A Validated Stability-Indicating HPLC Related substances method for Carmustine in bulk drug
A rapid, sensitive reversed phase stability-indicating high-performance liquid chromatographic (HPLC) assay method was developed and validated for quantitative determination of carmustine in bulk drugs and the degradation products generated from forced degradation. A gradient, reversed phase HPLC method was developed to separate the drug from the degradation products, using an YMC ODS-A C18 (250mm x 4.6) mm,5u column and the Mobile phase-A 0.01 M Potassium dihydrogen phosphate in water, adjust PH 3.2 with orthophosphuric acid and mobile phase-B methanol was used as mobile phase. The detection was carried out at wavelength 230 nm and 205 nm. The chromatographic resolution between its degraded products was found to be greater than two. The carmustine was subjected to stress conditions of acid, base, oxidation (30 % H2O2), thermal degradation and photolytic degradation. The degradation was observed for carmustine in alkali, acid and in thermal hydrolysis. The mass balance was close to 100 in all the stress conditions. The degraded products were well resolved from main peak. The developed method was validated with respect to linearity, accuracy, recovery, precision, system suitability, selectivity, robustness and forced degradation studies prove the stability indicating ability of the method.
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Comparative study and nutritional assesment of dehulled and whole hunteria umbellata seed
The nutritional compositions of Hunteria umbellata were examined in this study. Proximate, mineral and inorganic elements of dehulled Hunteria umbellata seed (DHUS) and whole Hunteria umbellata seed (WHUS) were analyzed. The proximate composition (%) of the DHUS and WHUS seed are as follows; crude protein (13.65) and (9.0), crude fibre (26.79) and (2.74), crude fat (2.87) and (14.97), ash (3.89) and (3.45), moisture (9.57) and (10.95) and carbohydrate (43.23) and (58.88). Hunteria umbellata are good source of macro and micro nutrient (mg/100g) with Potassium (1130) and 1150, Magnesium(180) and (189), Calcium (76) and (78), Sodium (87.5) and (90), Iron (60) and (63), Manganese (5) and (7) also present in appreciable quantities. The result of inorganic element (mg/100g) also revealed in Hunteria umbellata; Nitrogen (7.14) and (2.11), Carbon (52.1) and (68.4), Hydrogen (4.22) and (6.11), Sulphur (2.33) and (2.26) and Oxygen (34.3) and (21.1) respectively. Nitrogen content was determined by micro-Kjeldahl method. Total carbohydrate was calculated by the difference method while mineral analysis was carried out after acid digestion using spectrophotometer and flame photometry. The high value obtained for potassium, carbohydrate, and carbon reveal that Hunteria umbellata seed has potential of serving as supplement for food, source of synthetic and antimicrobial drugs, and traditional herbal medicine.
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Evaluation of Efficiency of Thermally Treated and Sulphuric acid Activated Sesamum Indicum carbons for Cd(II) removal from Aqueous solution
The efficiencies of activated carbons prepared from oil cake of Sesamum Indicum by thermal and sulphuric acid activation wereinvestigated for the removal of Cd(II) ions from aqueous solutions. Various parameters as a function of contact time, initialpH, initial adsorbent dosage and metal ion concentrations were studied. The optimum time required for the maximum removal of Cd(II) was found to be 1 hr for TAGOC and 2 hrs for STGOC. The equilibrium adsorption data were fitted to Langmuir and Freundlich adsorption isotherm models. The equilibrium adsorption isotherms showed that activated carbon has high affinity and sorption capacity for Cd(II) with monolayer sorption capacities of 44.92 mg/g for TAGOC and 35.97 mg/g for STGOC. The kinetic study indicated that the pseudo-second order rate equation better described the adsorption process. The adsorbent efficiency was also tested for the removal of Cd(II), Cu(II), Ni(II) and Zn(II) from synthetic electroplating wastewater. The results indicated that the prepared both activated carbons are efficient (99.9%), alternative low-cost adsorbent for the removal of Cd(II) and other metal ions from waste water.
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Synthesis and characterization of surfactant (PVP) capped Zinc Oxide nanorods
ZnO nanorods were successfully fabricated by using the chemical precipitated method. We report the synthesis and characterization of several sizes of ZnO nanocrystals, both in the free standing and the capped particle forms. The sizes of these nanocrystals could be controlled by capping them with polyvinylpyrollidone and were estimated by X-ray diffraction and transmission electron microscopy. The chemical compositions of the products were characterized by FT-IR spectroscopy. UV -Vis absorption spectroscopy measurements reveal that the capping of ZnO leads to blue shift due to quantum confinement effect.PL emission spectrum of PVP encapsulated ZnO shows red shift due to defect oriented emission. The morphology of the particles was evaluated by scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). Both the thermo gravimetric analysis (TGA) and differential thermal analysis (DTA) curves of the ZnO show that no further weight loss and thermal effect were observed at a temperature of above 510?C.
