HPLC METHOD DEVELOPMENT AND VALIDATION OF LERCANIDIPINE HCL AND ATENOLOL, CHARACTERIZATION OF ITS DEGRADANTS BY LC-MS/MS

Objective: An assay method was developed and validated for the simultaneous estimation of Lercanipine HCl and atenolol using RP-HPLC. Methods: An effective chromatographic separation was achieved using waters symmetry C18 column of dimensions 150x4.6 mm, 3.5 μm, as a stationary phase. 0.1 percent ortho phosphoric acid and acetonitrile in 50:50 v/v was used as a mobile process with a rate of flow 1 ml/min and UV detection was carried out at 230 nm, respectively. Isocratic chromatography at ambient temperature was performed. Results: Lercanidipine HCl and atenolol were separated by a running time of around 8 min. at 2.925 min. and 6.482 min. Respectively. By injecting the norm six times, device suitability parameters were studied and the outcomes were well under the acceptance criteria. The linearity analysis was performed at levels ranging from 10% to 150% and the R2 value was found to be 0.999. Conclusion: Assay method validation was performed by using the marketed formulation and found to be within the limit. Degradation tests were conducted and the degradants were characterized by using LC-MS/MS

(Chlorosulfinyloxy)-N,N-dimethylmethaniminium chloride mediated direct and chemoselective conversion of carboxylic acids into aldehydes

A new method for the direct conversion of carboxylic acids into aldehydes using (chlorosulfinyloxy)N,N-dimethylmethaniminium chloride and lithium triethylhydroborate (super-hydride) was established which provides a convenient way for the chemoselective reduction of carboxylic acids even with such functional groups as halide, ester, nitrile, olefin and ketone

Removal of lead(II) ions from aqueous solutions using activated carbon from Militia ferruginea plant leaves

The adsorption of lead(II) on to activated carbon developed from an indigenous Ethiopian medicinal plant leaves namely Birbira (Militia ferruginea) was investigated to assess the possible use of this adsorbent. The influences of contact time, adsorbent dose, Pb(II) concentration, pH and temperature on adsorption were investigated. The maximum adsorption took place at 3 h. at a dose of 4.0 g of adsorbent, and 97.3 % of Pb2+ adsorption at pH of 4.0. The amount of lead ion adsorbed per gram of the adsorbent increased with decreasing concentration of Pb2+. The percentage of adsorption had increased with the increasing temperature. The positive value of ∆H indicated that the adsorption of lead ions on the adsorbent was an endothermic process. The values of free energy (∆G) were negative as expected for a spontaneous process. The decrease in ∆G value with increasing temperature revealed that adsorption of the ion on the adsorbent became favorable at a higher temperature. The calculated value of ∆H was 25.05 kJ mol–1, ∆S was 135.48 JK-1 mol-1 and ∆G was also calculated for each temperature. The two theoretical adsorption isotherms, namely, Langmuir and Freundlich were used to describe the experimental results. The Freundlich adsorption isotherm best fits and adsorption capacity was calculated to be 3.3 mg of Pb(II) per g of adsorbent. The adsorption followed the first order kinetics and was found to be pH dependent being maximum at pH 4.0. The pH effect and desorption studies showed that ion exchange mechanism might be involved in the adsorption process. Reuse of the desorbed bio-adsorbent is possible. The effect of foreign ions on the removal of Pb(II) has been investigated. The removal of Pb(II) from industrial wastewater sample was also tested and showed that more than 97 % removal was possible. The results showed that activated carbon prepared from Birbira (Militia ferruginea) leaves could be used for the removal of Pb(II) from wastewater. KEY WORDS: Industrial wastewater, Lead removal, Adsorbent, Militia ferruginea  Bull. Chem. Soc. Ethiop. 2008, 22(3), 349-360

VALIDATED RP-HPLC METHOD FOR SIMULTANEOUS DETERMINATION OF ROSUVASTATIN CALCIUM AND EZETIMIBE IN PHARMACEUTICAL DOSAGE FORM

