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  • Author or Editor: K. S. Babu x
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Summary

A stability-indicating gradient reverse-phase liquid chromatographic method was developed for the quantitative determination of process-related impurities and forced degradation products of oxcarbazepine in pharmaceutical formulation. The method was developed by using Inertsil cyano (250 × 4.6 mm) 5 μm column with mobile phase containing a gradient mixture of solvent A (0.01 M sodium dihydrogen phosphate, pH adjusted to 2.7 with orthophosphoric acid and acetonitrile in the ratio of 80:20 v/v) and B (50:40:10 v/v/v mixture of acetonitrile, water, and methanol). The flow rate of mobile phase was 1.0 mL min−1. Column temperature was maintained at 25°C and detection wavelength at 220 nm. Developed reverse-phase high-performance liquid chromatography (RP-HPLC) method can adequately separate and quantitate five impurities of oxcarbazepine, namely imp-A, imp-B, imp-C, imp-D, and imp-E. Oxcarbazepine was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Oxcarbazepine was found to degrade significantly in acid, base, and oxidative stress conditions. The degradation products were well resolved from oxcarbazepine and its impurities. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, and robustness.

Open access

Abstract

For the past few decades innovation in construction material has grown a lot. This leads to special concrete such as self-compacting concrete, geopolymer concrete, self-healing concrete, etc. To prepare a special concrete apart from regular concreting material some sort of special materials was also needed, like mineral and chemical admixtures. Hence it is necessary to study the effect of these admixtures in cement paste and mortar before studying the same in concrete. Hence an attempt is made to study the effect of mineral and chemical admixtures in the fresh and hardened properties of cement paste and mortar. For this study ultrafine natural steatite powder is taken as mineral admixture and polycarboxylic based superplasticizer and glenium stream 2 were taken as chemical admixtures. Ultrafine natural steatite powder was used as additive to cement in various percentages like 0%, 5%, 10%, 15%, 20% and 25%. Superplasticizer and viscosity modifying admixture were taken as 1.5% and 0.5%, respectively. Then various combinations were worked out. To study the fresh property of cement paste consistency, initial setting time and miniature slump cone test were done based on the results yield stress of cement paste also calculated empirically. To study the hardened property compression test on cement mortar was done. Based on the test results it is clear that the addition of ultrafine natural steatite powder increases the water demand hence reduces the workability. On the other hand, it increases the compressive strength up to a certain limit. Adding superplasticizer increases the workability and reduces the water demand and viscosity modifying admixture reduces the bleeding and segregation effects hence increases the compressive strength.

Open access

Abstract  

Simultaneous measurement of gross alpha and gross beta activities by liquid scintillation counting technique using LKB Wallac Quantulus 1220 liquid scintillation counter (LSC) equipped with Pulse Shape Analyzer (PSA) is described. Three sets of pure alpha and pure beta standards simulating the activity concentration values of real samples in terms of α/β activity ratios were used to calibrate the LSC. Calibration methodology for the Quantulus 1220 with respect to the above measurements using 241Am and 90Sr/90Y standards of respective activity concentrations of ~25 dpm and ~104 dpm is described in detail. Also highlighted the need to calibrate the LSC using another set of 241Am and 90Sr/90Y standards of low and high activity concentrations respectively. The practicability and working performance of these calibration plots was checked by the validation trials with test samples spiked with 241Am and 90Sr/90Y covering range of α/β activity ratios from 1:1 to 1:50.

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