scholarly journals Development and Validation of HPLC Method for the Quantification of Atorvastatin in Pharmaceutical Dosage Forms and Biological Fluid

2021 ◽  
Vol 11 (2) ◽  
pp. 207
Author(s):  
SK Manirul Haque
Keyword(s):  
Biological Fluid ◽  
Current Method ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Pharmaceutical Industries ◽  
Development And Validation

<p>A<strong> </strong>reverse phase HPLC method was developed for the determination of atorvastatin. The mobile phase involved for the separation was phosphate buffer and acetonitrile with a ratio of 10:1. The HPLC column C<sub>18</sub> ODS hypersil column (250 mm×4.6 mm, 5 μm) was used and detected at 215 nm.   The run time of the current method was 5 minutes with excellent specificity; no interferences were observed in the pharmaceutical dosage form. The process was validated according to ICH guidelines. The linearity of the proposed method was within the range of 0.25–3.8 µg/ml. The LOD and LOQ values were found to be 0.21 and 0.64 µg/ml. The % recovery and %RSD were within the range of 98–100 %, and ±2% for accuracy, precision, robustness, ruggedness results. All the values are acceptable as per ICH guidelines. As well, this enhanced technique was applied to calculate the amount of atorvastatin in human urine samples. Therefore, the present method is reliable for quantifying atorvastatin in quality control samples in academic and pharmaceutical industries and can easily be used in research development and hospitals. </p>

scholarly journals Optimized and Validated RP-HPLC Method for the Determination of Clopidogrel in Bulk and Pharmaceutical Formulation

2016 ◽  
Vol 8 (3) ◽  
pp. 439-446 ◽  
Author(s):  
R. Akter ◽  
S. Banik ◽  
A. Ghosh ◽  
M. M. O. Rashid
Keyword(s):  
Pharmaceutical Preparations ◽  
Current Method ◽  
Hplc Method ◽  
Uv Detector ◽  
Reverse Phase Hplc ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Validation Parameters

This study was undertaken to develop a novel, simple, rapid, accurate and precise sensitive reverse phase HPLC method for estimating Clopidogrel in bulk and pharmaceutical dosage form. The current method in this study was achieved by Thermo Hypersil RP C-18 column (100 mm x 4.6 mm, 3.5 µm) using a mobile phase of Phosphate Buffer: Acetonitrile (pH 3.0) is 70: 30 at a column temperature of 25°C. The effluent was monitored by UV detector at 238 nm. The retention time of Clopidogrel was 4.75 min with a flow rate 1.0 mL/min. Calibration curve was linear in the range of 10-60 µg/mL. The method was validated for linearity, precision, robustness and accuracy as per ICH guidelines. The results of all the validation parameters were well within their acceptance values (%RSD <2.0 specified by the USP, ICH and FDA), which prove applicability of the proposed method for routine analyses and quality-control assay of Clopidogrel in pharmaceutical preparations.

scholarly journals Novel LC Method Development and Validation for Simultaneous Determination of Montelukast and Doxofylline in Bulk and Pharmaceutical Dosage Forms

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Gadapa Nirupa ◽  
A. Siva Kumar ◽  
Upendra M. Tripathi
Keyword(s):  
Simultaneous Determination ◽  
Method Development ◽  
Dosage Forms ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Development And Validation

A novel rapid HPLC method was developed for simultaneous determination of montelukast and doxofylline in bulk and pharmaceutical dosage forms. Development of an analytical method for simultaneous estimation of drugs requires a lot of efforts and of course it is a challenging task. The method was developed by using C18 (150 mm×4.6 mm, 5 μm) column; mobile phase consisting of methanol and phosphate buffer at pH 4.5; the flow rate of 1.0 mL/min and ultraviolet detection at 280 nm. Both drugs were sufficiently resolved having retention time of 4.7 min and 1.9 min for montelukast and doxofylline, respectively. The method was validated as per ICH Guidelines for various parameters like precision, linearity, accuracy, ruggedness, and robustness. The validated method was applied to the commercially available pharmaceutical dosage form and obtained the desired result.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

