scholarly journals Equivalent Method Development and Cross Validation of Pharmacopoeial Method of Montelukast Sodium

2021 ◽  
pp. 88-106
Author(s):  
. Vaishali ◽  
Sudhanshu Ranjan Swain ◽  
Santosh Kumar Verma
Keyword(s):  
Method Development ◽  
Cross Validation ◽  
Research Work ◽  
Hplc Method ◽  
Main Peak ◽  
Column Temperature ◽  
Related Impurities ◽  
Montelukast Sodium ◽  
Prime Design ◽  
Equivalent Method

The purpose of this exploration research work article is to develop equivalent method and evaluate its equivalency (Cross validation) against pharmacopoeial method of Montelukast sodium for the evaluation and assessment of process related impurities i.e. Methyl MLK impurity in Montelukast sodium by HPLC method and its principles. The method mentioned in European Pharmacopoeia (EP) and United States Pharmacopoeia (USP) does not sufficiently separates impurity C and impurity D , as these impurities elutes under the main peak and the pharmacopoeial methods were also not able to detect the Methyl MLK impurity which is not listed in USP monograph. So our prime design of experiment is to develop of new high-performance liquid chromatographic (HPLC) method which eliminates the drawback of two pharmacopoeial methods and this proposed created strategy is fit for recognition and detection of Methyl MLK impurity and separation of all process related impurities of Montelukast sodium mentioned in EP and USP monographs. An efficient strategy screening and scouting in which various C-18 columns were tried and tested. LUNA C-18 column utilized in RP HPLC mode ended up being the phenomenal decision for the technique streamlining. The proportion of acetonitrile and trifluoroacetic acid (TFA) in water and in the mobile phase, column temperature, flow rate and diluents were considered as basic strategy boundary. The method developed equivalency was checked in terms of Specificity, LOD, Quantitation (LOQ), Precision, Linearity, Relative response factor (RRF), and Accuracy.

scholarly journals Development of a Unified Reversed-Phase HPLC Method for Efficient Determination of EP and USP Process-Related Impurities in Celecoxib Using Analytical Quality by Design Principles

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 809 ◽  
Author(s):  
Tim Tome ◽  
Zdenko Časar ◽  
Aleš Obreza
Keyword(s):  
Quality By Design ◽  
Reversed Phase ◽  
Hplc Method ◽  
Drug Substance ◽  
Main Peak ◽  
Analytical Quality ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Related Impurities

This article presents the development of a reversed-phase (RP) high-performance liquid chromatographic (HPLC) method for determination of process-related impurities in a celecoxib drug substance following Analytical Quality by Design (AQbD) principles. The method from European Pharmacopeia (EP) for celecoxib drug substance does not sufficiently separate celecoxib from its EP impurity B because the system suitability criterion is not achieved (resolution NLT 1.8). The same issue was observed with the proposed method from United States Pharmacopeia (USP) for celecoxib capsules, where EP impurity A elutes under the main peak. A new HPLC method was developed that eliminates the disadvantages of the two pharmacopeial methods and is capable of efficiently separating and determining all seven impurities listed in EP and the proposed USP monographs. The development of a new HPLC method started with method scouting, in which various C18 and phenyl stationary phases were tested. Improved selectivity was obtained only with a chiral stationary phase. An immobilized Chiralpak IA-3 column used in RP mode turned out to be the most appropriate for method optimization. The ratio of acetonitrile in the mobile phase, flow rate, and column temperature were recognized as critical method parameters (CMPs) and were further investigated using a central composite face response-surface design. A multiple linear regression (MLR) method was applied to fit the mathematical models on the experimental data to determine factor–response relationships. The models created show adequate fit and good prediction abilities. The Monte Carlo simulation method was used to establish the design space. The method developed was verified in terms of precision, sensitivity, accuracy, and linearity, and the results showed that the new method is suitable for determination of seven process-related impurities of celecoxib.

