Optimizing surface finish in WEDM using the taguchi parameter design method

International audienc

METHOD DEVELOPMENT AND VALIDATION OF NORETHINDRONE ACE-TATE ASSAY AND ITS RELATED IMPURITIES IN API AND PHARMACEUTICAL FORMULATION WITH ORTOGONAL DETECTOR TECHNQUES

Objective: To develop and validate a sensitive and stability indicating gradient reverse phase ultra-high performance(UHPLC-PDA) liquid chromatography with photodiode array(PDA) and mass spectroscopy (MS) of Norethindrone Acetate (NA) assay and organic impurities (OI) in active pharmaceutical Ingredient(API) and Pharmaceutical Formulation (PF).Methods: The chromatographic conditions were optimized using Zorbax SB-C18 analytical UHPLC column with the dimensions (100 x 2.1) mm and 1.8 μm particle sizes. The mobile phase consisted of water (solution A) and acetonitrile (solution B) with gradient elution as mentioned time (min)/% Solution B: Initial/40,0.2/40, 9.2/55,12.0/55,12.2/90,15.5/90, 15.8/40 and 18.0/40. The flow rate was at the rate of 0.4 ml/min and the detection wavelengths were 254 nm and 210 nm. The column was kept at 40 °C and the injection volume was 5 μL. Stability of NA sample in different conditions was investigated by exposing the drug to stress study utilizing acid, base, oxidation, thermal, Humidity and photolytic.Results: There was no interference from excipients, impurities or degradation products at the retention time of NA about 9.1 min indicating the specificity of the method.The drug showed good stability under oxidation, thermal, humidity and photolytic conditions, but significant degradation was observed under acid and base conditions. The procedure was validated for specificity, linearity, accuracy, precision and robustness. The degradation products were well resolved from NA and its impurities. The obtained LOD (Limit of detection) values are 0.001% to 0.015% and LOQ (Limit of quantification) values are 0.003% to 0.05% of impurities.Conclusion: A sensitive, rapid, specific and stability indicating gradient Reverse Phase UHPLC-PDA-PDA with MS (Orthogonal detectors) method for the determination of NA for the assay and organic impurities was successfully developed. The developed method was validated to be specific, linear, accurate, precise and robust. The peak purity and LC-MS test results confirmed that the NA peak was homogenous in all stress samples and the mass balance was found to be more than 99%, thus proving the stability indicating power of the metho

Synthesis, characterization and nuclease activity of copper(II), nickel(II), cobalt(II) and iron(II) complexes with oxime-thiosemicarbazones

1233-1238A novel ligand viz. l-phenyl- 1,2-propanedione-2-oxime thiosemicarbazone (PPDOT) has been synthesized and characterized. Complexes of copper(II), nickel(II), cobalt(II) and iron(II) with PPDOT have been synthesized and characterized by molar conductance, magnetic moments, electronic, IR and ESR spectroscopy. Electrochemical behaviour of these complexes is investigated by cyclic voltammetric studies. The nuclease activity of these complexes has been carried out on double stranded pBR 322 plasmid DNA by using gel electrophoresis experiments in absence and in the presence of oxidant (H2O2) . Metal complexes of diacetylmonoxime thiosemicarbazone (DAMOT) are also investigated for better compariso

Luminescence and optical absorption properties of Nd3+ ions in K-Mg-Al phosphate and fluorophosphate glasses

Absorption and emission properties and fluorescence lifetimes for the transition of Nd3+ ions embedded in P2O5-K 2O-MgO-Al2O3 (PKMA)-based glasses modified with AlF3 and BaF2 are reported at room temperature. The observed energy levels of Nd3+ ions in these glasses have been analysed through a semi-empirical free-ion Hamiltonian model. The spin-orbit interaction and net electrostatic interaction experienced by the Nd3+ ions follow the trend as PKMA>PKMA+AlF3> PKMA+BaF2 glasses. Judd-Ofelt analysis has been carried out on the absorption spectra of 1.0 mol% Nd3+-doped glasses to predict the radiative properties for the fluorescent levels of the Nd3+ ion. Branching ratios and stimulated emission cross-sections show that the transition of the glasses under investigation has the potential for laser applications. The Inokuti-Hirayama model has been applied to investigate the non-radiative relaxation of the Nd3+ ion emitting state, 4F3/2. Based on the decay curve analysis, concentration quenching of the 4F3/2 emission has been attributed to a cross-relaxation process between the Nd 3+ ions