Analytical quality-by-design (AQbD) guided development of a robust HPLC method for the quantification of plumbagin from Plumbago species

2021 ◽  
pp. 1-9
Author(s):  
Ritu Tiwari ◽  
Amit Kumar ◽  
Pavitra Solanki ◽  
Mahaveer Dhobi ◽  
Velusamy Sundaresan ◽  
...  
Keyword(s):  
Quality By Design ◽  
Hplc Method ◽  
Analytical Quality

scholarly journals Analytical Quality by Design Assisted HPLC Method for Quantification of Canagliflozin/ Metformin and Stability Studies

2019 ◽  
Vol 53 (4s) ◽  
pp. s699-s709
Author(s):  
Sunitha Gurrala ◽  
Shivaraj Shivaraj S ◽  
Subrahmanyam CVS Subrahmanyam ◽  
Panikumar Durga Anumolu ◽  
Gowthami Saraf
Keyword(s):  
Quality By Design ◽  
Hplc Method ◽  
Stability Studies ◽  
Analytical Quality

Developing a Validated HPLC Method for Quantification of Ceftazidime Employing Analytical Quality by Design and Monte Carlo Simulations

2021 ◽  
Author(s):  
Ranjot Kaur ◽  
Sumant Saini ◽  
Asha Patel ◽  
Teenu Sharma ◽  
Ripandeep Kaur ◽  
...  
Keyword(s):  
Monte Carlo ◽  
Monte Carlo Simulations ◽  
Flow Rate ◽  
Analytical Method ◽  
Mobile Phase ◽  
Quality By Design ◽  
Hplc Method ◽  
Superior Performance ◽  
Analytical Quality ◽  
Method Performance

Abstract Background Ceftazidime, a third-generation cephalosporin, is widely used in the treatment of lung infections, often given as “off-label” nebulization. There is need for developing a sensitive and robust analytical method to compute aerodynamic properties of ceftazidime following nebulization. Objective The current study entails development of a simple, accurate and sensitive high-performance liquid chromatography method (HPLC) for ceftazidime estimation, employing the principles of analytical quality-by-design (AQbD) and Monte Carlo simulations. Methods Selection of critical material attributes (CMAs) affecting method performance was accomplished by factor screening exercise. Subsequently, the influential CMAs, i.e., mobile phase ratio and flow rate, were systemically optimized using a face-centred cubic design for the chosen critical analytical attributes (CAAs). The factor relationship(s) between CMAs and CAAs was explored employing 3 D-response surface and 2 D-contour plots, followed by numerical as well as graphical optimization, for establishing the optimal chromatographic conditions. The obtained method operable design region was validated by Monte Carlo simulations for defect rate analysis. Results The optimized HPLC conditions for estimating ceftazidime were acetonitrile to acetic acid solution (75:25) as mobile phase at a flow rate of 0.7 mL/min, leading to Rt of 4.5 min and peak tailing ≤ 2. Validation studies, as per ICH Q2(R1) guidance’s, demonstrated high sensitivity, accuracy and efficiency of the developed analytical method with LOD of 0.075 and LOQ of 0.227 µg/mL. Application of this chromatographic method was extrapolated for determining aerodynamic performance by nebulizing ceftazidime at flow rate of 15 L/min using next-generation impactor. The study indicated superior performance, sensitivity and specificity of the developed analytical system for quantifying ceftazidime. Conclusions Application of AQbD approach, coupled with Monte Carlo simulations, aided in developing a robust HPLC method for estimation of ceftazidime per se and on various stages of impactor.

scholarly journals Analytical quality by design approach to RP-HPLC method development and validation for simultaneous estimation of esomeprazole and naproxen in modified-release dosage form

2022 ◽  
Vol 8 (1) ◽  
Author(s):  
Khandokar Farjana Urmi ◽  
Md. Saddam Nawaz ◽  
S. M. Ashraful Islam
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Quality By Design ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Solution Stability ◽  
Modified Release ◽  
Analytical Quality ◽  
Rp Hplc ◽  
Development And Validation

