scholarly journals A review on analytical method development, optimization and validation of combination of Azithromycin and benzoyl peroxide by RP-HPLC using design of experiment as per ICH guideline

2018 ◽  
Vol 6 (02) ◽  
pp. 53-63
Author(s):  
Narendra Singh ◽  
Yogendra Singh ◽  
R. S. Bhadauria ◽  
Jeyabalan Govindasamy
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Degradation Products ◽  
High Specificity ◽  
Cost Effective ◽  
Review Literature ◽  
Phase Selection ◽  
Drug Products ◽  
Selection Of

Pharmaceutical analysis is one of the most challenging fields of analytical chemistry. Pharmaceutical analysts carry out the qualitative and quantitative control of APIs and drug products and also develop and validate appropriate methods. One of my main goals was to develop modern, rapid, precise and reproducible, but also cost-effective HPLC assay methods which are generally available and applicable for most users. The aim of this work was to develop LC methods for both compounds. The assay of erythromycin by LC offers several advantages, such as high specificity, the possibility of determining and quantifying impurities and degradation products, and improved accuracy. The developed methods were validated. My whole work containing following plan of work as Selection of drug, Review Literature, FITR of both drugs and Mixture, Preparation of standard solutions, Preparation of sample of pure drug in Standard solution, Method development by HPLC (as Selection of solvents to be used as diluents and mobile phase, Selection of wavelength, Selection of mobile phase and Selection of chromatographic conditions) Preparation of Mobile phase, Preparation of standard calibration curve combination of drug, Optimization of HPLC condition using box behnken design. Validation of analytical method following parameters as per ICH guidelines. (i). System suitability (ii). Linearity and range (iii). Specificity (iv).Accuracy and precision (v). Limits of detection (LOD) and Quantitation (LOQ). (vi). Selectivity and (vii).Robustness.

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.

scholarly journals COST EFFECTIVE STABILITY INDICATING RAPID, EFFICIENT ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF RELATED SUBSTANCES METHOD FOR SIMULTANEOUS DETERMINATION OF SIMVASTATIN AND EZETIMIBE IN TABLET FORMULATIONS

2021 ◽  
Vol 10 (3) ◽  
pp. 3024-3028
Author(s):  
Srinivasarao Kosanam
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Method Development ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Internal Diameter ◽  
Solution Stability ◽  
Pharmaceutical Dosage Forms ◽  
Validation Parameters

An efficient, cost effective, rapid reverse phase high-performance liquid chromatographic method was developed and validated for the determination of Ezetimibe and Simvastatin in pharmaceutical dosage forms. Chromatography was carried out by using X-terra C18, 150 x 4.6mm, 3.5µ or equivalent internal diameter with a mixture of 0.5 mL glacial acetic acid in 2000 mL water as mobile phase A and Acetonitrile as mobile phase B. Analytical method validation parameters such as specificity, linearity, precision, accuracy, solution stability and robustness, limit of detection (LOD) and limit of quantification (LOQ) was done. The correlation coefficient was found to be linear for each analyte in the desired concentration range. The average recovery was found with range of 96.7 and 107.7 for Ezetimibe and Simvastatin and their respective impurities respectively. The proposed method is highly sensitive, precise and accurate, which was evident from the LOD value range of minimum 0.135 ppm for Ezetimibe and 0.356 ppm for Lovastatin & Epilovastatin for Simvastatin impurities. Hence the present method can be applied successfully for the quantification of finished dosage form in the combined formulations of Ezetimibe and Simvastatin.

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 Ultra performance liquid chromatographic method for simultaneous quantitation of degradation products of telmisartan and hydrochlorothiazide in combination dosage form

2020 ◽  
Vol 11 (2) ◽  
pp. 2070-2082
Author(s):  
Narasimha Reddy G P ◽  
Sreenivasulu Reddy T ◽  
Sidda Reddy K ◽  
Shashi Kumar K N
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Wave Length ◽  
Stability Study ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating

This work is intended to thrive a stability indicating Ultra performance liquid method for the estimation of (TLM) and (HCTZ) and degradation products pharmaceutical dosage forms. Separation was carried out on Zorbax Eclipse XDB C-18(50 x 2.1 mm, 1.7 ) column using a gradient method. Mobile phase A is 10mM KH2PO4 having 1% (v/v) of and mobile phase B is used in this work. 0.5 / minute is the flow of rate and at 271nm noticed wave length is monitored. Method development trails were carried out on six different columns. For specificity, limit of quantification, limit of detection, linearity, accuracy, method precision, robustness and stability this method is validated. Correlation coefficient of the impurities is more than 0.99. Stability indicating method confirmed that there were no interference of all impurities of TLM and HCTZ. Hence, developed LC method was stability indicating and well applied for drug product stability study as well as to quality monitoring.

