scholarly journals Quantification of Pimavanserin in Bulk and Tablet Dosage Form Using A Stability Indicating High Performance Liquid Chromatographic Method

2018 ◽  
Vol 24 (4) ◽  
pp. 291-297 ◽  
Author(s):  
Geetha Bhavani Koduri ◽  
Hari Babu Bollikolla ◽  
Ramachandran Dittakavi ◽  
Srinivasu Navuluri
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Degradation Products ◽  
Antipsychotic Agent ◽  
Hplc Method ◽  
Array Detector ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Tablet Dosage

Background: Pimavanserin, an antipsychotic agent, is used to treat patients suffering with Parkinson's disease. Till now no stability indicating reverse phase HPLC method was reported for the quantification of pimavanserin in bulk and tablet dosage form. Hence in the present study, a new sensitive, precise and accurate stability indicating reverse phase HPLC method with photodiode array detector has been developed for the quantification of pimavanserin in bulk and tablet dosage form. Methods: Separation and analysis of pimavanserin was achieved on Kromasil C18 (5 µm, 250 mm × 4.6 mm) column using 0.1M NaH2PO4, methanol and acetonitrile in ratio of 55:30:15 (v/v/v) as mobile phase at 25°C. The flow rate was 1.0 ml/min. The effluents were monitored with detector set at 239 nm. The method validation was done with regard to the guidelines by the International Conference on Harmonization. Pimavanserin was subjected to acid, alkali and neutral hydrolysis, hydrogen peroxide oxidation, thermal degradation, and photo (sunlight) degradation. Results: Linear relationship was obtained between the concentration of drug and peak area response in the range of 4.25-34.0 µg/ml. The limits of detection and quantitation were found to be 0.027 µg/ml and 0.089 µg/ml, respectively. All the validation characteristics were within the acceptance criteria. The peaks of degradation products were well resolved from the pimavanserin peak. Conclusion: The developed and validated method is able to quantify the pimavanserin in the presence of degradation products.

scholarly journals Development and Validation of Reverse Phase HPLC Method for Simultaneous Estimation of Allopurinol and Lesinurad in its API and Pharmaceutical Dosage Form

2019 ◽  
Vol 4 (04) ◽  
pp. 50-57
Author(s):  
Sayma Khader ◽  
Ayesha Begum K ◽  
D. Ramakrishna
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Development And Validation ◽  
Tablet Dosage

A new, reliable, and validated reverse phase-high-performance liquid chromatography (HPLC) method was developed to quantify the amount of allopurinol and lesinurad simultaneously in solid (tablet) dosage form. A clear chromatographic division was attained on inertsil ODS (4.6 x 250 mm, 5 mm) column, and a mixture of 0.1% trifluoroacetic acid and methanol in the ratio of 40:60 v/v was used as mobile phase. The rate of flow was set at 1 mL/min, and UV detection was achieved at λmax of 255 nm. Injection volume was set to 20 μL. The correlation coefficient of 0.999 was established, and the accurateness was found to be 100.69 and 100.49 for both the drugs, respectively. Therefore, the developed method was simple, specific, precise, and stable. Hence, the method can be employed to estimate the said drugs in other pharmaceutical formulations.

REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR DETERMINATION OF REGORAFENIB IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 63-68
Author(s):  
R. Raut ◽  
◽  
A. Patil ◽  
V. K Munipalli ◽  
M. Patel ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Reverse Phase ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed for quantitative determination of Regorafenib in tablet dosage form. In this method Hypersil Gold (C18, 150mm× 4.6mm id, 3μ) column with mobile phase consisting of Trifluoroacetic acid (0.2% v/v) and Acetonitrile in the ratio of (50: 50 v/v) at 400C in an isocratic mode was used. The detection was carried out at 260 nm and 20μL injection volume was selected with the flow rate 1mL/min. The linearity range of Regorafenib shows concentration between 5-200 μg/mL. The regression coefficient obtained was 0.999. Retention time of Regorafenib was found to be 6.49 minutes. Acetonitrile and Water in the ratio of (3:1) was used as a diluent. The method was validated as per ICH guidelines and is simple, fast, accurate, precise and can be applied for routine quality control analysis of Regorafenib in tablet dosage form.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF β-ACETYLDIGOXIN

2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Array Detector ◽  
Forced Degradation ◽  
Simple Method ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF NEW STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF METFORMIN HYDROCHLORIDE AND EMPAGLIFLOZIN IN TABLET DOSAGE FORM

2019 ◽  
Vol 12 (1) ◽  
pp. 241 ◽  
Author(s):  
Geetha Susmita A ◽  
Rajitha G ◽  
Ramya Yadav Y ◽  
Uma P
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Tablet Dosage