Objective: To develop and validate a rapid, sensitive and specific reverse phase high performance liquid chromatography (RP-HPLC) method for simultaneous determination of Rosuvastatin Calcium and Ezetimibe in a combined dosage form.Methods: The chromatographic separation of the two drugs were achieved using Enable C18G (5 μm, 250 mm x 4.6 mm i. d. column). The drugs were separated in isocratic elution mode with a mobile phase consists of Acetonitrile-Water (75:25, v/v) at a flow rate of 0.6 ml/min and a detection wavelength of 252 nm using a UV detector.Results: The linearity and range for both Rosuvastatin Calcium and Ezetimibe were 5-40 µg/ml (R2= 0.9995) and 5-40 µg/ml (R2= 0.9992), respectively. Accuracy of the method was determined through recovery studies by adding known quantities of standard drug to the preanalyzed test solution and was found to be 99.6-100.3 % and 99.5-99.9% for Rosuvastatin Calcium and Ezetimibe respectively. The % RSD values for both interday and intraday precision were found to be<2%.Conclusion: A rapid, sensitive and specific RP-HPLC method was developed and validated for simultaneous determination of Rosuvastatin Calcium and Ezetimibe in a combined dosage form and hence, it can be used in the quality control analysis of an active pharmaceutical ingredient and pharmaceutical dosage form.Â

Feasibility and growth of hatchery produced green mussel (Perna viridis) spat in Bhimili Estuary, Visakhapatnam, Andhra Pradesh

The Bhimili Estuary situated in Visakhapatnam District of Andhra Pradesh is a fairly large but shallow estuary and supports the livelihood of over 5000 fishers. Nearly 3000 clam/oyster pickers exploit the bivalve resources of this estuary. The Gostani River joins the sea at Bhimilipatnam carrying freshwater from Anantagiri hills, Padmanabhan, Boni, Pandrangi, Taditorru, Gudivada, Chittivalasa, Jutmill, Mulakuddu and Nagamayyapalem

Spectrophotometric determination of trace amounts of cadmium with iodide and methyl violet

445-446A selective spectrophotometric method based on the interaction of an anionic iodo complex of cadmium with methyl violet has been described for the determination of trace amounts of cadmium. The developed method is precise, accurate and has been applied to determination of cadmium at trace levels (25 ppb) in sea water and high purity samples of indium and zinc materials

Hatching, Growth and Feed Preference of Hatchlings of Volagalea cochlidium (Linnaeus, 1758)

The hatching, growth and feed preference of hatchlings of the whelk Volagalea cochlidium (Linnaeus, 1758) (synonymous with Hemifusus pugilinus) under laboratory conditions is described. The egg capsules were semi-transparent; light yellow in color and trapezoidal in shape. Each capsule had 75-80 embryos. The length of the capsules along with the holdfast ranged from 14.98 to 23.26 mm. The hatchlings crawled out of the capsules after 30 days of incubation at 28-30℃. The mean shell length of the newly hatched out hatchling was 1.364 ± 0.009 and mean width 0.096 ± 0.011 mm. The hatchlings were fed five different diets and reared for 62 days to compare the effects on growth and survival. The most preferred feed was mussel meat, followed by clam feed, shrimp meat. Higher growth rates were recorded for those fed with mussel meat and highest cumulative mortality occurred in those fed with oyster meat. The whelk is in high demand for its shell and operculum and is exploited indiscriminately. This study indicates its potential for aquaculture and replenishment of wild stock through stock enhancement programs using hatchery produced juveniles of the whel

Shell boring polychaete (Polydora sp.) infestation in black lipped pearl oyster Pinctada margaritifera

Black lipped pearl oyster Pinctada margaritifera of size ranging from 3 to 40 mm were collected from the rocky beach of Lawson’s Bay along Visakhapatnam coast and were reared in the marine hatchery of the Visakhapatnam Regional Centre of CMFRI. The oysters were reared in 1 t capacity fibre glass tanks in 32‰ filtered seawater, provided with continuous aeration and mixed microalgal diet comprising Isochrysis galbana and Cheatoceros calcitrans. During the course of domestication for a period of nearly 22 months, the oysters were regularly cleaned of fouling and boring organisms at monthly intervals. The growth was also recorded periodically. During this period