Qbd hplc for the method development
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
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
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
214201161
RP HPLC Stability Indicating Method Development and Validation of Pseudoephedrine Sulfate and Related Organic Impurities in Tablet Dosage Forms, Robustness by QbD Approach
Abstract Pseudoephedrine is used for the temporary relief of stuffy nose and sinus pain/pressure caused by infection such as the common cold and flu. Here we were reporting a simple and precise validated stability indicating RP HPLC method for estimation of Pseudoephedrine Sulfate and its related compounds in solid oral dosage forms. The stability indicating nature of current method has been demonstrated by a forced degradation study. All process related impurities and degradation products from forced degradation samples were well resolved from each other. The chromatographic separation of impurities was achieved with a Hypersil phenyl column (25 cm x 4.6 mm i.d. particle size 5 m) using buffer and acetonitrile in the ratio of 95:5 v/v respectively as the mobile phase. The buffer used in mobile phase contained 10 mM potassium dihydrogen phosphate and its pH was adjusted to 3.0 0.05 with diluted orthophosphoric acid. The flow rate of HPLC was 1.0 mL min 1 and the wavelength of UV detector at 210 nm. The method was shown a linear response over range of 0.125 mg mL 1 to 0.750 mg mL 1 PES and impurities. The correlation coefficient was more than 0.999. Performed the robustness by using design experiments. GRAPHICAL ABSTRACT
Analytical Chemistry Letters
Thirupathi Dongala Lakshmi Narasimha Rao Katakam Ashok Kumar Palakurthi Naresh Kumar Katari
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
29535881
Application of QbD based approach in method development of RP HPLC for simultaneous estimation of antidiabetic drugs in pharmaceutical dosage form
The aim of the proposed study was to develop a novel sensitive and rugged stability indicating HPLC method based on an approach of fractional factorial design (FFD) for the simultaneous of estimation of gliclazide and metformin hydrochloride without prior separation in tablets. Preliminary experiments were conducted to identify the critical attribute factors and using Taguchi screening method to assess risk management method process parameters. Later on FFD was applied to optimize the resolution as response between both drugs in short run time. Sixteen experimental runs were performed from grid search data using design of expert software v.7.0. Furthermore, the optimized method was then validated according to the ICH guidelines. The generated model using FFD for the resolution was found to be highly statistically significant (p 0.05) and after analyzing the optimized zone within the design space, the final chromatographic conditions were selected as mobile phase 60:20:20:0.5, pH 7.5, flow rate 1.0 ml/min and column temperature 25 degC using analytical column C18 Nucleosil ODS (250 x 4.6 mm2 i.d, 5 u) at 227 nm of detector wavelength. Validation of the developed method by QbD has manifested the specificity, accuracy and excellent linearity range and correlation values (R2) 0.997 and 0.996 for drugs. From the analysis it was measured that their LOD and LOQ values for the drugs were 0.035, 0.080 mg/ml and 0.40, 0.55 mg/ml. Therefore, a novel sensitive, accurate and stability indicating method was developed with high degree of practical utility of both drugs estimation in pharmaceutical dosage forms.
Journal of Pharmaceutical Investigation
Deepika Thakur Amandeep Kaur Suraj Sharma
139234615
HPLC Method Development by QbD Compatible Resolution Modeling (DryLab4)
Szabolcs Fekete Imre Molnar H-J Rieger Robert Kormany
93267480
Quality by Design (QbD) Based Development and Optimization of a Simple, Robust RP HPLC Method for the Estimation of Methotrexate
Methotrexate (MTX) is most widely utilized drug for anticancer therapy, as well as in the treatment of autoimmune diseases like arthritis and psoriasis. However, its estimation in different dosage forms is still a challenge. Though, various analytical methods have been reported, but they are tedious, difficult to reproduce, and time consuming. USP method is only reliable for MTX estimation, but suffers from disadvantage of having high buffer concentration leading to column blockage. So there is need to develop a novel HPLC method to overcome this problem. A simple, fast, and robust HPLC analytical method was developed by employing quality by design (QbD) for the estimation of drug in different dosage forms. The reverse phase (RP) HPLC method was successfully developed and validated according to International Conference of Harmonization (ICH) guidelines with respect to linearity, accuracy, precision, etc. Further, the method was applied for estimation of MTX in different dosage forms like tablet, injection, lipid nanocarriers, lipid polymer hybrid nanoparticles (LPHNPs) and gel. The good recoveries of MTX were obtained as more than 95% with RSD of 0.5 2% from 0.5 to 40 ug/mL, all values were found to be within the acceptable range. The results showed that the developed RP HPLC method could be successfully utilized for identification and quantification of MTX in any dosage forms, with high resolution, accuracy, and precision.
Neera Garg G Veera Raghava Sharma Bhupinder Singh Pradip Nirbhavane Om Prakash Katare
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
196011404
A QbD based approach to analytical method development and validation for the determination of selective drugs using hplc technique
Gauri Rao