A simple, rapid reverse phase high-performance liquid chromatographic method was developed and validated for the simultaneous estimation of Tenofovir and Emtricitabine in bulk and pharmaceutical dosage forms. Chromatography was carried out by using Hypersil, 250 X 4.6 mm, 5minternal diameter with a mixture of Buffer: acetonitrile in the ratio of 60:40 (v/v) as mobile phase. Determination of the different analytical parameter such as linearity, accuracy, precision and specificity, limit of detection (LOD), limit of quantification (LOQ) was done. The calibration curve was found to be linear for each analyte in the desired concentration range. The % recovery was found to be 99.85 and 99.99 for emtricitabine and tenofovir respectively. The proposed method is highly sensitive, precise, and accurate, which was evident from the LOD value of 0.4 and 1.3 for emtricitabine and tenofovir respectively and hence the present method can be applied successfully for the quantification of active pharmaceutical ingredient (API) content in the combined formulation of emtricitabine and tenofovir.
M. Venkatesh*, A.L.M.N. Sumanth, P. Venkateswa Rao.
A simple, rapid reverse phase high-performance liquid chromatographic method was developed and validated for the simultaneous estimation of Atazanavir and Ritonavir in bulk and pharmaceutical dosage forms. Chromatography was carried out by using Agilent XDB, 150 X 4.6 mm, 5minternal diameter with a mixture of Buffer : acetonitrile in the ratio of 45:55 (v/v) as mobile phase. Determination of the different analytical parameter such as linearity, accuracy, precision and specificity, limit of detection (LOD), limit of quantification (LOQ) was done. The calibration curve was found to be linear for each analyte in the desired concentration range. The % recovery was found to be 99.7 and 99.61 for Atazanavir and Ritonavir respectively. The preposed method is highly sensitive, precise, and accurate, which was evident from the LOD value of 2.4 and 2.2 for Atazanavir and Ritonavir respectively and hence the present method can be applied successfully for the quantification of active pharmaceutical ingredient (API) content in the combined formulation of Atazanavir and Ritonavir.
The HPLC method was developed for the estimation of Benzil impurity present in the Phenytoin. The method was carried out using a stationary phase of Hibar® column RP18 (250 X 4.6 mm I.D, 5µm), 25 mM potassium dihydrogen orthophosphate buffer (pH 3.0) and acetonitrile (20: 80 %v/v) used as mobile phase at a flow rate of 1.0 mL min-1 with a detection wavelength of 217 nm. The Rt were 5.45 min and 3.22 min for Benzil and Phenytoin respectively. The relative retention time was 1.65 min. The recovery of Benzil obtained was from 97.75 % w/w to 100.41 % w/w. The benzil was produced linear response from 0.1 to 1.5 µg mL-1. The R2 was 0.995. LOQ and LOD were 7.66 ng mL-1 and 23.23 ng mL-1 respectively. The proposed method valuable for the quantification of Benzil in Phenytoin for the safety of the drug in bulk and formulation.
A series of 2, 4‐disubstituted‐1,5‐benzodiazepine derivatives were synthesized by the condensation of o‐phenylendiamine and various 1‐(4’‐substituted phenyl)‐ 3‐ (6’’‐ methoxy napthaline)‐2‐propene‐1‐one. The structures of newly synthesized compounds were confirmed by IR, 1H NMR, mass and elemental analysis. All the compounds were tested for in vitro activities against a panel of Gram‐positive and Gram‐negative bacteria. All the compounds exhibited mild to moderate antimicrobial activity.
A simple, rapid and sensitive difference spectrophotometric method was used for the determination of Pantoprazole in pharmaceutical dosage forms. The method is based on the induced spectral changes upon changing the pH of the medium that differ in their UVspectra. Difference spectrum, obtained by keeping Pantoprazole in 0.1N H2SO4 in reference cell and Pantoprazole in 0.1N KOH in sample cell, showed two characteristic peaks at 296 nm and 314 nm with positive and negative absorbance respectively. Difference of absorbance between these two maxima was calculated to find out the amplitude, which was plotted against concentration. The calibration curve is linear over the concentration range of 5-25 μg/ml (r²= 0.996), with a detection limit of 0.0954μg/ml. The method was successfully applied to the commercial pharmaceutical drug without interference from common ingredient accompanying the drug. The result statistically compared with those obtained by the reference method. The proposed methods were successfully applied to the assay of Pantoprazole in pure and tablet dosage form. No interference was found from tablet excipients at the selected wavelengths and assay conditions. The data were compared with those obtained from the spectrophotometric method given in the literature and no difference was found statistically.
