scholarly journals Improvement of Development and Validation of an RP-HPLC Method for The Fluvastatin Sodium Using QbD Approach and Its Application to Forced Degradation Studies

2020 ◽  
Vol 11 (4) ◽  
pp. 6938-6948
Author(s):  
Dhamdhere Rupali Balasaheb ◽  
Vijayalakshmi A
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Test Configuration ◽  
Rp Hplc ◽  
Maintenance Time ◽  
Forced Degradation Studies ◽  
Connection Coefficient ◽  
Development And Validation

The current examination portrays the improvement of the QbD way to deal with Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) framework utilizing Design of Experiments.Each of the three principle parts of the RP-HPLC measure (Buffer pH, Organic Step-percent acetonitrile, Organic Modifier-Methanol) are introduced in a successful test configuration zeroed in on methodical exploring. Through measurable investigation devices, for example, Analysis of Variance (ANOVA) and plots that uncovered the last chromatographic states of the strategy, the criticalness and communication impacts of these boundaries on the reaction factors (maintenance time and following component) were assessed. The chromatographic detachment was accomplished on Thermo Hypersil BDS RP C18 (250 × 4.6 mm, 5μ) section utilizing Buffer (pH 6.8): Acetonitrile (60:40v/v) as portable stage and discovery was finished utilizing Photo-Diode Array (PDA) identifier at 288 nm. The created fluvastatin sodium technique is direct with coefficients of relationship over a scope of 10-80μg/ml. The (R2) estimation of the connection coefficient is 0.999. The percent RSD for the strategy's exactness and accuracy was discovered to be under 2 percent. Investigations of Forced Degradation uncovered that the method was found to show security. The outcomes indicated that the strategy proposed is proper for the exact and precise assurance and detailing of fluvastatin sodium in mass.

scholarly journals ESTIMATION OF AMLODIPINE BESYLATE AND IRBESARTAN IN PHARMACEUTICAL FORMULATION BY RP-HPLC WITH FORCED DEGRADATION STUDIES

2019 ◽  
pp. 159-167 ◽  
Author(s):  
T Hemant Kumar ◽  
CH. ASHA ◽  
D. GOWRI SANKAR
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Forced Degradation ◽  
Amlodipine Besylate ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Liquid Chromatographic

Objective: To develop and validate a simple, specific, accurate, precise and sensitive reverse phase high performance liquid chromatographic (RP-HPLC) method with forced degradation studies for the simultaneous estimation of amlodipine besylate and irbesartan in the pharmaceutical formulation. Methods: The chromatographic separation of the two drugs were achieved using Enable C 18G column (250 ×4.6 mm; 5 µm) in isocratic mode with mobile phase consisting of sodium acetate buffer (pH 4.0) and acetonitrile (30:70, % v/v) with a flow rate of 0.6 ml/min. Ultraviolet(UV) detection was carried out at 238 nm. The proposed method was validated for linearity, range, accuracy, precision, robustness, limit of detection (LOD) and limit of quantification (LOQ). The tablet formulation was subjected to stress conditions of degradation including acidic, alkaline, oxidative, thermal and photolysis. Results: The retention time for amlodipine besylate and irbesartan were found to be 5.512 and 6.321 min respectively. Linearity was observed over a concentration range 4-32 µg/ml for amlodipine besylate (r2 =0.9999) and 10-70 µg/ml for Irbesartan (r2 =0.9998). The % relative standard deviation (RSD) for Intraday and Interday precision was found to be 0.436 and 0.699 for amlodipine besylate and 0.435 and 0.30 for irbesartan. Amlodipine besylate shown stability towards acidic and thermal whereas in basic, oxidative and photolytic it shown less stability in which it degraded to more extent. Irbesartan shown stability towards thermal conditions whereas in remaining conditions it degrades to more extent especially in oxidative conditions. Conclusion: The developed reverse phase high performance liquid chromatographic (RP-HPLC) method was also found to be simple, precise and sensitive for the simultaneous determination of amlodipine besylate and irbesartan in the tablet dosage form.

scholarly journals REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION AND FORCED DEGRADATION STUDIES OF EMTRICITABINE, RILPIVIRINE, AND TENOFOVIR ALAFENAMIDE IN SOLID DOSAGE FORM

2019 ◽  
Vol 12 (1) ◽  
pp. 112
Author(s):  
Juluri Krishna Dutta Tejaswi ◽  
Govinda Rajan R
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies ◽  
Tenofovir Alafenamide

