scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF ENTECAVIR IN BULK AND PHARMACEUTICAL DOSAGE FORMS BY RP-HPLC

2017 ◽  
pp. 107-111
Author(s):  
Swathi P. ◽  
S. Vidyadhara ◽  
R. L. C. Sasidhar ◽  
K. Kalyan Chakravarthi
Keyword(s):  
Flow Rate ◽  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Degradation Studies

Objective: The objective and purpose of the analysis have sensibly assessed by selecting of a rapid and sensitive RP-HPLC method for Entecavir in bulk and pharmaceutical dosage form by using the most commonly employed C-18column with UV detection.Methods: In estimation by RP-HPLC method Agilent 1120 compact LC system with variable programmable UV detector and Rheodyne injector with 20 µl fixed loop was used for the chromatographic separation. The mode of operation was isocratic with the components of a solution consisting of methanol: acetonitrile(70:30v/v) and triethanolamine (2-4drops)at the flow rate of 1.2 ml/min and run time was 10 min. Forced degradation studies were conducted to evaluate the stability and specificity of the method along with the validation parameters.Results: Validation parameters of HPLC were found at a detection wavelength of 255 nm. Linearity was observed with the concentration range (Beer’s law range) 20-100µg/ml with R2=0.9991. Robustness with detection wavelengths 253 and 257 nm with a flow rate of 1 ml/min and 1.4 ml/min showed good results. The retention time of the drug was 2.64 min and assay showed 98.1%.Conclusion: The proposed RP-HPLC method was validated as per the ICH Q2B Guidelines, and was found to be applicable for routine quantitative analysis of Entecavir by RP-HPLC using UV detector in pharmaceutical dosage forms. The results of linearity, precision, accuracy and specificity, were proved, that does not exceed certain specified limits. The method provides selective quantification with no interference from other formulation excipients. The proposed method was highly sensitive, reproducible, reliable, robust and specific. Therefore, this method is a simple, rapid analysis may actually be more desirable than a more complicated and time-consuming process. The degradation studies at various stress conditions like thermal and hydrolytic, drug gets degraded at a temperature of 80 °c and refluxing with water at 70 °c for 24hours. 

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 RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

scholarly journals SIMULTANEOUS ESTIMATION, VALIDATION, AND FORCED DEGRADATION STUDIES OF BETAHISTINE DIHYDROCHLORIDE AND DOMPERIDONE IN A PHARMACEUTICAL DOSAGE FORM USING RP-HPLC METHOD

2018 ◽  
Vol 11 (10) ◽  
pp. 125
Author(s):  
Vaishali Mistry ◽  
Rohan Mishra
Keyword(s):  
Hplc Method ◽  
Base Hydrolysis ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Betahistine Dihydrochloride ◽  
The Stability

Objective: This study describes the stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of betahistine dihydrochloride and domperidone in pharmaceutical dosage forms.Methods: The proposed RP-HPLC method was developed using Shimadzu Prominence-i LC-2030 HPLC system equipped with UV detector and chromatographic operation was carried on Shim-pack C18 (250 mm×4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 10 min. The mobile phase consisted of methanol and water in the ratio of 80:20% v/v and eluents were scanned using a UV detector at 244 nm.Results: The retention time of betahistine dihydrochloride and domperidone was found to be 2.3 and 3.6 min, respectively. A linearity response was observed in the concentration range of 9.6 μg/ml–22.4 μg/ml for betahistine dihydrochloride and 6–14 μg/ml for domperidone, respectively. Limit of detection and limit of quantification for betahistine dihydrochloride were 0.52 μg/ml and 1.58 μg/ml and for domperidone are 0.64 μg/ml and 1.94 μg/ml, respectively.Conclusion: The stability-indicating method was developed by subjecting drugs to stress conditions such as acid and base hydrolysis, oxidation, photo and thermal degradation, and degraded products formed were resolved successfully from samples.

scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for the Estimation of Cinacalcet Hydrochloride in Bulk and Their Formulations

2020 ◽  
Vol 10 (6) ◽  
pp. 6610-6618
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Cinacalcet Hydrochloride ◽  
Development And Validation ◽  
Tablet Dosage