Stability Indicating RP-HPLC Method Development and Validation for the Determination of Solifenacin Succinate in Bulk and its Pharmaceutical Formulation

2021 ◽  
pp. 3509-3514
Author(s):  
A. Tanuja ◽  
S. Ganapaty ◽  
Varanasi S N Murthy
Keyword(s):  
Method Development ◽  
Current Method ◽  
Hplc Method ◽  
Pharmaceutical Ingredients ◽  
Solifenacin Succinate ◽  
Ich Guidelines ◽  
Degradation Studies ◽  
Hplc Method Development ◽  
Development And Validation

The current work aims to establish a novel and advanced reverse phase isocratic liquid chromatography system followed by validation and to conduct stability analysis in active pharmaceutical ingredients and formulations for the quantification of Solifenacin Succinate. The optimized elution was achieved with column Sunfire C8 (4.6 x 150mm, 5µm), using the mobile phase of Buffer: Methanol: Acetonitrile in the composition ratio of 45:45:10 v/v. The wavelength of detection was selected as 220nm with 1.0ml/ min flow rate and 30μl injection volume. The retention time of Solifenacin Succinate was found 2.94 min respectively. The method developed has been validated for various analytical parameters according to ICH guidelines. The Linearity was attained at 20 to100 μg/ml of concentration range. The established method was proved as reproducible. The Assay was obtained as 100.40%. The degradation studies were carried out at all degradative conditions and the results of degradation studies denote that the current method was specific, reliable, and economical. Hence, the developed method can be applied for the qualitative and quantitative determination of the selected drug and its commercial formulations.

Simple and Sensitive Analytical Method Development and Validation of Nitazoxanide and Ofloxacin by RP- HPLC

2021 ◽  
pp. 84-86
Author(s):  
Abhishek Agrawal ◽  
Prem Kumar Bichala ◽  
Swapna Singh
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Quality Control Laboratory ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation

RP-HPLC method was developed for the determination for the validation of Nitazoxanide and Ofloxacin in pharmaceutical dosage form. Chromatographic separation was performed on Develosil ODS HG-5 RP C18, 15x4.6mm, 5µm column, with mobile phase comprising of mixture of ACN: Methanol: Citric acid in the ratio of 50:45:5 v/v, at the flow rate 1.0ml/min and the detection was carried out at 296nm. The comprehensive forced stress testing has been carried out as per USP guidelines. The drug Nitazoxanide is subjected to synthetic Benzamide, and the drug Ofloxacin is subject to synthetic Fluoroquinolone. RP- HPLC method was developed to separate analyte from all other degradation peaks. The method was successfully validated as per ICH guidelines for the purpose of conducting studies of the analyte in quality control laboratory. The drug was subjected to different degradation conditions; it was found to be stable in all degradation conditions. The purposed HPLC method was found to be precise, specific, accurate, rapid and economical for the determination of Nitazoxanide and Ofloxacin in pharmaceutical dosage form. The sample recoveries in all formulations were in good agreement with their respective label claims and this method can be used for routine analysis. The linearity range was found to be 0-50 (µg/ml) for Nitazoxanide and 0-50 (µg/ml) for Ofloxacin. Calibration curve was plotted and correlation co-efficient for the drugs found to be 0.999 and 0.997. Hence the results obtained were within the limits.

scholarly journals Validated Stability-Indicating RP-HPLC Method for the Determination of Norfloxacin in Pharmaceutical Dosage Form

2021 ◽  
Vol 10 (4) ◽  
Author(s):  
Sirajunisa Talath ◽  
Syeda Humaira
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Relative Standard

