Qbd for the hplc method development
208707559
HPLC METHOD DEVELOPMENT FOR DETERMINATION OF PYRAZINAMIDE AND RELATED SUBSTANCE BY USING QUALITY BY DESIGN (QBD) APPROACH
A robust and simplified high performance liquid chromatography (HPLC) method was developed for the estimation of Pyrazinamide and its related substance. A systematic approach, one of the parts of QbD (quality by design) was used in suitable analytical method development. The HPLC segregation method was carried out with C 18 Column (3.9x300 mm, I. D. 10 um) a mobile phase of phosphate buffer: acetonitrile (pH 3.0) 90:10 v/v, detected at 270 nm. Optimization to this method was done by response surface methodology by applying a three level Box Behnken design with three center points.
European Chemical Bulletin
Ashish Dalal Mohamamad Imran Anees Faraz Khan Mallinath M Langade Firoz A Kalam Khan Aniruddha Chabukshwar Jaiprakash N Sangshetti
198344825
QbD approach in RP HPLC method development for the assay of benzocaine and diclofenac in dosage forms
The present study was conducted to determine simultaneous various response optimization with the help of Derringer's desirability function. Using the optimization HPLC method development was done to detect Benzocaine andDiclofenac in the marketed pharmaceutical formulation. Liquid chromatography using C18column was used with Central Composite design for the study. DoE is a tool for the optimization of composition parameters. It is utilized for the evaluation of principal effects along with their interactions. CCD is a part of RSM which shows quadratic response surfaces without a three level factorial design. Twenty experiments along with 5 center points were studies with three factors for BEN and DIC in A: Content of Acetonitrile in mobile phase w/w) B: Flow rate (ml/mins) C: pH. The factor space was increased within the range of Acetonitrile concentrations from 55 65 v/v, pH 3 4, Flow rate change 0.8 1.2 ml/min, the capacity factor for peak of benzocaine, (k1) the retention time of Diclofenac(tR2) Resolution of the critical separated peak, Benzocaine and Diclofenac, (Rs1,2) were used as responses. The resolution between peak (Rs1,2) were found to be greater than 1.5 in the preliminary study. Therefore, these 2 peaks are critical peaks and utilized as response for global optimization. Predicted contour data for Rt was verified and it satisfies with experimental data.
K Manikandan Karunanidhi Santhana Lakshmi Aswitha Pai
198351324
Quality by Design (QBD) Approach to Stability Indicating RP HPLC Method Development and Validation for Simultaneous Estimation of Esomeprazole and Naproxen in Tablet Dosage Form
Khondokar Farjana Urmi Rahima Khatun S M Ashraful Islam
181946781
APPLICATION OF QBD LIFE CYCLE APPROACH FOR STABILITY INDICATING HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF IMPURITIES IN TENOFOVIR DISOPROXIL FUMARATE AND EMTRICITABINE COMBINATION TABLETS
International Research Journal Of Pharmacy
Bhupatsinh Vihol Seema Kothari Parth Patel Nimit Vasa Vrajesh Prajapati
204834218
Stability indicating RP HPLC method development and validation for determination of 9 impurities in apixaban tablet dosage forms. Robustness study by Quality by Design approach.
Quality by Design (QbD) based high resolution HPLC method is described for impurities in Apixaban (APX) in the tablet dosage form. Employing a simple and stability indicating HPLC method, nine known impurities were quantified with good peak resolution. Mobile phase A (MP A) was prepared with buffer and acetonitrile 90:10 v/v, while Mobile phase B (MP B) contained water and acetonitrile (ACN) 10:90 v/v. The Gradient program was at 0 min, MP A 75% B 25% 20 min, MP A 65% B 35% 30 min, MP A 40% B 60% 40 min, MP A 40% B 60% 42 min, MP A 75% B 25% and 50 min, MP A 75% B 25% The chromatographic separation was achieved by using Zorbax RX C18 250 x 4.6 mm column, 5mm (1.0 mL/min, 280 nm, 50 mL) and column temperature 40degC. Several separation studies were carried out using Design of Experiments (DoE) to optimize the method. Validation results confirm the applicability of the developed method for quality analysis and stability studies of the regular product on the manufacturing stream.
Biomedical chromatography BMC
Balasubramanian V Naresh Kumar Katari Thirupathi Dongala Sreekantha Babu Jonnalagadda
215812305
Integration of MS and UV Data for Peak Tracking in HPLC Method Development
(QbD) and Lifecycle Management concepts into pharmaceutical method development promise to improve the quality of methods throughout the method lifecycle. Quantitative characterization of a robust analytical method design space, a central element of the QbD methodology, has been consistently demonstrated to improve method performance and repeatability, thereby reducing downstream failures [1, 2, 3] This analytical method design space has recently been referred to in Analytical QbD circles as the method operable design region (MODR) [4] Software such as Fusion QbD (S Matrix Corporation, Eureka, CA USA) promotes this approach with the ability to generate statistically defensible multifactor designed experiments, automatically transcribe these experiments into readyto run sequences and instrument control methods within the Chromatography Data Software (CDS) and directly import all experiment results from the CDS for automated modeling and visualization.
