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ARTICLES Possible conformation of amphotericin B dimer in membrane-bound assembly as deduced from solid-state NMR pp 5699-5704 Yuichi Umegawa, Takeshi Adachi, Nobuaki Matsumori*, Michio Murata* Discovery and preclinical profile of teneligliptin (3-[(2S,4S)-4-[4-(3-methyl-1-phenyl-1H-pyrazol-5-yl)piperazin-1yl]pyrrolidin-2-ylcarbonyl]thiazolidine): A highly potent, selective, long-lasting and orally active dipeptidyl peptidase IV inhibitor for the treatment of type 2 diabetes pp 5705-5719

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It is a simple, precise and economical UV-spectrophotometric method has been developed for the estimation of Vandetanib from bulk. Two method was developed First method (A) applied was area under curve (AUC) in this method area was integrated in wavelength from 323.59-333.36nm. Second method (B) was first order derivative spectrometric method. In this method absorbance at λmin=311.27nm, λmax=340.54nm and zero cross=328.37nm was measured. Calibration curves were plotted for the method by using instrumental response at selected wavelength and concentration of analyte in the solution. Both the method linearity was observed in the concentration range of 5-30µg/ml at the λmax=328.44nm. Accuracy and precision studies were carried out and result were satisfactory obtained. The drug at each of the 80 %, 100 % and 120 % levels showed good recoveries that is in the range of 97.00 to 99.00% for both methods, hence it could be said that the method was accurate. Limit of detection (LOD) and limit of quantitation (LOQ) were determined for the method. The method was validated by the International Conference on Harmonization. All validation parameters were within the acceptable limit. The developed method was successfully applied to estimate the amount of vandetanib in pharmaceutical formulation.

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A simple, precise, accurate, and rapid high-performance thin layer chromatographic method has been developed and validated for the simultaneous quantitation of flunarizine dihydrochloride and propranolol hydrochloride in a combined capsule dosage form. The method was carried out on precoated silica gel 60 F254 TLC aluminum plate, (20×10 cm2). The solvent system was ethyl acetate:methanol:glacial acetic acid in the proportion of 8:1:1, (v/v/v). Rf value for flunarizine dihydrochloride and propranolol hydrochloride was found to be 0.62±0.02 and 0.18±0.02, respectively. The linearity regression analysis for calibration showed 0.999 and 0.999 for flunarizine dihydrochloride and propranolol hydrochloride with respect to peak area and height in the concentration range of 50-350 ng/spot and 500-3500 ng/spot, respectively. Accuracy of recovery studies was found to be 98-100.28 and 99.11-99.45% for flunarizine dihydrochloride and propranolol hydrochloride, respectively. The amounts of drug in marketed formulation were 100.5 and 101.25% of flunarizine dihydrochloride and propranolol hydrochloride, respectively. The method developed can be used for routine analysis in bulk drug and capsule dosage form.

The main aim of the study was to develop and validate simple, sensitive, precise and cost-effective method for the estimation of Adenosine in bulk and pharmaceutical dosage form as per ICH guidelines. Two spectrophotometric methods have been developed for determination of Adenosine from tablet dosage form. First method was area under curve method in which the range of 251.28-260.88 nm was selected. Second method was first order derivative spectrophotometric method which had absorbance measured at λ min = 243.99 nm, λ max = 268.62nm and Zero cross = 256.30 nm. The calibration curves were plotted for the method by using instrumental response at selected wavelengths and concentrations of analyte in the solution. Linearity for detector response was observed in the concentration range of 10-18μg/ml at the λ max = 256.89 nm. The method was validated by the International Conference on Harmonization using parameters of Accuracy, Precision, LOD and LOQ. Good reproducibility and recovery was observed in both the above methods with % RSD less than 2. The proposed methods were found to be rapid, specific, economical and accurate and can be successfully applied for the routine analysis of Adenosine in bulk and pharmaceutical dosage forms.

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