Objective: A stability indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the estimation of emtricitabine (EMT), rilpivirine (RIL), and tenofovir alafenamide (TAF) in combined dosage forms and its API.Methods: Chromatographic separation was achieved on Waters ACQUITY RP-HPLC with PDA detector having Zodiac C18 Column (250×4.6×5μ) using mobile phase mixture of phosphate buffer: acetonitrile in the ratio of 40:60 v/v at 262 nm.Results: The assay was performed with tablets, and the % assay was found to be 100.104 for EMT, 99.74 for RIL, and 102.41 for TAF which shows that the method is useful for routine analysis. The linearity was found to be linear with a correlation coefficient of 0.999, which shows that the method is capable of producing good sensitivity. The retention time (RT) of EMT, RIL, and TAF using optimum conditions was found to be 2.517, 3.273, and 6.697 min. Forced degradation studies (FDS) were performed on sample using acid, base, thermal, photolytic, and peroxide degradation.Conclusion: Due to its simplicity, rapidness, high precision, and low RT value, this method was successfully applied to the estimation of EMT, RIL, and TAF combined dosage form. The drugs were found to be stable at FDS, and the net degradation was found to be within the limits.

scholarly journals METHOD DEVELOPMENT AND VALIDATION OF EPROSARTAN MESYLATE AND ITS IMPURITIES USING REVERSE PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2016 ◽  
Vol 8 (4) ◽  
pp. 49 ◽  
Author(s):  
O. S. S. Chandana ◽  
D. Sathis Kumar ◽  
R. Ravichandra Babu
Keyword(s):  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Reverse Phase ◽  
Related Substances ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
The Mean ◽  
Development And Validation

Objective: Our main objective is to develop an accurate and precise RP-HPLC method for the determination of Eprosartan Mesylate and its impurities. Methods: A Develosil ODS UG-5; (150 × 4.6) mm; 5 µm column was used for the Separation of drugs by a mobile phase consisting of Buffer and Acetonitrile mixture in the gradient proportion. The flow rate maintained was 0.8 ml/min and the wavelength used for detection was 235 nm.Results: The linearity was observed in the range of 0.025-50µg/ml of spiked impurities in Eprosartan Mesylate, impurity 1 and impurity 2 with a correlation coefficient of 0.99927, 0.99910 and 0.99934 respectively. The mean percentage recoveries for LOQ, 50%, 80%, 100%, 150% and 200% accuracy were found to be 101.5±1.51, 107.0±1.7, 104.6±0.4, 102.8±0.36, 101.7±0.26 and 101.3±0.15 respectively for impurities in Eprosartan Mesylate, impurity 1 and impurity 2. Linearity, accuracy, precision and robustness parameters for the suggested method were estimated for validation.Conclusion: The developed method is uncomplicated, accurate, sensitive and precise for the determination of related substances in the Eprosartan Mesylate. The satisfying % recoveries and low % RSD Values confirmed the suitability of the developed method for the usual analysis of Eprosartan mesylate in pharmaceuticals.

scholarly journals Reverse-phase High-Performance Liquid Chromatography Method Development and Validation for Estimation of Glimepiride in Bulk and Tablet Dosage Form

2020 ◽  
Vol 11 (02) ◽  
pp. 296-302
Author(s):  
Aseem Kumar ◽  
Anil Kumar Sharma ◽  
Rohit Dutt
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Development And Validation

The present work demonstrates a simple, rapid, precise, specific, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method for analyzing glimepiride in pure and tablet forms. The present method was developed using a C18 column 150 × 4.6 mm, with 5 μm, and packing L1 maintained at a temperature of 30°C. The mobile phase was prepared by dissolving 0.5 gram of monobasic sodium phosphate in 500 mL of distilled water, pH of the solution adjusted to 2.1 to 2.7 with 10% phosphoric acid, and added 500 mL of acetonitrile. The mobile phase was pumped in the highperformance liquid chromatography (HPLC) system at a flow rate of 1 mL/min, and separation was carried out at 228 nm, using an ultraviolet (UV) detector. The chromatographic separation was achieved with peak retention time (RT) at about 9.30 minutes, and the method was found to be linear over a concentration range of 40 to 140 μg/mL. The specificity of the method represented no interference of the excipients during the analysis, and stability testing after 24 hours also showed that the method is suitable and specific. The accuracy was between 99.93 to 99.96%, with limit of detection (LOD) and limit of quantitation (LOQ) being 0.354 μg/mL, 1.18 μg/mL, respectively. Satisfactory results were found for precision and robustness parameters during the development and validation stage for the analytical method. The proposed method was also adopted for the analysis of glimepiride tablets to improve the overall quality control. Using this method, symmetric peak shape was obtained with reasonable retention time. The retention time of glimepiride for six repetitions is 9.3 ± 0.1 minutes; the run time is 21 minutes. The proposed RP-HPLC method is a modification of the United States Pharmacopeia (USP) method, and it was found to be valid for glimepiride within concentration ranges 40 to 140 μg/mL, using C18 analytical columns, and isocratic elution with UV detection, and at 1 mL/min of flow rate.