Abstract Background The present work describes the development and validation of a new, specific, accurate, and precise stability-indicating RP-HPLC method for the simultaneous estimation of Esomeprazole (ESP) and Naproxen (NAP) in modified-release bi-layer tablet dosage form. Analytical Quality by Design concept was implemented through the method development exercise to establish the robustness of the method. Results Method development was performed on C18, 250 × 4.6 mm ID, and 5 µm particle size column with 10 µl injection volume using a photodiode array (PDA) detector to monitor the detection at 280 nm. The mobile phase consisted of the buffer: methanol at a ratio of 50: 50 (v/v), and the flow rate was maintained at 1.5 ml/min, and the column oven temperature was maintained at 30 °C. The retention times for NAP and ESP were found 5.9 ± 0.1 and 8.9 ± 0.1 min, respectively. The method was validated in terms of system suitability, specificity, accuracy, linearity, precision, and solution stability. Linearity was observed over the range of concentration 8–12 µg/ml for ESP and 200–300 µg/ml for NAP, and the correlation coefficient (R2) was found excellent > 0.999. The method was specific to ESP and NAP, and the peak purity was found 99.97% for ESP and 100.00% for NAP. The method was precise and had %RSD less than 2. Recovery study for accuracy with placebo was found in the range of 99.63–100.36% for ESP and 99.91–100.43% for NAP. Conclusion This proposed fast, reliable, cost-effective method can be used as a quality control tool for the simultaneous determination of Esomeprazole and Naproxen in routine laboratory analysis. Graphical Abstract

Implementing Analytical Quality by Design (AQbD) Approach for Simultaneous Estimation of Tadalafil and Macitentan by RP-HPLC Method

2021 ◽  
Vol 11 (4) ◽  
pp. 539-552
Author(s):  
Amitkumar J. Vyas ◽  
Dhruvanshi A. Gol ◽  
Ajay I. Patel ◽  
Ashok B. Patel ◽  
Nilesh K. Patel ◽  
...  
Keyword(s):  
Quality By Design ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Analytical Quality ◽  
Rp Hplc

ANALYTICAL QUALITY BY DESIGN APPROACH IN RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF DUVELISIB

2021 ◽  
pp. 99-108
Author(s):  
SRUJANI CH ◽  
ANNAPURNA P ◽  
NATARAJ KS ◽  
KRISHNA MANJARI PAWAR A
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Quality By Design ◽  
Hplc Method ◽  
Design Approach ◽  
Analytical Quality ◽  
Column Temperature ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Quality By Design Approach

Objective: A simple, accurate, and robust RP-HPLC method was developed and validated for the estimation of Duvelisib using analytical quality by design approach. Methods: The critical method parameters (CMP) were systematically optimized using box-Behnken design (BBD). The CMP’s selected were % organic phase composition, column temperature, and flow rate. The critical quality attributes investigated were retention time and theoretical plates. Results: Chromatographic separation was accomplished on Agilent Zorbax Eclipse C18 (150×4.6 mm, 5 μm) column. The optimized and predicted data from Design Expert software consist of mobile phase 0.1 % orthophosphoric acid (46.3%): Acetonitrile (53.7%), pumped at a flow rate of 0.91 ml/min at 32.6°C gave the highest desirability function of 1. The retention time of the drug was found to be 2.85 min. The developed method was validated as per the ICH Q2 (R1) guidelines. Conclusion: Based on the analysis of variance values, the selected models were found to be significant with p<0.05. The results of the validation parameters were within the acceptable limit. The stability of the drug was examined under different stress conditions forcibly and significant degradation was found in acidic condition.

scholarly journals Perspectives in modeling and model validation during analytical quality by design chromatographic method evaluation: a case study

AAPS Open ◽  
2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Yongzhi Dong ◽  
Zhimin Liu ◽  
Charles Li ◽  
Emily Pinter ◽  
Alan Potts ◽  
...  
Keyword(s):  
Quality By Design ◽  
Hplc Method ◽  
Original Method ◽  
Analytical Quality ◽  
Method Evaluation ◽  
Phase Gradient ◽  
Solid Models ◽  
Development And Validation ◽  
And Control

AbstractDesign of experiments (DOE)-based analytical quality by design (AQbD) method evaluation, development, and validation is gaining momentum and has the potential to create robust chromatographic methods through deeper understanding and control of variability. In this paper, a case study is used to explore the pros, cons, and pitfalls of using various chromatographic responses as modeling targets during a DOE-based AQbD approach. The case study involves evaluation of a reverse phase gradient HPLC method by a modified circumscribed central composite (CCC) response surface DOE.Solid models were produced for most responses and their validation was assessed with graphical and numeric statistics as well as chromatographic mechanistic understanding. The five most relevant responses with valid models were selected for multiple responses method optimization and the final optimized method was chosen based on the Method Operable Design Region (MODR). The final method has a much larger MODR than the original method and is thus more robust.This study showcases how to use AQbD to gain deep method understanding and make informed decisions on method suitability. Discoveries and discussions in this case study may contribute to continuous improvement of AQbD chromatography practices in the pharmaceutical industry.

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