The objective of this work was to develop a simple, sensitive, accurate, precise and reproducible high performance liquid chromatography (HPLC) method for the determination of norfloxacin in pharmaceutical dosage forms. Shimadzo Prominance model L20 AD HPLC system equipped with SPD 20A UV-Vis detector was used for the analysis. The separation was done on RESTEX allure C18 column (3 μm, 15 cm × 4.6 mm), for an isocratic elution a mixture of methanol and water (60:40, v/v) mobile phase at a wavelength of 254 nm. The flow rate was 1.0 mL/min. The RP-HPLC method developed for analysis of norfloxacin was validated with respect to specificity, selectivity, linearity, accuracy, precision and robustness as per the ICH guidelines. The retention time of norfloxacin was 7.5 min. The linearity was established over the concentration ranges of 50-350 μg/mL with correlation coefficients ( r2) 0.999.  The percentage accuracy of norfloxacin ranged from 99.76 -101.66%. The relative standard deviation values for intra-day and inter-day precision was lower than 2.0% and the assay result was found to be 100.65 %. Norfloxacin was subjected to stress conditions such as neutral, acidic, alkaline, oxidation and photolysis degradations as per ICH guidelines. The degradation studies revealed that the drug was found to degrade maximum (1.67%) in alkaline degradation conditions and was highly resistant towards neutral, acidic, oxidative and photolytic degradation conditions. Keywords: Norfloxacin, Validation, Stability-indicating, stress degradation, ICH guidelines.  

DETERMINATION OF BIMATOPROST IN BULK AND OPHTHALMIC DOSAGE FORMS: DEVELOPMENT AND VALIDATION OF AN RP-HPLC METHOD

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 49-55
Author(s):  
N. P Ambhore ◽  
◽  
P. M. Dandagi ◽  
A. P. Gadad ◽  
N. H. S. Reddy
Keyword(s):  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Suggested Approach ◽  
Rp Hplc ◽  
System Suitability ◽  
Development And Validation

The main objective of the current study was to develop a simple, accurate, precise and rapid RPHPLC method and subsequent validation using ICH suggested approach for the determination of bimatoprost in bulk and pharmaceutical dosage form. The chromatographic separation of bimatoprost was achieved on a phenomenex C18 column (150 mm × 4.6 mm; 5 μm) using PDA detector at 194 nm. The compound was separated with a mixture of acetonitrile and 0.2% triethylamine (pH 7.0 adjusted with o-phosphoric acid) in the ratio of 50:50 v/v as the optimized mobile phase at the flow rate of 1 mL/min. Chromatogram showed peak of bimatoprost at retention time of 3.8 min. The method was validated for linearity, sensitivity, precision, accuracy, system suitability and robustness. Calibrations were linear over the concentration range of 6.25-100 μg/mL as indicated by correlation coefficient (r2) of 0.999. Developed method can be applicable for routine quantitative determination of bimatoprost in pharmaceutical dosage forms.

scholarly journals Novel Method development and Validation of Bortezomib in Bulk and Pharmaceutical dosage form by RP- HPLC

2019 ◽  
Vol 9 (1) ◽  
pp. 17-21
Author(s):  
Pasupuleti Laxmi Prasanna ◽  
Pedapanga Sandhya ◽  
Pittala Geetha ◽  
Vallapatla M Anuhya
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Wave Length ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Development And Validation

A simple, rapid, precise and accurate RP-HPLC method was developed and validated for the determination of Bortezomib, in bulk and pharmaceutical dosage form. The separation is achieved on RP-HPLC using a PDA detector by incorporation of enpower 2 software with a flow rate of 1.0ml/min using a mixture of Methanol and water (15:85% v/v) as mobile phase. The column used was Hypersil C18 (4.6×150mm, 5µ) at a wave length of 284nm. The retention time of the Bortezomib was 3.515min.. The linearity of the drug was 25-125µg/m and the method precision for the determination of assay was below 2.0% RSD. The proposed method was validated and applied for the estimation of Bortezomib in quality control of bulk and pharmaceutical dosage forms. Keywords: Bortezomib, RP-HPLC, validation.

scholarly journals Development and validation of RP HPLC method for the estimation of Sofosbuvir and related impurity in bulk and pharmaceutical dosage form

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Shiny Ganji ◽  
Satyavati Dhulipala ◽  
Appala Raju Nemala
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Extensive Literature ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Development And Validation

