Stability-Indicating Chromatographic Methods for Simultaneous Determination of Mosapride and Pantoprazole in Pharmaceutical Dosage Form and Plasma Samples

Simple, sensitive, selective, precise, and stability-indicating thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) methods for the determination of mosapride and pantoprazole in pharmaceutical tablets were developed and validated as per the International Conference on Harmonization guidelines. The TLC method employs aluminum TLC plates precoated with silica gel 60F₂₅₄ as the stationary phase and ethyl acetate/methanol/toluene (4:1:2, v/v/v) as the mobile phase to give compact spots for mosapride (R _f 0.73) and pantoprazole (R _f 0.45) separated from their degradation products; the chromatogram was scanned at 276 nm. The HPLC method utilizes a C18 column and a mobile phase consisting of acetonitrile/methanol/20 mM ammonium acetate (4:2:4, v/v/v) at a flow rate of 1.0 mL min^?1 for the separation of mosapride (t _R 11.4) and pantoprazole (t _R 4.4) from their degradation products. Quantitation was achieved with UV detection at 280 nm. The same HPLC method was successfully used in performing calibrations in lower concentration ranges for both drugs in human plasma using ezetimibe as internal standard. The methods were validated in terms of accuracy, precision, linearity, limits of detection, and limits of quantification. Mosapride and pantoprazole were exposed to acid hydrolysis and then analyzed by the proposed methods. As the methods could effectively separate the drugs from their degradation products, these techniques can be employed as stability-indicating methods that have been successively applied to pharmaceutical formulations without interference from the excipients. Moreover the HPLC method was successfully used in the determination of both drugs in spiked human plasma.     

Gas‐phase pyrolysis in organic synthesis. Part 3: Novel cyclization of 2‐arylhydrazonopropanals into cinnolines1

3‐oxo‐3‐aryl‐2‐arylhydrazonopropanals (1) have been converted under thermal gas‐phase conditions cleanly into cinnolines (2) . A plausible mechanism is suggested to account for this transformation based on the kinetics and products of reaction. © 2001 John Wiley & Sons, Inc. Int J Chem Kinet 33: 402–406, 2001     

Gas phase hydration and deprotonation of the cyclic C3H3+ cation. Solvation by acetonitrile, and comparison with the benzene radical cation

The binding energies of the first 5 H2O molecules to c-C3H3+ were determined by equilibrium measurements. The measured binding energies of the hydrated clusters of 9-12 kcal/mol are typical of carbon-based CH+...X hydrogen bonds. The ion solvation with the more polar CH3CN molecules results in stronger bonds consistent with the increased ion-dipole interaction. Ab initio calculations show that the lowest energy isomer of the c-C3H3+(H2O)4 cluster consists of a cyclic water tetramer interacting with the c-C3H3+ ion, which suggests the presence of orientational restraint of the water molecules consistent with the observed large entropy loss. The c-C3H3+ ion is deprotonated by 3 or more H2O molecules, driven energetically by the association of the solvent molecules to form strongly hydrogen bonded (H2O)nH+ clusters. The kinetics of the associative proton transfer (APT) reaction C3H3+ + nH2O --> (H2O)nH+ + C3H2* exhibits an unusually steep negative temperature coefficient of k = cT(-63+/-4) (or activation energy of -37 +/- 1 kcal mol(-1)). The behavior of the C3H3+/water system is exactly analogous to the benzene+*/water system, suggesting that the mechanism, kinetics and large negative temperature coefficients may be general to multibody APT reactions. These reactions can become fast at low temperatures, allowing ionized polycyclic aromatics to initiate ice formation in cold astrochemical environments.     