A Simple, selective, accurate, precise, linear, and stability-indicating RP-HPLC method was developed and validated for the estimation of Cinacalcet hydrochloride in bulk and tablet dosage forms. Chromatographic separation was achieved on X-Terra Symmetry C18 (4.6 x 150mm; 5 m) with mobile phase containing Phosphate buffer: Acetonitrile (40:60 v/v) pH adjusted to 3.0 ±0.05 with diluted ortho-phosphoric acid. The flow rate was maintained at 0.9 mL/min. The eluent was monitored at 282 nm. Moreover, the retention time of Cinacalcet was 2.8 minutes. The method was validated for linearity, accuracy, precision, and robustness as per ICH guidelines. The developed method was found linear between 25-150 μg/ml, and the linear regression coefficient was 0.999. The % RSD values are less than 2 % indicating the accuracy and precision of the method. The percentage of recovery was obtained from 98-102%. The system suitability parameters were found to be within the limit. Forced degradation studies were conducted under various conditions. The proposed method is simple, rapid, precise, and accurate. It can be used for the quantitation of Cinacalcet hydrochloride in bulk and commercial pharmaceutical dosage forms.

scholarly journals HPLC METHOD FOR SIMULTANEOUS DETERMINATION OF METFORMIN AND SITAGLIPTIN IN PHARMACEUTICAL DOSAGE FORMS AND ITS APPLICATIONS TO DISSOLUTION STUDY

2019 ◽  
Vol 3 (7) ◽  
Author(s):  
Hemraj Sharma ◽  
Boya Madhuri ◽  
Yiragamreddy Padmanabha Reddy ◽  
Kondareddy Vinod Kumar ◽  
Nanda Kishor Bhatta ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detector ◽  
Pharmaceutical Dosage Forms ◽  
Dissolution Study ◽  
Rp Hplc

A novel approach was used to develop and validate a rapid, specific, accurate and precise Reverse phase High performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of Metformin and Sitagliptin in pharmaceutical dosage forms and its applications to dissolution study. The chromatographic separation was carried out on a C8 (250mm X 4.6 mm i.d., 5μm) column with a mobile phase of 40 Acetonitrile: 60 Phosphate Buffer (pH 6.8), using UV detector at 257 nm at 1ml min-1 flow rate. The retention time for Metformin was 2.11 minutes and 5.30 minutes for Sitagliptin. The Linearity for Metformin was found to be 10-80 µg ml-1 with R2 value of 0.9998 and for Sitagliptin 1-8 µg ml-1 with R2 value of 0.9976. Dissolution study of both for Metformin and Sitagliptin was carried, Percentage of drug release was established which was found to be 96.23% and 102.64% respectively, in the period of 50 minutes. Keywords: RP-HPLC, Metformin, Sitagliptin, Dissolution study

DEVELOPMENT AND VALIDATION OF NEW RP-HPLC METHOD FOR QUANTITATIVE ESTIMATION OF VITAMIN-D3 IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (06) ◽  
pp. 40-45
Author(s):  
T Mohan ◽  
◽  
S Prabhakara ◽  
K Anbazhagan ◽  
Krishnan Pavithra ◽  
...  
Keyword(s):  
Vitamin D3 ◽  
Dosage Form ◽  
Quantitative Estimation ◽  
Hplc Method ◽  
Control Analysis ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Bulk Drug

An accurate, simple, rapid, sensitive and cost effective method for the determination of Vitamin-D3 in pharmaceutical dosage form was developed and validated by RP-HPLC method. Chromatographic separation was achieved on phenomenex C18 column (150 mm X 4.6 mm, 5μm) using methanol: acetonitrile: water (90:5:5 V/V/V) as mobile phase, at a flow rate of 1.5 mL/min. The retention time of Vitamin-D3 was found to be 8.3 minutes; the detection was monitored at 265 nm by using UV detector. The developed method was validated according to International Conference on Harmonization (ICH) guidelines. The linearity of Vitamin-D3 was in the range of 2.50 ppm to 6.00 ppm. This method showed an excellent linear response with the correlation coefficient (R2) value of 0.999 for the Vitamin-D3. The recovery of the drug ranged from 99.59% to 103.83% with an average of 101.34%. The percentage RSD was found to be less than two, indicating high degree of accuracy and precision of the proposed RPHPLC method. Due to simplicity, cost effectiveness, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis of Vitamin-D3 in bulk drug and pharmaceutical dosage forms.