Abstract Background The present work is aimed at development and validation of RP HPLC method which is simple, specific, precise, and accurate for estimation of Sofosbuvir and its process-related impurity in bulk and pharmaceutical dosage forms. Extensive literature survey revealed no method for estimation of the above said. The chromatographic separation was achieved on Agilent Eclipse XDB-C18, 4.6 × 250 mm, 5 μm with mobile phase composed of 0.1% trifluoroacetic acid in 1000 ml of water:acetonitrile (50:50) using an isocratic mode of elution. Detection was made using UV detector at 260.0 nm and LC solution software for analysis of data. The developed method was validated according to ICH guidelines. Results The linearity of calibration curve for Sofosbuvir in concentration range of 160-480 μg/ml was good. The curve was linear for its process related impurity (Phosphoryl) in concentration range of 10-30 μg/ml. There exists a good correlation between peak area and analyte concentration. Retention time for Sofosbuvir was found to be 3.674 min and its impurity was 5.704 min. Relative standard deviation values for Sofosbuvir is 1.741 and its process related impurity is 0.043. LOD for Sofosbuvir and its impurity was found to be 0.01% (0.04 μg) and 0.03% (0.12 μg) respectively. LOQ for Sofosbuvir and its impurity was found to be 0.50% (0.125 μg) and 1.50% (0.375 μg) respectively. Conclusion All the results reveal that the proposed method was found to be highly sensitive, simple, precise, accurate, robust, and fast. Large number of samples can be analyzed in shorter time due to shorter retention times, so it can be successfully applied for routine analysis of Sofosbuvir and related phosphoryl impurity in bulk and pharmaceutical dosage forms.

scholarly journals DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING HPLC METHOD FOR THE DETERMINATION OF NILOTINIB HYDROCHLORIDE IN BULK AND PHARMACEUTICAL DOSAGE FORM

2016 ◽  
Vol 8 (9) ◽  
pp. 41
Author(s):  
Ramu Ivaturi ◽  
T. Manikya Sastry ◽  
S. Satyaveni
Keyword(s):  
Linear Regression Analysis ◽  
Analysis Data ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines

<p><strong>Objective</strong>:<strong> </strong>To develop a rapid, accurate, linear, sensitive and stability indicating RP-HPLC method for the determination of nilotinib in bulk and pharmaceutical dosage forms in the presence of its four related substances.</p><p><strong>Methods</strong>:<strong> </strong>The RP-HPLC method was developed for the chromatographic separation of nilotinib and its impurities by using waters Xterra RP-18 (150*4.6 mm, 3.5 µm) column with a mobile phase combination of 10 mM ammonium formate with pH-3.5 and acetonitrile in gradient mode. An injection volume of 20 µl. Flow rate was 1.0 ml/min and detection was carried a wavelength of 250 nm. The method was validated as per ICH guidelines.</p><p><strong>Results</strong>:<strong> </strong>The retention time for nilotinib and its four impurities were found to be 4.37, 7.40, 8.96, 10.21 and 10.87 min respectively. The linear regression analysis data for the calibration plots showed the good linear relationship in the concentration range of 0.04-3.0 ppm for the nilotinib impurities. The % recovery of nilotinib impurities was found to be 96.8-99.4% in the linearity range. The detection limit (LOD) values were about 0.014, 0.016, 0.005 and 0.03 ppm respectively and the quantification limit (LOQ) values were 0.042, 0.048, 0.014 and 0.09 ppm respectively. The % degradation at various stress conditions like acid, alkaline, oxidative, thermal and photolytic stress was found to be 8.92, 18.35,5.63, 0.88 and 3.89 respectively.</p><p><strong>Conclusion: </strong>The RP-HPLC method compatible with LC-MS was developed for the analysis of nilotinib and its four impurities. It was validated as per the ICH guidelines and found to be linear, robust, precise, accurate, sensitive, stability indicating and can be used for routine as well as stability analysis of capsule dosage forms as well as for drug substance.</p>

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