214288778
DEVELOPMENT OF HPLC METHOD FOR DETERMINATION OF TAMSULOSIN USING QUALITY BY DESIGN (QBD) APPROACH
An HPLC method for Tamsulosin was developed by using a quality by design (QbD) novel concept. QbD has gained importance in recent times due to regulatory requirements in industrial application. Chromatographic separation of Tamsulosin was carried out by using C 8 column, and mobile phase used was methanol and distilled water (40:60 v/v) for proper separation process. Separation by using water as a solvent is beneficial as it is cost effective process and industrially applicable. In the development of the HPLC method, factors like injection volume, conc. of methanol, the column vent temperature is critical in maintaining. Hence the Box Behnken optimization model was applied for the main, interaction and quadratic effects of these three factors on the selected response. The effect of these parameters was studied on the tailing factor (resolution) Results were analysed during a surface diagram. Verification of the software generated result was done by taking six replicates of the run. Finally, the method was validated according to ICH guidelines.
European Chemical Bulletin
Jaiprakash N Sangshetti Dhanashree K Chivte Mohamamad Imran Anees Mallinath M Langade Firoz A Kalam Khan Rana Zainuddin Zahid Zaheer Paresh Ramesh Mahaparale
196892195
Application of chemometric approach for QbD Enabled development and validation of an RP HPLC method for estimation of methotrexate
Abstract The present work describes Quality by design (QbD) oriented development of a reverse phase high performance liquid chromatographic (RP HPLC) method for quantification of methotrexate (MTX) Initially, for performing HPLC studies with UV detector, an appropriate wavelength was selected using a novel technique of Principal Component Analysis (PCA) Risk assessment study was performed, followed by factor screening study using a fractional factorial design (FFD) Subsequently, factor optimization was conducted using a central composite design (CCD) with flow rate and mobile phase ratio as the critical method parameters (CMPs) and tailing factor (TF) theoretical plate count (TPC) and assay selected as the critical analytical attributes (CAAs) Polynomial modeling was performed to embark upon an optimal solution, followed by numerical and graphical optimization. Chromatographic separation was conducted using the mobile phase composition of acetonitrile (ACN) and ammonium acetate buffer (10 mM, pH 6) in the ratio of 25:75 v/v, flow rate of 0.8 mL/min, column oven temperature of 40 degC, and UV detection at 257 nm. Further, the analytical method was validated as per ICH Q2(R1) guidelines for linearity, accuracy, precision, sensitivity and robustness, ratifying that all the parameters were within the acceptable limits for quantification of MTX. GRAPHICAL ABSTRACT
Journal of Liquid Chromatography Related Technologies
Atul Jain Sarwar Beg Sumant Saini Teenu Sharma Om Prakash Katare Bhupinder Singh
139234615
HPLC Method Development by QbD Compatible Resolution Modeling (DryLab4)
Szabolcs Fekete Imre Molnar H-J Rieger Robert Kormany
99421250
Analytical QbD based systematic bioanalytical HPLC method development for estimation of quercetin dihydrate
ABSTRACT The current work entails development of rapid, sensitive, and inexpensive high performance liquid chromatographic method of quercetin dihydrate using the quality by design approach. Quality target method profile was defined and critical analytical attributes (CAAs) were earmarked. Chromatographic separation was accomplished on a C18 column using acetonitrile and ammonium acetate buffer (35:65) %v/v (containing 0.1% acetic acid, pH 3.5) as mobile phase at 0.7 mL/min flow rate with UV detector at 237 nm. Screening studies using fractional factorial design revealed that organic modifier, injection volume, column temperature, and buffer strength have significant influence on method CAAs, namely, peak area, retention time, and peak tailing. The critical method parameters were systematically optimized using Box Behnken design. Response surface mapping was used along with numerical optimization and desirability function for identifying the optimal chromatographic conditions. Linearity was observed in the drug concentration ranging between 2 and 50 ug/mL. Accuracy analysis revealed mean recovery between 93.6 and 96.2% while precision study revealed mean recovery between 93.7 and 96.5% Limits of detection and quantification of the developed method were found to be 12.1 and 36.6 ng/mL. Overall, the studies construed successful development of chromatographic method of quercetin with enhanced method performance. GRAPHICAL ABSTRACT
Premjeet Singh Sandhu Sarwar Beg Rajendra Kumar Om Prakash Katare Bhupinder Singh