scholarly journals STABILITY-INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF ROSUVASTATIN CALCIUM IN BULK AND TABLET FORMULATION BY REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 251-256
Author(s):  
SAILAJA B ◽  
SRAVANA KUMARI K
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Tablet Formulation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Development And Validation ◽  
Rosuvastatin Calcium

Objective: The present work was focused on the development and validation of reverse-phase high-performance liquid chromatography (RP-HPLC) method which is simple, rapid, precise, accurate, sensitive, economical, and stability indicating for the quantitation of rosuvastatin calcium in bulk and tablet formulation. Methods: The separation was attained on Waters Symmetry C18 column with dimensions 150×4.6 mm, 5 mm particle size employing 0.1% orthophosphoric acid buffer:acetonitrile in the ratio of 55:45% v/v as mobile phase, which was pumped at a rate of 1.0 ml/min and detected at a wavelength of 241 nm. Results: The linearity of the method was demonstrated in the concentration range of 2–12 μg/ml for rosuvastatin calcium with a correlation coefficient (r2) of 0.999, percentage drug recovery was found to be 100.22–101.16%, and percentage relative standard deviation <2. Limit of detection and limit of quantitation values were found to be 0.013 μg/ml and 0.042 μg/ml, respectively, and assay of marketed tablet formulation was found to be 99.76%. Conclusion: The developed RP-HPLC method was found to be simple, specific, sensitive, rapid, linear, accurate, precise, and economical and could be used for regular quality control of rosuvastatin calcium in bulk and tablet formulation.

scholarly journals REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION AND FORCED DEGRADATION STUDIES OF EMTRICITABINE, RILPIVIRINE, AND TENOFOVIR ALAFENAMIDE IN SOLID DOSAGE FORM

2019 ◽  
Vol 12 (1) ◽  
pp. 112
Author(s):  
Juluri Krishna Dutta Tejaswi ◽  
Govinda Rajan R
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Forced Degradation ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies ◽  
Tenofovir Alafenamide

Objective: A stability indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the estimation of emtricitabine (EMT), rilpivirine (RIL), and tenofovir alafenamide (TAF) in combined dosage forms and its API.Methods: Chromatographic separation was achieved on Waters ACQUITY RP-HPLC with PDA detector having Zodiac C18 Column (250×4.6×5μ) using mobile phase mixture of phosphate buffer: acetonitrile in the ratio of 40:60 v/v at 262 nm.Results: The assay was performed with tablets, and the % assay was found to be 100.104 for EMT, 99.74 for RIL, and 102.41 for TAF which shows that the method is useful for routine analysis. The linearity was found to be linear with a correlation coefficient of 0.999, which shows that the method is capable of producing good sensitivity. The retention time (RT) of EMT, RIL, and TAF using optimum conditions was found to be 2.517, 3.273, and 6.697 min. Forced degradation studies (FDS) were performed on sample using acid, base, thermal, photolytic, and peroxide degradation.Conclusion: Due to its simplicity, rapidness, high precision, and low RT value, this method was successfully applied to the estimation of EMT, RIL, and TAF combined dosage form. The drugs were found to be stable at FDS, and the net degradation was found to be within the limits.

scholarly journals Development and validation of RP-HPLC method for the estimation of omeprazole in bulk and capsule dosage forms

2012 ◽  
Vol 1 (11) ◽  
pp. 366-369 ◽  
Author(s):  
Kalakonda Sri Nataraj ◽  
Mohammad Badrud Duza ◽  
Kalyani Pragallapati ◽  
Dussa Kiran Kumar
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Accurate Method ◽  
Pharmaceutical Journal ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Development And Validation

A method for the determination of omeprazole in bulk and capsule dosage form by reverse phase high performance liquid chromatography has been developed. This is a simple, rapid, precise and an accurate method. The method was developed on a Novapak C18, (250 x 4.6 mm, 5µ) column using phosphate buffer (pH 7.4) and acetonitrile in the ratio of 60:40, v/v as a mobile phase which was pumped at a flow rate of 1.0 ml/min and detection was done at 302 nm. The retention time of the drug was found to be 7.71 min. The method was validated for accuracy, precision, linearity, specificity, robustness. The linearity was observed in the range of 20-60 ppm. The results of recovery studies indicated that the method was accurate. Hence the developed method was found to be suitable for the estimation of omeprazole in bulk and capsule dosage forms.DOI: http://dx.doi.org/10.3329/icpj.v1i11.12062 International Current Pharmaceutical Journal 2012, 1(11): 366-369

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