scholarly journals Quality by Design Approach for the Development and Validation of Glipizide, an Antidiabetic Drug, by RP-UPLC with Application to Formulated Forms and Urine

2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Cijo M. Xavier ◽  
Kanakapura Basavaiah ◽  
K. B. Vinay ◽  
N. Swamy
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
Quality By Design ◽  
Calibration Graph ◽  
Multivariate Approach ◽  
Antidiabetic Drug ◽  
Validation Criteria ◽  
Relative Standard ◽  
Quality By Design Approach ◽  
Development And Validation

Quality by design (QbD) refers to the achievement of certain predictable quality with desired and predetermined specifications. The objective of this study was to develop and demonstrate an integrated multivariate approach to develop and quantify the constituent concentrations of glipizide (GPZ) drug in its pure and tablet forms. The method was developed using Zorbax Extend C-18 (50 mm × 4.6 mm × 1.8 μm) column with mobile phase consisting of a mixture of phosphate buffer of pH 3.5 and acetonitrile (60 : 40 v/v). The method fulfilled validation criteria and was shown to be sensitive, with limits of detection (LOD) and quantitation (LOQ) of 0.001 and 0.005 μg mL−1, respectively. The percentage relative standard deviations for robustness and ruggedness were observed within the range of 0.1 and 0.99. The calibration graph was linear in the range of 0.005–300 μg mL−1. The applicability of the method was shown by the analysis of formulated drug and spiked urine samples. The proposed method can be used for routine analysis in quality control laboratories for its bulk and formulated product, and this is the first UPLC method reported for the assay of GPZ in bulk, formulated form and urine.

scholarly journals Implementation of Quality by Design for the Development and Validation of Pioglitazone Hydrochloride by RP-UPLC with Application to Formulated Forms

2012 ◽  
Vol 2012 ◽  
pp. 1-11 ◽  
Author(s):  
Cijo M. Xavier ◽  
Kanakapura Basavaiah
Keyword(s):  
Quality By Design ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Process Understanding ◽  
Validation Criteria ◽  
Relative Standard ◽  
Level Of Knowledge ◽  
Bulk Drug ◽  
Development And Validation

Quality by Design (QbD) is a philosophy that refines the level of knowledge associated with a product that uses process understanding to deliver a product with the desired critical quality attributes. The objective of this study was to develop an integrated multivariate QbD approach to develop and quantify the constituent concentrations of pioglitazone hydrochloride (PGZ) drug in its pure and formulated forms. To facilitate studies investigating the determination of PGZ in bulk drug and its pharmaceutical formulations, a rapid UPLC method was developed and validated for the determination of PGZ accompanied by its degradation studies in different stress conditions. The method fulfilled validation criteria and was shown to be sensitive, with limits of detection (LOD) and quantitation (LOQ) of 0.01 and 0.05 μg mL−1, respectively. The percent relative standard deviations for robustness and ruggedness were observed within the range of 0.1–1.74. The calibration graph was linear in the range of 0.05–300 μg mL−1. The applicability of the method was shown by analysis of formulated drug samples and spiked human urine. The proposed method can be used for routine analysis in quality controlled laboratories for its bulk and formulated product and this is the first reported UPLC method for the assay of PGZ.

Integrated Quality by Design (QbD) Approach for Stability Indicating RP-HPLC Method for Estimation of Tadalafil Hydrochloride in Bulk Drug and Pharmaceutical Formulations

2020 ◽  
Vol 16 ◽  
Author(s):  
Prajakta H Patil ◽  
B.M. Gurupadayya ◽  
P.D. Hamrapurkar
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
Quality By Design ◽  
Degradation Products ◽  
Hplc Method ◽  
Design Approach ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Quality By Design Approach ◽  
Bulk Drug

