AN IMPROVED RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF ASPIRIN, ATORVASTATIN, AND CLOPIDOGREL IN PHARMACEUTICAL FORMULATION USING EXPERIMENTAL DESIGN METHODOLOGY

Objective: In this study an improved RP-HPLC method was developed for the simultaneous estimation of Aspirin, Atrovastatin, and Clopidogrel in pharmaceutical dosage form. For improving the separation, an experimental design approach was employed. Methods: Factors–independent variables (Organic modifier, pH of the mobile phase and flow rate) were extracted from the preliminary study and as dependent three responses variables viz. Capacity factor of tR1, resolution between Atorvastatin and internal standard, retention time of tR4 were selected. To improve method development and optimization, Derringer's desirability function was applied to simultaneously optimize the chosen three responses. Results: The procedure allowed deduction of optimal conditions and the predicted optimum was Acetonitrile: Methanol: 0.1% of Triethylamine (52:05:43, v/v/v), pH of the aqueous phase adjusted at to 3.0 with 10 % ortho phosphoric acid, and the separation was achieved within 8 minutes. The method showed good agreement between the experimental data and predictive value throughout the studied parameter space. Conclusion: The optimized assay condition was validated according to International Conference on Harmonisation (ICH) guidelines to confirm specificity, linearity, accuracy and precision. The proposed validated method was successfully applied for the analysis of commercially available dosage form

FAST CHIRAL HPLC PROCEDURE FOR THE SIMULTANEOUS DETERMINATION OF DROPROPIZINE ENANTIOMERS AND ITS NONPOLAR IMPURITY IN RAW MATERIAL AND PHARMACEUTICAL FORMULATION

Objective: Levodropropizine is a novel antitussive drug, which occurs as enantiomers. They are levodropropizine (2S) [LDP] and dextrodropropizine (impurity A) (2R) [DDP]. An isocratic chiral high performance liquid chromatographic (Normal phase HPLC) method has been developed and validated for simultaneous determination of dropropizine enantiomers along with non-polar impurity-B, (1-phenyl piperazine) [1-PP] in raw material and in dosage forms. Methods: The compounds were separated on chiral stationary phase (CSP) Chiralpak AD-H column, with a mixture of n-hexane, anhydrous ethanol, diethyl amine (DEA) in the ratio of 55:45:0.1 v/v as mobile phase at a flow rate of 1.4 ml/min. UV detection was performed at 254 nm. The method was validated for accuracy, precision, specificity, linearity, and sensitivity. The developed and validated method was successfully used for quantitative analysis of commercially available Tablets. Results: Total chromatographic analysis time per sample was ~5 min. with 1-PP, levodrpropizne, dextropropizine eluting with retention times of 2.5 min., 3.05 min., and 3.66 min., respectively. Validation studies revealed the method is specific, rapid, reliable and reproducible for levodropropizne and its impurity A and non chiral impurity B. Calibration plots were linear over the concentration ranges 0.5-5 µg/ml and 0.5-5 µg/ml for levodropropizine and dextrodropropizine respectively. Conclusion: The high recovery and low relative standard deviation confirm the suitability of the method for determination of dropropizine compounds in commercial tablets

DEVELOPMENT AND VALIDATION OF CHROMATOGRAPHIC METHOD FOR THE SIMULTANEOUS ESTIMATION OF OLMESARTAN MEDOXOMIL, AMLODIPINE BESYLATE, CILNIDIPINE IN COMBINATION TABLET DOSAGE FORM

Objective: To develop and validate a simple, sensitive and isocratic reverse phase high performance liquid chromatography (RP-HPLC) method for the simultaneous determination of olmesartan medoxomil (OLM), amlodipine besylate (AML) and cilnidipine (CIL) in pharmaceutical tablet formulation.Methods: In this work we have taken 2 combinations, combination 1-OLM & AML and combination 2-OLM & CIL. HPLC analysis was carried out by using reverse phase isocratic elution with a C 18 column and a mobile phase of 0.05 M ammonium acetate, acetonitrile and methanol in the ratio of 30:50:20, v/v, pH was adjusted to 7.3. Detection of the analyte was achieved by using UV detector at 240 nm.Results: The retention time of olmesartan medoxomil, amlodipine besylate and cilnidipine were 2.2, 3 and 4.5 minutes respectively. Linearity of the method was found to be in the concentration range of 10-100µg/ml for olmesartan medoxomil, 5-50µg/ml for amlodipine and 10-100µg/ml for cilnidipine. The correlation coefficient value was greater than 0.999 for all the analytes.Conclusion: The method was validated as per ICH guidelines and is applied for the estimation of these components simultaneously in pharmaceutical tablet formulation.Â

A Review on the Mechanical Modeling of Composite Manufacturing Processes

© 2016, The Author(s). The increased usage of fiber reinforced polymer composites in load bearing applications requires a detailed understanding of the process induced residual stresses and their effect on the shape distortions. This is utmost necessary in order to have more reliable composite manufacturing since the residual stresses alter the internal stress level of the composite part during the service life and the residual shape distortions may lead to not meeting the desired geometrical tolerances. The occurrence of residual stresses during the manufacturing process inherently contains diverse interactions between the involved physical phenomena mainly related to material flow, heat transfer and polymerization or crystallization. Development of numerical process models is required for virtual design and optimization of the composite manufacturing process which avoids the expensive trial-and-error based approaches. The process models as well as applications focusing on the prediction of residual stresses and shape distortions taking place in composite manufacturing are discussed in this study. The applications on both thermoset and thermoplastic based composites are reviewed in detail

Prediction of chiral separation of ketoprofen using experimental design

1334-1340The paper demonstrates how experimental design could be applied to predict chiral resolution and run time for indirect chiral high performance liquid chromatography (HPLC) analysis of ketoprofen. An attempt is made to establish quantitative relationship between chromatographic variables and the response factors (resolution and retention time). The effects of important chromatographic variables on chiral resolution and retention time have been highlighted by way of interaction studies. This technique enables optimal utilization of resources by avoiding trial and error approach. The study advocates that experimental design is a prospective tool to predict and optimize chromatographic conditions for chiral HPLC analysis