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 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.

scholarly journals Stability Indicating HPLC Method for the Determination of Delamanid in Pharmaceutical Dosage Form

2021 ◽  
Vol 11 (1-s) ◽  
pp. 108-112
Author(s):  
Advaita B. Patel ◽  
Deepa R. Patel ◽  
Dhaval M. Patel ◽  
Mansi Babaria
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Stress Test ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

Delamanid is successfully used for treatment of MDR TB. A stability indicating analytical method has been developed and validated. In this study Delamanid was degraded under different stress test conditions as per International Conference on Harmonization. The degraded samples were used to develop a stability-indicating high performance liquid chromatographic (HPLC) method for the Delamanid. The Delamanid was well separated from degradation products using a reversed-phase Hypersil BDS C18 (250 mm × 4.6mm i.d., 5µm) column and a mobile phase comprising of 0.01M pH 2.70 Phosphate Buffer: Acetonitrile (pH 3.50) 70:30, pH of mobile phase was adjusted with Glacial acetic acid and other HPLC parameters were flow rate 1 mL/min, detection wavelength 254 nm and injection volume 10 µl. The method was validated for linearity, precision, accuracy, ruggedness and robustness. Results obtained after validation study indicating that the proposed single method allowed analysis of Delamanid in the presence of their degradation products formed under a variety of stress conditions. The developed procedure was also applicable to the determination of stability of the Delamanid in commercial pharmaceutical dosage form. Keywords:  Delamanid, stability indicating analytical method, HPLC

High Performance HPLC-UV Method Development and Validation for Sulfadoxine from its Potential Interfering Impurities

2021 ◽  
Vol 08 ◽  
Author(s):  
Nayan S. Gadhari ◽  
Jayram V. Gholave ◽  
Suyog S. Patil ◽  
Ajay R. Patil ◽  
Kiran F. Shelke ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Degradation Products ◽  
Drug Product ◽  
Ich Guidelines ◽  
Daunting Task ◽  
Method Development And Validation ◽  
The Stability ◽  
Development And Validation

Objective: To address the separation of interfering potential impurities associated with the drug is always a daunting task. We present the method validation and quantitative determination of sulfadoxine (SUL), an anti-malarial drug with most important interfering impurities present pharmaceutical dosages and in bulk samples using HPLC-UV method. Methods: The UV detection was obtained at 270 nm and SUL is separated on Sunfire C18 (25 cm x 4.6 mm x 5 µ m) column at 45°C with flow rate of 1.0 mL/min in a mobile phase (CH3COOH:CH3CN). The stress testing (acidic/basic/oxidative) was performed using HPLC for SUL and its impurities showing the highly efficient separation peaks between degradant and drug product. Results: The developed method was found to be highly accurate and sensitive in regulation with ICH guidelines. Also, it was found to be free from interference from degradation products which allows the stability indicating capability of developed HPLC-UV method for SUL for validation in bulk drugs. Conclusion: The main advantages of the present method; (a) Separation achieved in 30 minutes, (b) MS compatible mobile phase renders this developed method can be directly adapted to LC-MS without any major modifications in near future, and (c) separation of twelve impurities on Sunfire C18 column. The CFs (correction factors) had been calculated for all the impurities. It was found to be 1.6 (IMP IX), 1.70 (IMP XI) and in between 0.8-1.3 for all other impurities. The LOD of the developed method for all the analytes were in the range of 0.05 to 0.11 μg/mL and the LOQ values were in the range of 0.17 to 0.36 μg/mL.

Development and Validation of a Robust HPLC Method for Simultaneous Estimation of 5-Fluorouracil and Resveratrol and Its Application in the Engineered Nanostructured Lipid Carrier

2020 ◽  
Vol 16 ◽  
Author(s):  
Mohammad Kashif Iqubal ◽  
Abid Kamal ◽  
Ashif Iqubal ◽  
Mohammad Imran ◽  
Javed Ali ◽  
...  
Keyword(s):  
Combination Therapy ◽  
Analytical Method ◽  
Analytical Methods ◽  
Mobile Phase ◽  
Cost Effective ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Nanostructured Lipid Carrier ◽  
Development And Validation ◽  
Ich Guideline

Background: 5-fluorouracil and resveratrol are the two most effective anticancer drugs. Combination therapy with these two drugs has shown promising results in cancer. The formulation containing 5-fluorouracil and resveratrol has been prepared, but no analytical method is available in the literature for their simultaneous estimation. However, several analytical methods are there for estimation of either 5-fluorouracil or resveratrol alone. Therefore, the present article is designed for the simultaneous estimation of 5-fluorouracil and resveratrol by HPLC and its application in the quantification of the drugs present in the formulated nanostructured lipid carrier (NLC). Methods: The method was developed using a C18 column (Purospher® STAR RP-18 endcapped (5 µm) Hibar® RT 250- 4.6) with acetonitrile and water as the mobile phase (25:75 v/v) and estimated at 272 nm. The currently developed method was further validated by the ICH guideline Q2 (R1). Combinatorial NLC of 5-fluorouracil and resveratrol was also prepared and characterized. Results: The LOD and LOQ were 8.22 and 24.91 µg mL-1 and 6.58 and 19.93 µg mL-1 , respectively. The precisions was under the acceptable limits of < 2% RSD. The content of 5-fluorouracil and resveratrol in NLC were found to be 65.558±1.343% and 96.326±1.421%, respectively. Conclusion: The findings showed that the developed and validated method was simple, fast, cost-effective and reproducible for the simultaneous estimation of both the drugs in the same formulation.

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