The development of a meaningful dissolution procedure for drug products with limited water solubility has been a challenge to the pharmaceutical industry. Satranidazole (BCS Class II drug) is a new nitroimidazole derivative with potent antiamoebic action. There is no official dissolution medium available in the literature. In the present study, parameters such as saturation solubility in different pH medium, dissolution behavior of formulations, influence of sink conditions, stability, and discriminatory effect of dissolution testing were studied for the selection of a proper dissolution medium. Results of solubility data revealed that solubility of Satranidazole decreases with an increase in pH. Satranidazole showed better sink condition in 0.1&#x2009;N HCl as compared to other media. The drug and marketed formulations were stable in the dissolution media used. An agitation speed of 75&#x2009;rpm showed a more discriminating drug release profile than 50&#x2009;rpm. Using optimized dissolution parameters (paddle at 75&#x2009;rpm, 900&#x2009;mL 0.1&#x2009;N HCl) greater than 80&#x25; of the label amount is released over 60 minutes. UV-spectroscopic method used was validated for the specificity, linearity, precision, robustness, and solution stability. The method was successfully applied to granular formulations and also to marketed tablets containing 300&#x2009;mg Satranidazole.

Harshal Ashok Pawar

Pooja Rasiklal Joshi

Development and Validation of a Discriminating In Vitro Dissolution Method for Oral Formulations Containing Satranidazole

Maillard reaction is a nonenzymatic reaction between reducing sugars and free amino acid moieties, which is known as one of the most important modifications in food science. It is essential to characterize the structure of Amadori rearrangement products (ARPs) formed in the early stage of Maillard reaction. In the present study, the N&#x3b1;-acetyl-lysine-glucose model had been successfully set up to produce ARP, N&#x3b1;-acetyl-lysine-glucose. After HPLC purification, ARP had been identified by ESI-MS with intense [M+H]+ ion at 351&#x2009;m/z and the purity of ARP was confirmed to be over 90&#x25; by the relative intensity of [M+H]+ ion. Further structural characterization of the ARP was accomplished by using nuclear magnetic resonance (NMR) spectroscopy, including 1D 1H NMR and 13C NMR, the distortionless enhancement by polarization transfer (DEPT-135) and 2D 1H-1H and 13C-1H correlation spectroscopy (COSY) and 2D nuclear overhauser enhancement spectroscopy (NOESY). The complexity of 1D 1H NMR and 13C NMR was observed due to the presence of isomers in glucose moiety of ARP. However, DEPT-135 and 2D NMR techniques provided more structural information to assign the 1H and 13C resonances of ARP. 2D NOESY had successfully confirmed the glycosylated site between 10-N in N&#x3b1;-acetyl-lysine and 7&#x2032;-C in glucose.

Chuanjiang Li

Hui Wang

Manuel Ju&#xe1;rez

Eric Dongliang Ruan

Structural Characterization of Amadori Rearrangement Product of Glucosylated N&#x3b1;-Acetyl-Lysine by Nuclear Magnetic Resonance Spectroscopy

We investigate the interaction of Ba with the Ni(110) surface at elevated temperatures by means of Auger electron spectroscopy and low energy electron diffraction. The results show that annealing of the substrate causes desorption and ordering of the initially amorphous overlayer, resulting in c<svg style="vertical-align:-2.21957pt;width:45.737499px;" id="M1" height="15.0875" version="1.1" viewBox="0 0 45.737499 15.0875" width="45.737499" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg">
	
		
			<g transform="matrix(.017,-0,0,-.017,.062,12.138)"><path id="x28" d="M300 -147l-18 -23q-106 71 -159 185.5t-53 254.5v1q0 139 53 252.5t159 186.5l18 -24q-74 -62 -115.5 -173.5t-41.5 -242.5q0 -130 41.5 -242.5t115.5 -174.5z" /></g><g transform="matrix(.017,-0,0,-.017,5.944,12.138)"><path id="x32" d="M412 140l28 -9q0 -2 -35 -131h-373v23q112 112 161 170q59 70 92 127t33 115q0 63 -31 98t-86 35q-75 0 -137 -93l-22 20l57 81q55 59 135 59q69 0 118.5 -46.5t49.5 -122.5q0 -62 -29.5 -114t-102.5 -130l-141 -149h186q42 0 58.5 10.5t38.5 56.5z" /></g><g transform="matrix(.017,-0,0,-.017,17.877,12.138)"><path id="xD7" d="M528 54l-36 -38l-198 201l-198 -201l-36 38l197 200l-197 201l36 38l198 -202l198 202l36 -38l-197 -201z" /></g><g transform="matrix(.017,-0,0,-.017,31.629,12.138)"><use xlink:href="#x32"/></g><g transform="matrix(.017,-0,0,-.017,39.789,12.138)"><path id="x29" d="M275 270q0 -296 -211 -440l-19 23q75 62 116.5 174t41.5 243t-42 243t-116 173l19 24q211 -144 211 -440z" /></g>

		
	
</svg> and <svg style="vertical-align:-2.21957pt;width:45.737499px;" id="M2" height="15.0875" version="1.1" viewBox="0 0 45.737499 15.0875" width="45.737499" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg">
	
		
			<g transform="matrix(.017,-0,0,-.017,.062,12.138)"><use xlink:href="#x28"/></g><g transform="matrix(.017,-0,0,-.017,5.944,12.138)"><use xlink:href="#x32"/></g><g transform="matrix(.017,-0,0,-.017,17.877,12.138)"><use xlink:href="#xD7"/></g><g transform="matrix(.017,-0,0,-.017,31.629,12.138)"><use xlink:href="#x32"/></g><g transform="matrix(.017,-0,0,-.017,39.789,12.138)"><use xlink:href="#x29"/></g>

		
	
</svg> structures. It is observed that the induced ordering crucially affects the lineshape of the double Auger transition line Ba(73&#x2009;eV)N45O23P1, establishing this line as an index of ordering of the Ba overlayer. The underlying physics of this effect is discussed.

