fundida (40 cm de comprimento efetivo x 50 µm de diâmetro interno) usando como fase móvel solução tampão borato 35.0 mmol L^-1 e solução de dodecil sulfato de sódio (SDS) 50.0 mmol L^-1 pH 8,8. A temperatura de análise foi de 32 °C, com voltagem aplicada de 25 kV, detecção no comprimento de onda de 280 nm e injeção da amostra realizada a 45 mBar por 4 s em modo hidrodinâmico. Para este método MEKC, foi utilizado diclofenaco de potássio (200.0 µg mL^-1) como padrão interno. Todos os métodos foram analisados estatisticamente e demostraram ser equivalentes para a análise quantitativa de raloxifeno em comprimidos e foram aplicados com sucesso na determinação do fármaco...

Validated UV-Visible Spectrophotometric method for simultaneous estimation of Cefixime and Moxifloxacin in Pharmaceutical Dosage Form.

A simple, accurate, sensitive, economical and reliable first order derivative spectrophotometric method was developed and validated for the estimation of cefixime and moxifloxacin in pharmaceutical dosage form. The optimum conditions for the analysis of the drugs were established. First order derivative method was developed for quantification of cefixime and moxifloxacin. Spectrum was obtained by dissolving cefixime and moxifloxacin in methanol and water (60:40 v/v); wavelength selected was 260 nm for cefixime and 316 nm for moxifloxacin. The Beer’s law was obeyed in the concentration range of 2-12 μg/ml. Results of tablet analysis showed percent relative standard deviation (% RSD) in the range of 0.1576 to 0.2183 for cefixime and moxifloxacin which indicate repeatability of the method respectively. Recoveries do not differ significantly from 100% which show there was no interference from the common excipient used in tablet formulation indicating accuracy and reliability of the method. The method was validated as per ICH guideline and found to be accurate, precise and rugged. It was also validated in terms of linearity, accuracy, precision, and specificity, limit of detection and limit of quantitation.

Development and Validation of UV Spectrophotometric Method for the Estimation of Haloperidol.

Aims: The aim of the present work was to develop and validate a sensitive, simple, accurate, precise & cost effective UV spectrophotometric method for the estimation of haloperidol in prepared pharmaceutical formulations of solid lipid nanoparticles. Methodology: The different analytical performance parameters such as linearity, range, precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ) were determined according to International Conference on Harmonization (ICH) Q2 (R1) guidelines. The study was performed in phosphate buffer of pH 7.4. Results: The peak (λmax) of haloperidol appeared at a wavelength of 247.5 nm in phosphate buffer (pH 7.4). Beer-Lambert’s law was obeyed in the concentration range of 2–20 μg/ml with correlation coefficient (R2) 0.9994. Conclusion: The results of the study demonstrated that the developed procedure was accurate, precise and reproducible, while being simple, cheap and less time consuming. Therefore, this method can be suitably applied for the estimation of haloperidol in prepared solid lipid nanoparticles.

Oxcarbazepine: validation and application of an analytical method

Oxcarbazepine (OXC) is an important anticonvulsant and mood stabilizing drug. A pharmacopoeial monograph for OXC is not yet available and therefore the development and validation of a new analytical method for quantification of this drug is essential. In the present study, a UV spectrophotometric method for the determination of OXC was developed. The various parameters, such as linearity, precision, accuracy and specificity, were studied according to International Conference on Harmonization Guidelines. Batches of 150 mg OXC capsules were prepared and analyzed using the validated UV method. The formulations were also evaluated for parameters including drug-excipient compatibility, flowability, uniformity of weight, disintegration time, assay, uniformity of content and the amount of drug dissolved during the first hour.

Oxcarbazepina (OXC) é um fármaco anticonvulsivante e estabilizante do humor. O desenvolvimento e validação de método analítico para quantificação da OXC são de fundamental importância devido à ausência de monografias farmacopéicas oficiais para esse fármaco. Nesse trabalho, um método espectrofotométrico UV para determinação da OXC foi desenvolvido. O método proposto foi validado seguindo os parâmetros de linearidade, precisão, exatidão e especificidade de acordo com as normas da Conferência Internacional de Harmonização. Cápsulas de OXC 150 mg foram preparadas e analisadas utilizando-se o método analítico validado. As formulações foram avaliadas com relação à compatibilidade fármaco-excipientes, fluidez, determinação de peso, tempo de desintegração, doseamento, uniformidade de conteúdo e quantidade do fármaco dissolvido após 60 minutos.