Analytical method development and validation for simultaneous estimation of Teneligliptin hydrobromide hydrate and Metformin hydrochloride from it’s pharmaceutical dosage form by three different UV spectrophotometric methods.

Three new UV spectrophotometric methods namely simultaneous equation, absorbance ratio and first derivative (zero crossing) spectroscopic methods were developed and validated for simultaneous estimation of teneligliptin hydrobromide hydrate and metformin hydrochloride in tablet formulation which were simple, sensitive, precise and accurate. In simultaneous equation method, absorbance was measured at 237 and 246 nm for both the drugs. Teneligliptin hydrobromide hydrate and metformin hydrochloride was estimated using 237 and 247.5 nm in absorbance ratio method. First derivative (zero crossing) method was based on the transformation of UV spectra in to first derivative spectra followed by measurement of first derivative signal at 237 and 246 nm for teneligliptin hydrobromide hydrate and metformin hydrochloride, respectively using 2 nm as wavelength interval (Δλ) and 1 as scaling factor. Developed methods were validated according to ICH guidelines including parameters viz., specificity, linearity and range, precision, accuracy, limit of detection and quantification. All the three methods showed linear response in the concentration range of 1-20 µg/ml for both the drugs. Results of method validation parameters follows ICH guideline acceptable limits. Based on the assay results obtained, methods were compared using one-way ANOVA followed by Bonferroni multiple comparison tests (95% confidence level) using computer based fitting program (Prism, Graphpad version 5, Graphpad Software Inc). Outcome of the statistical analysis proved that there was no considerable dissimilarity between all the developed methods. Methods were found to be simple, fast, highly sensitive, cost effective and hence can be useful for simultaneous estimation of teneligliptin hydrobromide hydrate and metformin hydrochloride in commercial tablet formulation for routine quality control analysis.

Simultaneous estimation of Aliskiren hemifumarate and Hydrochlorothiazide in combined Tablet Formulation by Simultaneous equation, Absorbance ratio and First derivative Spectroscopic Methods.

Three simple, sensitive, precise and accurate UV-spectroscopic methods namely simultaneous equation, absorbance ratio and first derivative (zero crossing) spectroscopic methods were developed and validated for simultaneous determination of aliskiren hemifumarate and hydrochlorothiazide in tablet dosage form. Simultaneous equation method was based on the measurement of absorbance at 271 and 280 nm for both the drugs. In absorbance ratio method 255 and 271 nm was used for the quantification of aliskiren hemifumarate and hydrochlorothiazide. First derivative method was involved in the conversion of UV-spectra in to first derivative spectra and measurement of first derivative signal at 241 and 280.2 nm for aliskiren hemifumarate and hydrochlorothiazide, respectively using 2 nm as wavelength interval (Δλ) and 1 as scaling factor. Methods were validated as per ICH guidelines including parameters viz., specificity, linearity and range, precision, accuracy, limit of detection and quantification. All the methods were found to be linear in the concentration range of 6-300 μg/ml for aliskiren hemifumarate and 0.5-25 μg/ml for hydrochlorothiazide. Results of validation studies follows ICH guideline acceptable limits. Methods were compared based on the assay results obtained using one-way ANOVA followed by Bonferroni multiple comparison tests (95% confidence level) as appropriate using computer based fitting program (Prism, Graphpad version 5, Graphpad Software Inc). Results of statistical analysis revealed that there was no significant difference between simultaneous equation, absorbance ratio and first derivative method. Developed methods were simple, rapid, highly sensitive and cost effective as compared to existing methods and can be useful for simultaneous estimation of aliskiren hemifumarate and hydrochlorothiazide in commercial tablet formulation for routine quality control.

Antilithiatic activity of poly-herbal formulation tablets by in-vitro method.

Hydroalcoholic extracts of Kalanchoe pinnata and Rotula aquatica and its combination were formulated herbal tablets, evaluated for antilithiatic in vitro method. The homogenous precipitation method was used. The study was carried out in glass tubes. The buffer system used was TRIS buffer pH 7.4. The experiment consists of the following tubes for control and test, 25 ml each of 25 mM CaCl2. 2H2O, 25 mM Na2HPO4. 2H2O or 25mM Na2C2O4. To the tubes of each set, tablet formulation or an equal amount of vehicle was added. The tubes were incubated at 37°C for 4 h. The precipitate of calcium phosphate was generated by mixing 1 ml of solution from the tubes having calcium chloride dihydrate and disodium hydrogen phosphate monohydrate and Calcium oxalate precipitate was generated by mixing 1 ml of solutions from the tubes having calcium chloride dihydrate and sodium oxalate solutions. Calcium was estimated using titrimetry and phosphorus was estimated using colorimetric analysis. Appropriate standard curves were done with each set of experiments. The amounts of precipitate of calcium and phosphate were determined in each of the respectively. The percent inhibition of the test was calculated in comparison with the control samples. Herbal tablet formulation showed antilithiatic activity to the marketed formulation in terms of inhibiting the formation of phosphate precipitate but showed a significantly better potential in preventing the formation of the calcium precipitate. The herbal tablet formulation of Kalanchoe pinnata and Rotula aquatica have inhibitory effect on calcium oxalate crystallization thus may be beneficial in the treatment of renal lithiasis.

Comparação da bioequivalência entre duas formulações de dicloridrato de betaistina 24 mg comprimidos em voluntários sadios após a administração de dose única / Comparison of the bioequivalence between two formulations of betahistine hydrochloride 24 mg tablets in healthy volunteers after a single dose dministration

A biodisponibilidade de uma dose única de dicloridrato de betaistina em comprimidos de 24 mg produzidos por Aché Laboratórios Farmacêuticos S.A. foi comparada com o medicamento referência (à época do estudo) dicloridrato de betaistina 24 mg (Labirin®, Apsen Farmacêutica S.A.). Um estudo de dose única, randomizado, aberto, cruzado em dois períodos foi realizado em 34 voluntários brasileiros, sadios, de ambos os gêneros. Dezenove coletas de sangue foram realizadas durante 24 horas. As amostras foram mantidas congeladas até o momento de análise. As concentrações plasmáticas de ácido 2-piridilacético, um metabólito da betaistina, foram determinadas utilizando um método de CLAE-EM/EM validado. Os intervalos com 90% de confiança para concentração plasmática máxima (Cmáx) e área sob a curva (ASC0-t) foram determinados utilizando os dados após transformação logarítmica. As formulações teste e referência foram consideradas bioequivalentes se os intervalos com 90% de confiança para a média geométrica da razão teste/referência ficassem compreendidos na faixa de 80% a 125%. Os intervalos com 90% de confiança para as razões das médias geométricas para Cmáx foi 105,18% (97,31%-113,70%) e para ASC0-t foi 99,33% (95,55%-103,26%). Em conclusão, os comprimidos de dicloridrato de betaistina 24 mg testados (Aché Laboratórios Farmacêuticos S.A.) foram bioequivalentes aos comprimidos de Labirin® 24 mg, de acordo com taxa e extensão de absorção.

Phytochemical evaluation, proximate analysis and laxative activity of linum usitatissimum tablet formulations.

Linum Usitatissimum seeds were collected and qualitatively analyzed for the identification of phytochemical constituents. The results showed the presence of bioactive constituents of carbohydrates, proteins and amino acids. The proximate analysis of the leaves revealed a composition of 3.21% total ash value, 7.61% alcohol soluble extractive value, 4.21% water soluble extractive value and 2.67% acid insoluble ash value. Laxative activity of three different formulations was studied. More research work is recommended on the plant leaves for isolation and characterization of bioactive compounds that may be active against laxative activity.