Background: In the view of the current FDA standardization and product quality control criteria, Quality by design approach for analytical methods gaining importance to develop a robust analytical method. A new Quality by Design approach by RP-HPLC was developed and validated for the quantification and purification of Tadalafil hydrochloride and its tablet formulations. Objective: The objective of the study was to develop and validate a simple, robust, and accurate method by QbD approach for detection Tadalafil hydrochloride and its degradation products in bulk drug and tablet formulation. Materials and Methods: The chromatographic separation was performed on JASCO Crest Pack RPC18 column (250mm×4.6mm, 5μm) with a mobile phase consisting of a mixture of mobile phase A: Acetonitrile: Methanol (40:20 v/ v) and mobile phase B: 0.01M Ammonium acetate in water adjusted pH 3.50± 0.05 with glacial acetic acid with 1.0ml/ min flow rate at 285nm. Box-Behnken's three-level 3 factorial design was employed to create and analyze a "Design Space" (DoE). This design was statistically analyzed by ANOVA, counter-plot, and 3D response surfaces plots which demonstrated that the model is statically significant. The developed method was validated as per ICH guidelines Q2 (R1). Results and Discussion: The tadalafil hydrochloride showed good regression (R2>0.9995) within test ranges, and the percent recovery was found to be 98% in marketed formulation. Conclusion: The method was found to be highly specific without the interference of impurities and degradation products of tadalafil hydrochloride. For quantification and routine quality control of tadalafil and its marketed formulation, the stability-indicating the RP-HPLC method could thus be extended.

scholarly journals Quality by Design Approach for Development and Validation of Stability Indicating RP-HPLC Method for Fosaprepitant Dimeglumine

2020 ◽  
Vol 32 (9) ◽  
pp. 2158-2164
Author(s):  
JALIL K. SHAIKH ◽  
MAZAHAR FAROOQUI ◽  
UMMUL KHAIR ASEMA SYED
Keyword(s):  
Mobile Phase ◽  
Quality By Design ◽  
Orthophosphoric Acid ◽  
Design Space ◽  
Acid Base ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hydrogen Sulphate ◽  
Quality By Design Approach

Quality by design approach has been used to develop simple, rapid, sensitive gradient RP-HPLC stability indicating method for fosaprepitant dimeglumine and its related impurities. The chromatographic method has been developed by using symmetry shield RP-18 (250 mm × 4.6 mm; 5 μm) column maintained at column temperature of 20 ºC. The mobile phase-A consisted of water and acetonitrile (800:200, v/v), added 2 mL of orthophosphoric acid and 0.17 g of tetrabutylammonium hydrogen sulphate. The mobile phase-B consisted of water and acetonitrile (200:800, v/v), added 2 mL of orthophosphoric acid and 0.17 g of tetrabutylammonium hydrogen sulphate. Gradient program was executed as time (min)/% MP-A: 0/80, 3/80, 12/40, 20/20, 24/20, 25/80, and 30/80. The UV detection was carried out at wavelength 210 nm and 20 μL of sample was injected. Sample cooler was maintained at 5 ºC. Stability of fosaprepitant dimeglumine sample was investigated in different stress condition as acid, base, oxidation, thermal, humidity and photolytic. The method was developed in two phases, screening and optimization. During the screening phase, the most suitable stationary phase, organic modifier, and solvent were identified based on the behaviour of each stationary phase with fosaprepitant dimeglumine and its impurities using each buffer and solvent. Total 18 experiments were performed to find out the best experimental condition. The optimization was done for secondary influential parameters like column temperature, gradient program, using six experiments to examine multifactorial effects of system suitability parameters and generated design space representing the robust region. A verification experiment was performed within the working design space and the model was accurate. Drug showed unstable behaviour under acid, base, oxidation, thermal, and humidity conditions. Apripetant was found as major degradation impurity. The method was validated as per ICH guideline for specificity, limit of detection (LOD), limit of quantitation (LOQ), linearity, accuracy, precision, ruggedness and robustness. Correlation coefficient is about 0.999 for all impurities, recovery is between 90% to 103% at all level. LOD value of each impurity is less than 0.01% w/w. DOE statistically based experimental designs proved to be an important approach in optimizing selectivity-controlling parameters for the organic impurities determination in FD API. The method was found to be specific, linear, accurate, precise and robust. The peak purity test results confirmed that the fosaprepitant dimeglumine 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 method. Present method is found to be suitable for routine analysis in quality control laboratory.

scholarly journals Development and validation of new analytical method for the simultaneous estimation of daunorubicin and cytarabine in bulk and pharmaceutical dosage form

2021 ◽  
pp. 32-39
Author(s):  
Kankipati Benjimen ◽  
K. Thejomoorthy ◽  
P.Sreenivasa Prasanna
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Regression Equations ◽  
Control Test ◽  
Pharmaceutical Dosage Form ◽  
Precise Method ◽  
Development And Validation ◽  
Quality Control Test