HPLC METHOD DEVELOPMENT, VALIDATION, AND FORCED DEGRADATION FOR SIMULTANEOUS ANALYSIS OF OXYCODONE AND NALTREXONEIN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (02) ◽  
pp. 31-38
Author(s):  
R. S. Ch Phani ◽  
◽  
K. R. S. Prasad ◽  
R. M Useni
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Degradation Study ◽  
Ich Guidelines ◽  
Hplc Method Development

A simple, precise and stability-indicating RP-HPLC method was developed for simultaneous quantification of oxycodone (OXCD) and naltrexone (NTRX) in combined dosage form. The developed method was validated with respect to precision, linearity, accuracy, robustness, ruggedness, sensitivity and solution stability. The method was developed with ammonium di hydrogen phosphate buffer (pH 5.0) and acetonitrile in a ratio of 55:45 (v/v) as mobile phase at a flow rate of 1.0 mL/minute over Intersil ODS C18 column (250 mm × 4.6 mm×5μ).The UV detection wavelength was fixed at 235 nm. The column temperature was maintained at ambient temperature. The method showed good linearity with correlation coefficient values of 0.9990 and 0.9994 for OXCD and NTRX. The percent recoveries of the two drugs found within the limits of 98.0–102.0%. The LOQ concentrations of OXCD and NTRX are 0.625 μg/ mL and 0.075 μg/mL, respectively. The LOD concentrations of OXCD and NTRX are 0.3125 μg/mL and 0.0375 μg/mL, respectively. According to ICH guidelines forced degradation study was validated.

LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION OF RELATED IMPURITIES OF LURASIDONE AND ITS FORMULATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (09) ◽  
pp. 41-48
Author(s):  
R. N Kachave ◽  
◽  
P. B. Mandlik ◽  
S. R. Nisal
Keyword(s):  
Method Development ◽  
Gradient Elution ◽  
Hplc Method ◽  
Chromatography Method ◽  
Related Impurities ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Liquid Chromatography Method ◽  
The Stability ◽  
Development And Validation

An RP-HPLC method was developed for the quantification of related impurities of lurasidone and its formulation. The chromatographic separation employs gradient elution using an Inertsil ODS C18 (150x4.6) mm, 5μm columns. Mobile phase consisting of solvent A-buffer (pH 3.0): methanol (90:10 %v/v) and solvent B-acetonitrile: water (80:20 % v/v) delivered at a flow rate of 1.0 mL/min. The analytes were detected and quantified at 210 nm using PDA. The method was validated as per ICH guidelines, demonstrating to be a simple, precise, selective, linear and accurate within the corresponding range of impurities of lurasidone. Linearity was observed in the concentration range of 2-6 µg/mL. The RT for Lurasidone was about 18.5 min and three known impurities at RRT about 0.15, 0.21 and 0.36. The specificity of the method was investigated under different stress conditions including hydrolytic, oxidative, photolytic and thermal as recommended by ICH guidelines. Relevant degradation was found to take place under oxidative conditions. Degradation impurities did not interfere with the RT of drug. The peak purity obtained with the aid of PDA detection and satisfactory resolution between related impurities established the specificity of the determination. All these results provide the stability indicating capability of the method.

Method Development and Validation for Related Impurities of Efavirenz by RP-HPLC Method

2017 ◽  
Vol 7 (5) ◽  
pp. 737-747
Author(s):  
Desaraju Bhargavi ◽  
Bhukya Babu Rao ◽  
Gangarapu Kiran ◽  
Thumma Gouthami ◽  
Vasudha Bakshi
Keyword(s):  
Method Development ◽  
Hplc Method ◽  
Related Impurities ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Development And Validation

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Lansoprazole in Presence of Related Substances by QbD Approach

2021 ◽  
pp. 138-150
Author(s):  
Sachin B. Gholve ◽  
Jaiprakash N. Sangshetti ◽  
Omprakash G. Bhusnure ◽  
Ram S. Sakhare ◽  
Pratap H. Bhosale ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Drug Substance ◽  
Gastric Ulcers ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Rp Hplc