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Studies on the Additive Performance of Azo Phenol Liquid Crystal as Antioxidant for Base stock
Two novel azo phenols mesogenic group namely 2-sec-butyl-4-(p-tolyldiazenyl)phenyl 4-(dodecyloxy) benzoate I12a,and 4-((4-bromophenyl)diazenyl)-2-sec-butylphenyl 4-(dodecyloxy) benzoate I12b were synthesized .The prepared compound were characterized using FT-IR, 1H-NMR, Mass Spectroscopy and Elemental Analysis. Their mesophase was investigated by Differential Scanning Calorimetry (DSC). Their antioxidant efficiency for Egyptian lubricating base oil was tested via monitoring the oxidation reaction through the change in total acid number (TAN) and viscosity. The obtained results showed that, the efficiency of these compounds was ranked as follows I12a > I12b.
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Synthesis and Characterization of Poly[bis 4-methoxybenzylammonium] tetra-µ-chlorido-cadmate (II)
The crystal structure of the new inorganic-organic hybrid compound [4-OCH3C6H4CH2NH3]2[CdCl4] has been determined by single crystal X-ray diffraction The compound crystallizes in the triclinic space group P with lattice parameters a = 19.007(2), b = 7.3410(8), c = 7.4451(8) Å, , ? =97.222(1)°, V = 1030.59(19) Å3, and Z = 2. The framework of the title compound is built upon layers parallel to (100) made up from corner-sharing [CdCl6] octahedra. 4-methoxybenzylammonium cations are situated between the layers and connect them via an N-H…Cl hydrogen-bonding network. The Cd atom is located on an inversion centre and the coordination environment is described as distorted octahedra. Solid state 13C CP-MAS NMR spectroscopy is in agreement with the X – ray structure. DFT calculations allow the attribution of the carbon peaks to the independent crystallographic sites. Thermal analysis and Infrared spectroscopy were also used to characterize the complex.
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Ultrasonic Studies of Binary Mixture Ethyl Oleate and Toluene in the temperature range of 303.15K to 318.15k
Ultrasonic velocity, density and viscosity for binary liquid mixture of fatty acid ester Ethyl Oleate with toluene have been measured at 2 MHz ultrasonic frequency within the temperature range of 303.15K to 318.15k. Thermo-acoustic parameters like adiabatic compressibility, acoustic impedance and intermolecular free length are calculated. The results are interpreted for interaction studies among the molecules of the mixtures.
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Synthesis and characterization of a new noncentrosymmetric dihydrogenmonophosphate [C3H6N3S2]H2PO4
The crystal structure of the title organic-inorganic hybrid material [
C3H6N3S2]
H2P
O4, has been determined by single crystal X-ray diffraction. The compound crystallizes in the noncentrosymmetric orthorhombic space group
Pna21 with the lattice parameters a =
7.662 (1), b =
26.553 (3), c =
4.4258 (6) Å, V =
900.4 (2) Å3, and Z = 4. The framework is built upon layers parallel to (0 1 0) made up from H
2PO
4- entities associated by O---H...O strong hydrogen bonds. The organic cations are located between the layers and connect them via N-H…O and C-H…O hydrogen bonding network. The exocyclic C-N bond length reveals the presence of the imine and enamine tautomers in the starting reagent. Results from solid state
1H,
31P,
13C and
15N spectroscopy are in good agreement with the X-ray structure. Density functional theory calculations allowed for the assignment of the carbon and nitrogen peaks to the independent crystallographic sites.
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Physicochemical characterization of the Jubilee crude oil
The physicochemical parameters and some contaminants of crude oil samples from the Jubilee oil field at Cape Three Points, western region and Saltpond oil field in Central region of Ghana were analyzed to classify and assess the quality of the crude oils. The physicochemical parameters determined were density, specific gravity, API, pour point, total sulphur content, salt in crude, total acid number, viscosity, reid vapour pressure and ash weight whereas the contaminants measured were water and sediments. Results from the physicochemical parameters for both samples showed a perfect Pearson’s correlation (r ?1). Low water and sediments levels (<1%) were recorded for both crude oils. This is an indication of low or minimal microbial growth and reduced ability of both crude oils to serve as a collector of water soluble metals and salts. This enhances the quality of the crude oils making them less fouling and corrosion resistant at high temperatures. High API values (API>30), coupled with low specific gravity, viscosity and pour point for both crude oils make them light crude oils. The sulphur concentration for both samples were low and within globally accepted range of 0.1-0.5 wt. % for sweet crude oil.
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