A simple, Accurate, precise method was developed for the simultaneous estimation of the Daunorubicin and Cytarabine inhalation dosage form. Chromatogram was run through BDS C18 150 x 4.6 mm, 5m. Mobile phase containing 0.1% OPA: Acetonitrile taken in the ratio 60:40 was pumped through column at a flow rate of 1.0 ml/min. Temperature was maintained at 30°C. Optimized wavelength selected was 240nm. Retention time of Daunorubicin and Cytarabine were found to be 2.245 min and 2.813. %RSD of the Daunorubicin and Cytarabine were and found to be 0.6and 0.3 respectively. %Recovery was obtained as 99.39% and 99.26% for Daunorubicin and Cytarabine respectively. LOD, LOQ values obtained from regression equations of Daunorubicin and Cytarabine were 0.03, 0.10 and 0.31, 0.94 respectively. Regression equation of Daunorubicin is y = 2677x + 703.5, y = 2524x + 104.7 of Cytarabine.Retention times were decreased and that run time was decreased, so the method developed was simple and economical that can be adopted in regular Quality control test in Industries.  

scholarly journals QbD approach to HPLC method development and validation of ceftriaxone sodium

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Krunal Y. Patel ◽  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
Unnati Patel
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Quality By Design ◽  
Hplc Method ◽  
Design Expert ◽  
Ceftriaxone Sodium ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation ◽  
Central Composite

Abstract Background Quality by design (QbD) refers to the achievement of certain predictable quality with desired and predetermined specifications. A quality-by-design approach to method development can potentially lead to a more robust/rugged method due to emphasis on risk assessment and management than traditional or conventional approach. An important component of the QbD is the understanding of dependent variables, various factors, and their interaction effects by a desired set of experiments on the responses to be analyzed. The present study describes the risk based HPLC method development and validation of ceftriaxone sodium in pharmaceutical dosage form. Results An efficient experimental design based on central composite design of two key components of the RP-HPLC method (mobile phase and pH) is presented. The chromatographic conditions were optimized with the Design Expert software 11.0 version, i.e., Phenomenex ODS column C18 (250 mm × 4.6 mm, 5.0 μ), mobile phase used acetonitrile to water (0.01% triethylamine with pH 6.5) (70:30, v/v), and the flow rate was 1 ml/min with retention time 4.15 min. The developed method was found to be linear with r2 = 0.991 for range of 10–200 μg/ml at 270 nm detection wavelength. The system suitability test parameters, tailing factor and theoretical plates, were found to be 1.49 and 5236. The % RSD for intraday and inter day precision was found to be 0.70–0.94 and 0.55–0.95 respectively. The robustness values were less than 2%. The assay was found to be 99.73 ± 0.61%. The results of chromatographic peak purity indicate the absence of any coeluting peaks with the ceftriaxone sodium peak. The method validation parameters were in the prescribed limit as per ICH guidelines. Conclusion The central composite design experimental design describes the interrelationships of mobile phase and pH at three different level and responses to be observed were retention time, theoretical plates, and peak asymmetry with the help of the Design Expert 11.0 version. Here, a better understanding of the factors that influence chromatographic separation with greater confidence in the ability of the developed HPLC method to meet their intended purposes is done. The QbD approach to analytical method development was used for better understanding of method variables with different levels.

scholarly journals Development and Validation of a Ultra Flow Liquid Chromatography Method for the Assay of Boceprevir Using a Quality-by-Design Approach

2020 ◽  
Vol 11 (SPL4) ◽  
pp. 3023-3032
Author(s):  
Manish Majumder ◽  
Ramesh B ◽  
Minaketan Tripathy
Keyword(s):  
Risk Assessment ◽  
Flow Rate ◽  
Mobile Phase ◽  
Quality By Design ◽  
Quality Attributes ◽  
Assay Method ◽  
Chromatography Method ◽  
Critical Quality Attributes ◽  
Critical Method ◽  
Quality By Design Approach