Validated HPLC and HPTLC stability-indicating methods for determination of alfuzosin hydrochloride in bulk powder and pharmaceutical formulations

Two sensitive, selective, and precise stability-indicating, high-performance liquid chromatography and high-performance thin-layer chromatography methods have been developed for the determination of alfuzosin hydrochloride in the presence of its degradation products. Alfuzosin.HCl was subjected to stress alkaline, acidic, oxidative, thermal, and photo-degradation. The drug could be well separated from the degradation products upon applying the two methods. Separation by HPLC was achieved using an Xterra RP18 column and acetonitrile/0.02 M KH2PO4 (pH=3) in a ratio of 20:80 as mobile phase. The flow rate was 1 mL/min. The linearity range was 0.25 to 11 microg/mL with mean percentage recovery of 100.26 +/- 1.54. The HPTLC method used ALUGRAM Nano-SIL silica gel 60 F254 plates; the optimized mobile phase was methanol/ammonia (100:1.2). Quantitatively the spots were scanned densitometrically at 245 nm. A second order polynomial equation was used for the regression. The range was 0.5-7 microg/spot. The mean percentage recovery was 100.13 +/- 1.67. Two main degradation products were obtained in most stress conditions, separated, and identified by FT-IR and NMR spectral analysis, from which the degradation pathway was proposed. The two methods were validated according to the International Conference on Harmonization. In addition, the HPLC method was used to study the kinetics of alkaline and acid degradation of the drug.     

Surface Aggregation of Candida albicans on Glass in the Absence and Presence of Adhering Streptococcus gordonii in a Parallel-Plate Flow Chamber: A Surface Thermodynamical Analysis Based on Acid-Base Interactions

Adhesive interactions between yeasts and bacteria are important in the maintenance of infectious mixed biofilms on natural and biomaterial surfaces in the human body. In this study, the extended DLVO (Derjaguin-Landau-Verwey-Overbeek) approach has been applied to explain adhesive interactions between C. albicans ATCC 10261 and S. gordonii NCTC 7869 adhering on glass. Contact angles with different liquids and the zeta potentials of both the yeasts and bacteria were determined and their adhesive interactions were measured in a parallel-plate flow chamber.Streptococci were first allowed to adhere to the bottom glass plate of the flow chamber to different seeding densities, and subsequently deposition of yeasts was monitored with an image analysis system, yielding the degree of initial surface aggregation of the adhering yeasts and their spatial arrangement in a stationary end point. Irrespective of growth temperature, the yeast cells appeared uncharged in TNMC buffer, but yeasts grown at 37 degrees C were intrinsically more hydrophilic and had an increased electron-donating character than cells grown at 30 degrees C. All yeasts showed surface aggregation due to attractive Lifshitz-van der Waals forces. In addition, acid-base interactions between yeasts, yeasts and the glass substratum, and yeasts and the streptococci were attractive for yeasts grown at 30 degrees C, but yeasts grown at 37 degrees C only had favorable acid-base interactions with the bacteria, explaining the positive relationship between the surface coverage of the glass by streptococci and the surface aggregation of the yeasts. Copyright 1999 Academic Press.     

Green approach using monolithic column for simultaneous determination of coformulated drugs

Green chemistry and sustainability is now entirely encompassed across the majority of pharmaceutical companies and research labs. Researchers’ attention is careworn toward implementing the green analytical chemistry principles for more eco‐friendly analytical methodologies. Solvents play a dominant role in determining the greenness of the analytical procedure. Using safer solvents, the greenness profile of the methodology could be increased remarkably. In this context, a green chromatographic method has been developed and validated for the simultaneous determination of phenylephrine, paracetamol, and guaifenesin in their ternary pharmaceutical mixture. The chromatographic separation was carried out using monolithic column and green solvents as mobile phase. The use of monolithic column allows efficient separation protocols at higher flow rates, which results in short time of analysis. Two‐factor three‐level experimental design was used to optimize the chromatographic conditions. The greenness profile of the proposed methodology was assessed using eco‐scale as a green metrics and was found to be an excellent green method with regard to the usage and production of hazardous chemicals and solvents, energy consumption, and amount of produced waste. The proposed method improved the environmental impact without compromising the analytical performance criteria and could be used as a safer alternate for the routine analysis of the studied drugs.     

High-spin structure of yrast-band in 78Kr

Lifetime of levels up to 22⁺, have been measured in ⁷⁸Kr and an oblate shape is assigned to the ground state using the CSM and the configuration dependent shell correction calculations. Calculations further show that ⁷⁸Kr is highly γ-soft nucleus. The experimental Q _t values coupled with theoretical calculations indicate an oblate shape for ⁷⁸Kr at low spins and triaxial shape at higher spins