A rapid specific RP-HPLC method has been developed for the determination of Lansoprazole impurities in the drug substance. The control of pharmaceutical impurities is currently a critical issue in the pharmaceutical industry. The International Council for Harmonization (ICH) has formulated a workable guideline regarding the control of impurities. The objective of the recent study was to develop and validate a HPLC method for the quantitative determination of process-related impurities of Lansoprazole in pharmaceutical drug substance. Lansoprazole, 2-[[[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridinyl] methyl]-sulfinyl]- 1H-benzimidazole is an proton pump inhibitor used in the management of gastric ulcers. Chromatographic identification of the impurities was carried out by response surface methodology, applying a three-level Box Behnken design with three center points. Three factors selected were a mobile phase, flow rate, column temperature. Evaluation of the main factor, their interaction, and the quadric effect on peak resolution were done on Waters Symmetry C8, 250 x 4.6mm, 5µm column is used for the development of the method. The mobile phase consists of buffer and acetonitrile. The flow rate of the mobile phase was 1.0 ml/min with gradient elution. The column temperature is ambient and the detection wavelength is 235 nm. The injection volume was 10 µL. The method was validated as per ICH guidelines for linearity in the range of 50-150 µg/ml and the LOD & LOQ values obtained were 0.437×10-4 and 0.1325×10-3 µg/ml respectively which specifies the method's sensitivity. The proposed method was successfully used to determine the Lansoprazole impurities in drug substances.

scholarly journals Reverse Phase-High Performance Liquid Chromatography method development and validation for estimation of efavirenz by Quality by Design approach

2019 ◽  
Vol 9 (1-s) ◽  
pp. 319-330
Author(s):  
Santosh A Waghmare ◽  
Arun M Kashid
Keyword(s):  
High Performance ◽  
Method Development ◽  
Quality By Design ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Design Approach ◽  
Main Peak ◽  
Chromatography Method ◽  
Design Expert ◽  
Quality By Design Approach

Quality by design (QbD) refers to the achievement of certain predictable quality with desired and predetermined specifications. A very useful component of the QbD is the understanding of factors and their interaction effects by a desired set of experiments by using software (design expert 8). The present study describes the development of a comprehensive science and risk based HPLC method which is given by design expert 8 and subsequent validation for the analysis of Efavirenz active pharmaceutical ingredient (API) using a quality by design approach. An efficient experimental design based on systematic scouting of all four key components of the RP‐HPLC method (column, pH, mobile phase and flow rate) is presented. The described method was linear. R2=0.9998. The precision, ruggedness and robustness values were also within the prescribed limits (<1% for system precision and <2% for other parameters). Chromatographic peak purity results indicated the absence of co‐eluting peaks with the main peak of Efavirenz. The proposed method can be used for routine analysis of Efavirenz in quality control laboratories. Keywords: Quality by design, HPLC, Efavirenz, design expert 8.

scholarly journals Development and validation of stability-indicating RP-HPLC method for estimation of dalfampridine in bulk drug and tablet dosage form

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Dipali Bagal ◽  
Akhil Nagar ◽  
Aditya Joshi ◽  
Aishwarya Chachare ◽  
Atul Shirkhedkar ◽  
...  
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Stability Study ◽  
Main Peak ◽  
Forced Degradation ◽  
Column Temperature ◽  
Limit Of Quantitation ◽  
Bulk Drug ◽  
Tablet Dosage

Abstract Background In the current study, a simple, improved, precise, rapid, and accurate reverse phase liquid chromatographic method was produced for the estimation of dalfampridine in bulk and tablet dosage form which is a potassium channel blocker used for the treatment of multiple sclerosis (MS). The separation of dalfampridine was achieved isocratically on a C18 column (250 × 4.6 mm, 5 μm) using (0.1% v/v) buffer pH 3.0 ± 0.05 adjusted with diluted orthophosphoric acid (OPA) and acetonitrile (ACN) in the ratio of 60:40% (v/v) as a mobile phase, at a flow rate of 0.5 mL/min, and column temperature of 40 °C. HPLC grade methanol as diluents was used. Five microliters of the standard solution of the drug was injected, and the eluted analytes were detected at 262 nm. Results Dalfampridine was eluted at 4.5 min with a run time of 10 min. Linearity in the method was measured in the concentration range of 25–75 ppm with a correlation coefficient of 0.999. Limit of detection and limit of quantitation were found to be 0.711 μg/mL and 2.154 μg/mL, respectively. Dalfampridine was subjected for forced degradation stability study in conditions of thermal, acid, alkali, and oxidation and photo-degradation condition. The degradants were well resolved from the dalfampridine main peak. Validation of the developed method is carried as per USFDA and ICH guidelines. Conclusion The results of the analysis prove that the method is simple, improved, precise, accurate, and rapid for estimating the content of dalfampridine in bulk drug and tablet dosage form and can be applied for routine analysis.

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