Quality by design guided. The assay method of Boceprevir is developed in accordance with ICH Q8(R2) guideline with due validation. .In this process, the Target analytical profile (TAP) of the drug was set and critical method parameters (CMP) were investigated by systematic risk assessment experimentation to control critical Quality Attributes (CQA). In this, A Cause Effect Risk Assessment Matrix with Control-Noise-Experiment (CNX) is used for identifying the high-risk variables i.e Percentage of Organic Modifier (% methanol), pH of the Buffer and flow rate of the mobile phase. The surface response methodology was applied to optimize the critical method parameters (CMP) as well as Critical Quality Attributes (CQA) to find out the Design space of the method. The Optimum assay method condition was mobile phase Acetate Buffer (50mM) pH 5.4: Methanol (11:89), Flow rate: 0.9 ml/min, Lambda Max: 207. The separation was achieved in the Eclip Plus C-18 column (250 × 4.6 mm, 5μm) at ambient temperature. The retention time of Boceprevir was found to be 4.2 min. The method evaluation was performed according to the (Q2R1) ICH guideline.

scholarly journals QbD Approach for the Development and Validation of RP-UHPLC Method for Quantitation of Vildagliptin

2017 ◽  
Vol 16 (1) ◽  
pp. 107-117
Author(s):  
Sharifa Sultana ◽  
Uttom Kumar ◽  
Md Shahadat Hossain ◽  
Dilshad Noor Lira ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Quality By Design ◽  
Response Surfaces ◽  
Routine Analysis ◽  
Pharmaceutical Dosage Forms ◽  
Independent Variables ◽  
Two Factors ◽  
Bulk Drug ◽  
Development And Validation

The present work describes a quality by design (QbD)-based rapid, simple, precise and robust RPUHPLC method for the routine analysis of vildagliptin in bulk drug and in pharmaceutical dosage forms. Chromatographic separation was achieved by a X-bridge C18 column with isocratic elution of mobile phase containing mixture of phosphate buffer (pH 6.8) and acetonitrile in the ratio of 67:33(v/v). The flow rate was 1.0 ml/min and the detection was done at 239 nm with photo-diode array plus (PDA+) detector. The optimization of chromatographic method was carried out by QbD approach using design of experiments (DoE). Two factors utilized for the experimental design of the method were (i) independent variables which comprise percentages of acetonitrile in mobile phase and flow rate and (ii) co-variates which include the retention time, tailing factor and theoretical plates. This design was statistically analyzed by ANOVA, normal plot of residual, box-cox plot for power transform, perturbation, counter plot and 3D response surfaces plots. This was further validated as per the requirements of ICHQ2B guidelines for linearity, LOD, LOQ, accuracy, precision, specificity and robustness. The results showed that proposed method is simple, sensitive and highly robust for routine analysis of vildagliptin.Dhaka Univ. J. Pharm. Sci. 16(1): 107-117, 2017 (June)

Development and Validation of Stability Indicating UPLC Method for Simultaneous Estimation of Phenylephrine and Fexofenadine in Suspension Dosage Form

2020 ◽  
Vol 13 (5) ◽  
pp. 5069-5074
Author(s):  
Rajitha G ◽  
Geetha Susmita Adepu
Keyword(s):  
Quality Control ◽  
Dosage Form ◽  
Orthophosphoric Acid ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Relative Standard ◽  
Pharmaceutical Industries ◽  
Acquity Uplc ◽  
Development And Validation ◽  
Liquid Chromatographic

Phenylephrine and fexofenadine are widely used products for common cold and allergic conditions. In this study, a simple, reliable, sensitive and economical Ultra Performance Liquid Chromatographic (UPLC) method was developed and validated for the simultaneous estimation of phenylephrine and fexofenadine in suspension dosage form. Efficient chromatographic separation was achieved on Acquity UPLC HSS C18 x 1.8μm column with mobile phase consisting of orthophosphoric acid buffer (pH = 2.8) and acetonitrile (55:45% v/v) at a flow rate of 0.3ml.min-1 and 1μl injection volume. TUV detector was used and detection wavelength was 272nm. The retention times of phenylephrine and fexofenadine were found to be 1.347 and 1.536 ± 0.01 mins respectively. The percentage recoveries of phenylephrine and fexofenadine were 99.93% and 99.31% respectively. The relative standard deviation for assay was found to be <2. The detection and quantification limits were found to be 0.04 and 0.13μg/ml for phenylephrine and 0.21 and 0.65μg/ml for fexofenadine respectively. Thus, the developed UPLC method was simple, rapid, sensitive and economical and it can be applied for the routine quality control analysis of combined dosage forms in quality control laboratories and in pharmaceutical industries.

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