QUANTITATIVE DETERMINATION OF TARTARIC ACID IN TOLTERODINE TARTRATE BY ION CHROMATOGRAPHY USING CONDUCTIVITY DETECTION

ABSTRACT The present paper deals with the development and validation of analytical method based on a single column high performance Ion chromatography with cation suppressed conductivity detection, developed for quantitation of tartaric acid. The diluent used for the preparation of sample solution was water and injected into a standard chromatographic system connected with 250mm length, 4.0 mm ID and 5.0 μm particle size Metrosep A supp 5 Ion exchange column and suppressed conductivity detector. The developed analytical method was highly precise and accurate compared to titration methods and HPLC-UV detection methods to analyze the counter-ion tartaric acid in Tolterodine tartrate drug substance. Calibration curves were linear with correlation co-efficient of > 0.999 for tartaric acid. The % RSD of area response of tartaric acid in standard injections was below 1.0, which demonstrates the system precision. The % RSD of results in samples is below 1.0, which demonstrates the method precision of the test procedure. The accuracy of the method is also studied and observed between 99% and 101%. The developed method was validated according to ICH guidelines for the quantitative determination of tartaric acid in Tolterodine tartrate taken for the study

A VALIDATED NORMAL PHASE CHIRAL LC METHOD FOR THE ENANTIOMERIC SEPARATION OF SERTRALINE AND ITS Cis-(1R, 4R) ENANTIOMER ON AMYLOSE BASED STATIONARY PHASE

ABSTRACT A simple and rapid chiral liquid chromatographic method was developed for the enantiomeric separation of Sertraline hydrochloride (cis-(1S, 4S)-4-(3, 4-dichlorophenyl)-N-methyl-1,2,3,4-tetrahydronaphthalen-1-amine hydrochloride) and its undesired cis-enantiomer (cis-(1R, 4R)-4-(3, 4-dichlorophenyl)-N-methyl-1,2,3,4-tetrahydronaphthalen-1-amine hydrochloride). Superior resolution between Sertraline and its cis-(1R, 4R) enantiomer was achieved on amylase based Chiralpak AD-H (250 x 4.6 mm, 5 µm particle size) column using hexane, isopropyl alcohol, ethanol and diethyl amine (850:100:50:0.1 v/v/v/v) as mobile phase at 25 °C temperature. Flow rate was kept as 1.0 ml/min and elution was monitored at 215 nm. The sample concentration was 0.3 mg/ml. The effects of the mobile phase composition, the flow rate and the temperature on the chromatographic separation were investigated. Developed method is capable to detect (LOD) and quantitate (LOQ) cis-(1R, 4R) enantiomer to the levels of 30 and 120 ng/ml respectively, for 10 µl injection volume. The percentage RSD of the peak area of six replicate injections of cis-(1R, 4R) enantiomer at LOQ concentration was 4.9. The percentage recoveries of cis-(1R, 4R) enantiomer from Sertraline were ranged from 93.8 to 103.9. The test solution and mobile phase was observed to be stable up to 24 h after the preparation. The developed method was validated with respect to limit of detection (LOD), limit of quantitation (LOQ), precision, linearity, accuracy, robustness and ruggedness

Electrospinning process parameters dependent investigation of TiO2 nanofibers

This paper reports the electrospinning fabrication and characterization of TiO2 nanofibers. Various electrospinning process parameters such as applied voltage, distance tip-collector, solution flow rate and polymer (PVP) concentration are studied. The prepared nanofibers were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), thermogravimetric-differential thermal analysis (TG-DTA) and Fourier transform infrared spectroscopy (FTIR). XRD pattern of TiO2 nanofibers evidenced the presence of mixed phases of anatase and rutile. TG/DTA investigation showed the characteristic peaks corresponding to the heating behavior of TiO2-PVP mat. FTIR investigation endorsed a vibration peak at 660 cm−1 associated with the characteristic TiOTi bond. With the optimized process parameters, TiO2 nanofibers diameter was found to be reduced to 74 nm as compared to the first sample prepared with the diameter of 343 nm. Furthermore, these nanofibers were employed as the photoanode material for the preparation of dye-sensitized solar cell (DSSC) and photovoltaic study is evaluated. Keywords: Electrospinning, Nanofibers, Process parameters, X-ray diffraction, Surface morpholog

A VALIDATED STABILITY-INDICATING METHOD FOR THE DETERMINATION OF RELATED SUBSTANCES AND ASSAY OF PAMIDRONATE SODIUM PENTAHYDRATE BY HPLC WITHOUT DERIVATIZATION

ABSTRACT A high performance liquid chromatography (HPLC) method is developed for determination related substances and assay in Pamidronate sodium without derivatization. The isocratic method was developed by using column Zorbax SB-C18 (250 mm x 4.6 mm), 5 µm employing the mobile phase containing the buffer (0.4 % v/v n-Hexylamine in water with pH 7.5): Methanol: Acetonitrile (75:25:05 v/v/v). This method is compatible to conductivity detector, Evaporative Light Scattering (ELS) detector and Refractive Index (RI) detector. The Limit of detection (LOD) and limit of quantitation (LOQ) was established for Pamidronate sodium with Conductivity detector, ELS detector and RI detector. The conductivity detector was found to be suitable for related substances determination in Pamidronate sodium when compared with ELS and RI detectors. The LOQ values obtained for phosphoric acid impurity is 0.05% and phosphorus acid impurity is 0.04% with respect to the target analyte concentration (1 mg mL -1 ) by using conductivity detector. The relative response factor was established by linearity method for phosphoric acid impurity and phosphorous acid impurity against Pamidronate sodium by using conductivity detector. The method was validated with respect to accuracy, precision, linearity and robustness by using conductivity detector. Specificity of the method was demonstrated in the presence of known impurities and degradation impurities