D. Vlachos

M. Kamaratos

S. D. Foulias

The Low Energy Auger Electron Spectroscopy Lines as an Index of the Ba Overlayer Order on the Ni(110) Surface

Silver nanoparticles were synthesized using solution combustion method with citric acid as fuel. The prepared silver nanoparticles exhibit fcc crystalline structure with particle size of &#x7E;50&#x2009;nm. The morphology and purity of the silver nanoparticles were also studied by high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray analysis (EDX). Surface-enhanced Raman scattering (SERS) spectra of 2,6-dicarbethoxy-3,5-bis(pyridine-3-yl)tetrahydro-1,4-thiazine-1,1-dioxide (DBTD) adsorbed on silver nanoparticles were investigated. Orientation of DBTD on silver nanoparticles has been inferred from normal Raman spectrum (nRs) and SERS spectral feature. The observed spectral feature evidenced that DBTD would adsorb on silver surface with tilted orientation through the lone pair electrons of C&#x2013;N, C=O, S=O, and pyridine ring. The present investigation has been a model system to deduce the interaction of drugs with DNA.

M. Anuratha

A. Jawahar

M. Umadevi

N. Edayadulla

V. G. Sathe

V. Meenakumari

A. Milton Franklin Benial

Orientation of 2,6-Dicarbethoxy-3,5-bis(pyridine-3-yl)tetrahydro-1,4-thiazine-1,1-dioxide on Silver Nanoparticles: Surface-Enhanced Raman Spectral Studies

A quantitative method using diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) was developed and validated for the estimation of ciprofloxacin in its tablet dosage forms. The solid-state samples were prepared by dilution in dry potassium bromide and were analyzed by FTIR spectrophotometer with DRIFT sampling technique. A linear relationship for the carbonyl peak area centered around 1709&#x2009;cm&#x2212;1 was observed in the range of 0.3&#x2013;1.5&#x25;&#x2009;w/w with good correlation coefficient of 0.998. The percent recovery of ciprofloxacin in three marketed tablet dosage forms was in the range of 98.76 &#xb1; 0.27. The present reported method is precise, reproducible, and eco-friendly. DRIFTS may have a potential as an alternative method for qualitative and quantitative analysis of ciprofloxacin in bulk drugs and tablet dosage forms.

Bhoomendra Bhongade

Sirajunisa Talath

Sunil Dhaneshwar

A Validated Method for the Quantitation of Ciprofloxacin Hydrochloride Using Diffuse Reflectance Infrared Fourier Transform Spectroscopy

Two UV-spectrophotometric methods have been developed and validated for simultaneous estimation of valsartan and hydrochlorothiazide in a tablet dosage form. The first method employed solving of simultaneous equations based on the measurement of absorbance at two wavelengths, 249.4&#x2009;nm and 272.6&#x2009;nm, <svg style="vertical-align:-3.39069pt;width:30.674999px;" id="M1" height="16.450001" version="1.1" viewBox="0 0 30.674999 16.450001" width="30.674999" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg">
	
		
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</svg> for valsartan and hydrochlorothiazide, respectively. The second method was absorbance ratio method, which involves formation of Q-absorbance equation at 258.4&#x2009;nm (isoabsorptive point) and also at 272.6&#x2009;nm (<svg style="vertical-align:-3.39069pt;width:30.674999px;" id="M2" height="16.450001" version="1.1" viewBox="0 0 30.674999 16.450001" width="30.674999" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg">
	
		
			<g transform="matrix(.017,-0,0,-.017,.062,12.162)"><use xlink:href="#x1D706"/></g>

			<g transform="matrix(.012,-0,0,-.012,9.45,16.25)"><use xlink:href="#x6D"/></g><g transform="matrix(.012,-0,0,-.012,19.159,16.25)"><use xlink:href="#x61"/></g><g transform="matrix(.012,-0,0,-.012,24.383,16.25)"><use xlink:href="#x78"/></g>

		
	
</svg> of hydrochlorothiazide). The methods were found to be linear between the range of 5&#x2013;30&#x2009;&#xb5;g/mL for valsartan and 4&#x2013;24&#x2009;&#x3bc;g/mL for hydrochlorothiazide using 0.1&#x2009;N NaOH as solvent. The mean percentage recovery was found to be 100.20&#x25; and 100.19&#x25; for the simultaneous equation method and 98.56&#x25; and 97.96&#x25; for the absorbance ratio method, for valsartan and hydrochlorothiazide, respectively, at three different levels of standard additions. The precision (intraday, interday) of methods was found within limits (<svg style="vertical-align:-0.4368pt;width:71.462502px;" id="M3" height="11.975" version="1.1" viewBox="0 0 71.462502 11.975" width="71.462502" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns="http://www.w3.org/2000/svg">
	
		
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</svg>). It could be concluded from the results obtained in the present investigation that the two methods for simultaneous estimation of valsartan and hydrochlorothiazide in tablet dosage form are simple, rapid, accurate, precise and economical and can be used, successfully, in the quality control of pharmaceutical formulations and other routine laboratory analysis.

Monika L. Jadhav

Manoj V. Girase

Shripad K. Tidme

Manish S. Junagade

Development and Validation of Spectrophotometric Methods for Simultaneous Estimation of Valsartan and Hydrochlorothiazide in Tablet Dosage Form

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International Journal of Spectroscopy - Table of contents 2014

International Journal of Spectroscopy | Hindawi

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