A number of hydrazone derivatives were synthesized, and were purified by crystallization or by column chromatography. Structures of all the synthesized compounds are supported by correct IR, 1H NMR, mass spectral and analytical data. Anti-inflammatory activity evaluation was carried out by using carrageenin-induced paw oedema assay and compounds I, II and III exhibited good anti-inflammatory activity, that is 38%, 37% and 52% at 75 mg/kg po, respectively. Therefore many researchers have synthesized these compounds as target structures and evaluated their biological activities. These observations have been guiding for the development of new hydrazones that possess varied biological activities.
P. Mail kumaran*, V. Mangayarkarasi, P. Parasuraman, S. Bhagyalakshmi, K. Vamsi krishna, N. Shireesha.
A simple, economical, rapid, accurate, precise spectrophotometric method was developed and validated for the anti-spasmodic agent, Drotaverine hydrochloride in active pharmaceutical ingredients (API) and intablet dosage forms. The absorption maxima of Drotaverine, was found to be at about 234 nm wave length using water as solvent. The method was found to be linear and obeys Beer’s law in the concentrationrange of 1-12µg/ml, with the correlation coefficient being more than 0.998. The relative standard deviation was found to be <2%. The percent recovery was within the range of 99% - 101%. The developed method was validated according to ICH guidelines and was found to be accurate and precise. The method can be applied for the routine analysis of Drotaverine hydrochloride in API andpharmaceutical dosage forms.
In the present work, eight novel 1-(8-methyl-furo[2,3-b]quinolin-2yl)ethanone derivatives [IVa-h] were synthesized by clasein schmidt condensation, it is condensation between1-(8-methyl-furo[2,3-b]quinolin-2yl)ethanone (ketone) and substituted aryl aldehyde to yield 1-(8-methyl-furo[2,3-b]quinolin-2yl)ethanone derivatives [IVa-h] called as chalcones. The structures of the synthesized compounds were characterized on the basis of IR, 1hnmr and Mass spectral data. Among all synthesized compounds only few selected compounds are screened for their anti-inflammatory activity by paw edema method, Diclofenac sodium is employed as a reference standard. From the results it is concluded that, compound IV-b and IV-f exhibited potent, rest of compounds exhibited mild to moderate activity anti-inflammatory activity.
N. Pramod*, M. Sreenivasulu, G. Mahaboob Basha, S. Chand Basha, Y. Pradeep, B.H.M. Jayakumar Swamy.
A simple, accurate, precise, and rapid high performance thin layer chromatographic method has been developed and validated for the estimation of rosiglitazone in tablet dosage forms. The method employed TLC aluminium plates precoated with silica gel 60 F 254 as the stationary phase. The mobile phase used was a mixture of Chloroform:Methanol (7:2) v/v. The detection of spot was carried out at 254 nm. The calibration curve was found to be linear between 200 to 2000 ng mL-1 with regression coefficient of 0.9992 and Rf value 0.53±0.01. The proposed method can be successfully used to determine the drug content of marketed formulation. The accuracy of the proposed method was determined by recovery studies and found to be 98.67 to 99.11 %. The proposed method is applicable to routine analysis of rosiglitazone in bulk and pharmaceutical formulations. The proposed method was validated according to various ICH parameters like linearity, accuracy, precision, specificity, limits of detection, limits of quantification, range and solution stability.
A simple, selective, accurate reverse-phase high performance liquid chromatographic method has been developed and validated for quantitative determination of Asenapine maleatein bulk and pharmaceutical formulations. The chromatographic separation was achieved using X Terra RP 18 (100mm × 4.6mm × 3.5μm) in isocratic mode employing Buffer (KH2PO4 and Tetrabutyl ammonium hydrogen sulphate pH 2.2), Acetonitrile and methanol in the ratio of 80:16:4(v/v) with a 1.2 mL/min flow rate was chosen. Detector wavelength monitored at 228 nm. The retention time was 6.1 min. The developed method is validated as per ICH Guidelines. The method is accurate (99.9-101.1%), precise (the relative standard deviations of intra and inter-day assay were 99.3% and 99.9% respectively) and linear within range 80-240μg/ml (R2=0.999) concentration and was successfully used in monitoring left over drug. The proposed method is applicable to stability studies and routine analysis of Asenapine maleatein bulk and pharmaceutical formulations.