DEVELOPMENT AND VALIDATION OF AN IMPROVED STABILITY-INDICATING RP-HPLC METHOD FOR THE ESTIMATION OF TROXIPIDE IN BULK AND TABLET DOSAGE FORMS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (07) ◽  
pp. 18-22
Author(s):  
D. Gowrisankar ◽  
◽  
N.M Rao
Keyword(s):  
Degradation Products ◽  
Thermal Conditions ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Improved Stability ◽  
Degradation Studies ◽  
Tablet Dosage

An improved stability-indicating RP-HPLC method was developed for the estimation of troxipide in bulk and tablet dosage forms. Chromatographic separation of troxipide from its degradation products was achieved on Agilent Zorbax SB-CN (150 × 4.6 mm, 3.5 μm) using sodium phosphate buffer (pH was adjusted to 4.0 ±0.05) and acetonitrile in the ratio of 40:60 V/V, at a flow rate of 0.8 mL/min. This system was found to give compact peak for troxipide at 2.1±0.2 min. The detection was monitored at 260 nm. The linear regression data for the calibration plots showed good relationship with r2 = 0.99 ± 0.001. The method was validated for precision, linearity, accuracy and robustness according to International Conference on Harmonization (ICH) guidelines. The percentage RSD was found to be less than two, indicating high degree of accuracy and precision of the proposed RP-HPLC method. The drug was subjected to stress degradation studies under acidic, basic, oxidative and thermal conditions. The degradation studies reveal that purity angle was less than the purity threshold, so the peak was said to be pure. It means that products resulting from stress studies did not interfere with the detection of troxipide and the assay can thus be considered as stability-indicating. Due to its simplicity, rapidness, high precision and accuracy, the proposed HPLC method may be used for determining troxipide in bulk and in pharmaceutical dosage forms.

scholarly journals Development and Validation of a Simple RP-HPLC Method for Determination of Naproxen in Pharmaceutical Dosage Forms

2015 ◽  
Vol 16 (2) ◽  
pp. 137-141 ◽  
Author(s):  
Saleha Tanjin ◽  
Farhana Islam ◽  
Md Zakir Sultan ◽  
Asma Rahman ◽  
Sharmin Reza Chowdhury ◽  
...  
Keyword(s):  
High Performance ◽  
Pharmaceutical Formulations ◽  
Pharmaceutical Journal ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detector ◽  
Allowable Limit ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A simple, sensitive and precise reversed phase high performance liquid chromatographic (RP-HPLC) method has been developed for the estimation of naproxen in pharmaceutical dosage forms. The method was developed using the mobile phase comprising of dibasic sodium phosphate buffer (Na2HPO4) at pH 7.80 (adjusted by sodium hydroxide) and acetonitrile in the ratio of 70:30 (v/v) over C-18 column (250 x 4.6 mm, 5?m, Phenomenex Inc.) at ambient temperature. The flow rate was at 0.7 ml/min and the column washing was monitored by UV detector at 225 nm. The retention time of naproxen was 4.8 ± 0.1 min. The recovery was found to be >97% which is demonstrative of accuracy of the protocol. Inter-day and intra-day precision of the newly developed method were less than the maximum allowable limit (RSD% ? 2.0) according to ICH, USP and FDA guidelines. The method showed linear response with correlation coefficient (r2) value of 0.9991. Therefore, the method was found to be accurate, reproducible, sensitive and less time consuming and can be successfully applied for routine analysis of naproxen in pharmaceutical formulations. DOI: http://dx.doi.org/10.3329/bpj.v16i2.22295 Bangladesh Pharmaceutical Journal 16(2): 137-141, 2013

Stability Indicating RP-HPLC Method Development and Validation for Estimation of Diroximel Fumarate in bulk and its dosage forms

2021 ◽  
pp. 2603-2607
Author(s):  
Ramachandrapuram Kiranjyothi ◽  
Mahalingam Balakrishnan ◽  
Kothapalli Bannoth Chandrasekhar
Keyword(s):  
Method Development ◽  
Research Work ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Hplc Method Development

Aim and objective: The aim of present research work is to develop validated RP-HPLC stability indicating method for the quantification of Diroximel Fumarate in bulk and its pharmaceutical dosage forms. Materials and methods: Chromatographic method was carried on C18 column (Waters 250mm x 4.6mm, 5m). Mobile phase was prepared by mixing water: Acetonitrile: 85% OPA: in the ratio of 70:30. The flow rate was 0.1 mL/min and the injection volume was 20μL. The absorbance maxima of Diroximel Fumarate was measured at 215nm. The retention time was found to be 2.390 min. Result: The method was proved to be specific and linear in the range of 50-150μg/mL with correlation coefficient of 0.999. The % RSD for precision was found to be less than 2% and the mean percentage recovery was 100.15%. All the validation parameters were statistically validated according to ICH guidelines and were found to be within acceptance criteria. Conclusion: The developed method was simple, specific, precise, accurate and robust. The described HPLC method can be successfully employed for the analysis of Diroximel Fumarate.

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.

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