scholarly journals Quality-by-Design Is a Tool for Quality Assurance in the Assessment of Enantioseparation of a Model Active Pharmaceutical Ingredient

2020 ◽  
Vol 13 (11) ◽  
pp. 364
Author(s):  
Dina Aboushady ◽  
Maria Kristina Parr ◽  
Rasha S. Hanafi
Keyword(s):  
Quality Assurance ◽  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Quality By Design ◽  
Active Pharmaceutical Ingredient ◽  
Binding Interaction ◽  
Mobile Phase Additives ◽  
Central Composite Designs ◽  
Chiral Mobile Phase Additives

The design of experiments (DoE) is one of the quality-by-design tools valued in analytical method development, not only for cost reduction and time effectiveness, but also for enabling analytical method control and understanding via a systematic workflow, leading to analytical methods with built-in quality. This work aimed at using DoE to enhance method understanding for a developed UHPLC enantioseparation of terbutaline (TER), a model chiral drug, and to define quality assurance parameters associated with using chiral mobile phase additives (CMPA). Within a response surface methodology workflow, the effect of different factors on both chiral resolution and retention was screened and optimized using Plackett-Burman and central composite designs, respectively, followed by multivariate mathematical modeling. This study was able to delimit method robustness and elucidate enantiorecognition mechanisms involved in interactions of TER with the chiral modifiers. Among many CMPAs, successful TER enantioresolution was achieved using hydroxypropyl β-cyclodextrin (HP-β-CD) added to the mobile phase as 5.4 mM HP-β-CD in 52.25 mM ammonium acetate. Yet, limited method robustness was observed upon switching between the different tested CMPA, concluding that quality can only be assured with specific minimal pre-run conditioning time with the CMPA, namely 16-column volume (60 min at 0.1 mL/min). For enantiorecognition understanding, computational molecular modeling revealed hydrogen bonding as the main binding interaction, in addition to dipole-dipole inside the CD cavity for the R enantiomer, while the S enantiomer was less interactive.

ANALYTICAL METHOD DEVELOPMENT AND ITS VALIDATION FOR EVALUATION OF POLYHERBAL FORMULATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (10) ◽  
pp. 66-68
Author(s):  
◽  
A. P Jadhav
Keyword(s):  
Immune Response ◽  
Ethyl Acetate ◽  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Simultaneous Estimation ◽  
Active Constituents ◽  
Polyherbal Formulation ◽  
Marker Compounds ◽  
Hptlc Method

Talekt capsule is a branded polyherbal formulation used for enhancing the immune response to dermal infections and also for treating skin disorders. Curcumin and embelin, which are the active constituents of Haridra and Vidanga, respectively were used as marker compounds for developing a simple, accurate, precise and robust HPTLC method for simultaneous estimation. The mobile phase of toluene: ethyl acetate: formic acid (6.5: 3: 0.2 v/v/v) was used for separation. 381nm was used as wavelength for analysis. The Rf value obtained for curcumin, and embelin was found to be 0.51 ± 0.2 and 0.33 ± 0.2, respectively. The developed method was validated on the basis of ICH Q2 (R1) guidelines.

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.

STABILITY INDICATING LIQUID CHROMATOGRAPHIC ASSESSMENT OF DOLUTEGRAVIR BY AQBD APPROACH – CENTRAL COMPOSITE DESIGN

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (10) ◽  
pp. 44-51
Author(s):  
G. Sunitha ◽  
◽  
P. D Anumolu ◽  
C.V.S Subrahmanyam ◽  
G Mounika ◽  
...  
Keyword(s):  
Flow Rate ◽  
Analytical Method ◽  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Values ◽  
Mass Spectral ◽  
Theoretical Plates

Based on the current regulatory requirements for analytical method development, a RP-HPLC method for quality control of dolutegravir in dosage form has been optimized using analytical quality by design (AQbD) approach. Experimental observations were analysed by full factorial experimental design in Sigmatech software with two variables (flow rate and % organic mobile phase) whilst the number of theoretical plates was considered as response. The analytical method conditions were optimized as mobile phase (40:60 % V/V) consisting of acetonitrile and ammonium formate buffer, pH 3.0 pumped at a flow rate of 0.6 mL/min in an isocratic mode on SPOLAR C18 Column (250 x 4.6mm, 5μm) with run time of 15 min. The plot between peak area vs. concentration was rectilinear in the range of 5-30 μg/mL with detection and quantification limit values at 0.01 and 0.3μg/mL, respectively at retention time of 13 min. The predicted data from contour diagram for theoretical plates was verified virtually and it was contented with concrete experimental data. The method was validated as per ICH guidelines. The proposed method was pertinent for assay of marketed dosage form (Tivicay) and further extended to quantify the drug in prevalence of degradation products. Degradation pathways of dolutegravir were postulated and characterized by IR and mass spectral data.

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF PERINDOPRIL ERBUMINE AND AMLODIPINE BESYLATE IN BULK AND TABLET DOSAGE FORM BY HPLC

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 32-35
Author(s):  
S. R Pattan ◽  
◽  
A.C Patni ◽  
R.A Mali ◽  
C.J. Patni ◽  
...  
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Amlodipine Besylate ◽  
Perindopril Erbumine ◽  
Relative Standard ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

The objective of this present work was to develop and validate analytical method for quantitative determination of perindopril erbumine and amlodipine besylate in bulk as well as in tablet formulation. The chromatographic separation of the two drugs was achieved on a Varian Microsorb-MV 100-5 C18 column (150×4.6mm, 10 μm). The mobile phase constituted of acetonitrile: buffer (65:35) and pH adjusted to 2.6 with ortho- phosphoric Acid was delivered at the flow rate 1mL/min. Detection was performed at 210 nm. Separation was completed within 6 min calibration curves were linear with correlation coefficient between 0.99 to 1.0 over the concentration range of 2.5 to 15 µg/mL of perindopril erbumine and 10 to 60 µg/mL of amlodipine besylate The relative standard deviation (R.S.D.) was found <2.3%. The proposed method is precise, accurate, selective and rapid for the simultaneous determination of perindopril erbumine and amlodipine besylate.

A REVIEW ON METHOD DEVELOPMENT AND VALIDATION BY USING HPLC

2021 ◽  
pp. 34-37
Author(s):  
Dipali S. Doifode ◽  
Shailesh G. Jawarkar ◽  
Monika P. Jadhao ◽  
Manali M. Bode
Keyword(s):  
Quality Assurance ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Science Research ◽  
Hplc Method ◽  
Pharmaceutical Drugs ◽  
Method Development And Validation ◽  
Development And Validation

Analytical method development and validation are the continuous and inter-dependent task associated with the research and development, quality control and quality assurance departments. High performance liquid chromatography (HPLC) has been widely used for years as an analytical method and is a key tool for the separation and analysis of pharmaceutical drugs, for drug monitoring and for quality assurance and life science research. Most of the drugs in multi component dosage forms can be analysed by HPLC method because of the several advantages like rapidity, specicity, accuracy, precision and ease of automation in this method. HPLC methods development and validation play important roles in new discovery, development, manufacture of pharmaceutical drugs and various other studies related to humans and animals. This review gives information regarding principle, types, instrumentation and along with various application of the method and Validation of HPLC method as per ICH Guidelines covers all the performance characteristics of validation, like Accuracy, precision, specicity, linearity, range and limit of detection, limit of quantication, robustness

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