Objective: The objective of this study was to develop and validate a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of the metformin and empagliflozin in tablet dosage forms.Methods: The chromatographic conditions were optimized and it was run through Std. BDS (250 mm × 4.6 mm, 5 m) column with mobile phase consisting of 0.1% orthophosphoric acid buffer: acetonitrile in the ratio of 50:50. The flow rate was 1 ml/min and optimized wavelength was 210 nm. Temperature was maintained at 30°C.Results: The retention times of metformin and empagliflozin were found to be 2.588 min and 3.679 min and percentage relative standard deviation (RSD) of the metformin and empagliflozin was found to be 0.59 and 1.2, respectively. Percentage recovery was in the range of 100.01–100.65% for metformin and empagliflozin, respectively.Conclusion: A sensitive, rapid, and specific method has been developed for the simultaneous estimation of metformin and empagliflozin using RP-HPLC in tablet dosage form.

A Validated Stability Indicating RP-HPLC Method for the Estimation of an Anti-Cancer Drug Regorafenib in Pure and Pharmaceutical Dosage Form

2017 ◽  
Vol 4 (1) ◽  
pp. 5-10 ◽  
Author(s):  
Ramesh Jayaprakash ◽  
Senthil Kumar Natesan
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Cancer Drug ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A simple, economic, accurate, sensitive, specific and precise stability indicating reverse phase high performance liquid chromatographic [RP-HPLC] method for the determination of Regorafenib in pure and tablet dosage from was developed and validated. The chromatographic separation was carried out using Phenomenex Luna-C18 column (4.5x250 mm; 5 µm particle size) as a stationary phase and methanol: acetonitrile: water (55:25:20 v/v/v) as a mobile phase. The flow rate of 1 mL/min was used with PDA detection at 275 nm. The retention time of Regorafenib was 2.480 min. RP-HPLC method was developed with linearity range of 40-240 µg/mL of Regorafenib. The correlation coefficient [r2] was found to be 0.9999. The assay results obtained was in good agreement with the corresponding labeled amount by developed method within range of 98.83 ± 0.6937. Accuracy of the method was confirmed by recovery studies and the recoveries were found to be between 99.61 % and 100.22 %, the corresponding %RSD was found to be 0.2029. Precision, LOD, LOQ, specificity, robustness and ruggedness were performed as per ICH Q2(R1) guidelines and were within the acceptance criteria. This method can be conveniently used to detect the possible degradation product in the dosage form of Regorafenib during stability studies (acidic, alkaline, oxidative, thermal and photolytic). The method proved to be effective on the analysis of stressed marketed tablet formulation.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF NEW STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR SIMULTANEOUS ESTIMATION OF METFORMIN HYDROCHLORIDE AND EMPAGLIFLOZIN IN TABLET DOSAGE FORM

2019 ◽  
Vol 12 (1) ◽  
pp. 241
Author(s):  
Geetha Susmita A ◽  
Rajitha G ◽  
Ramya Yadav Y ◽  
Uma P
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Tablet Dosage

Objective: The objective of this study was to develop and validate a stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of the metformin and empagliflozin in tablet dosage forms.Methods: The chromatographic conditions were optimized and it was run through Std. BDS (250 mm × 4.6 mm, 5 m) column with mobile phase consisting of 0.1% orthophosphoric acid buffer: acetonitrile in the ratio of 50:50. The flow rate was 1 ml/min and optimized wavelength was 210 nm. Temperature was maintained at 30°C.Results: The retention times of metformin and empagliflozin were found to be 2.588 min and 3.679 min and percentage relative standard deviation (RSD) of the metformin and empagliflozin was found to be 0.59 and 1.2, respectively. Percentage recovery was in the range of 100.01–100.65% for metformin and empagliflozin, respectively.Conclusion: A sensitive, rapid, and specific method has been developed for the simultaneous estimation of metformin and empagliflozin using RP-HPLC in tablet dosage form.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF SACUBITRIL AND VALSARTAN IN PHARMACEUTICAL DOSAGE FORM

2017 ◽  
Vol 9 (5) ◽  
pp. 1
Author(s):  
Shweta Mishra ◽  
C. J. Patel ◽  
M. M. Patel
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Development And Validation ◽  
Tablet Dosage

Objective: This study aims to develop and validate a stability indicating HPLC method for simultaneous estimation of sacubitril and valsartan in pharmaceutical dosage form.Methods: Sacubitril and valsartan separation were achieved by LC-20 AT C18 (250 mm x 4.6 mm) column and buffer (potassium phosphate, pH 3.0): methanol (50:50) as mobile phase, at a flow rate of 1 ml/min (millilitre per minute). Detection was carried out at 224 nm (nanometer). The different HPLC experimental parameters were optimized and the method was validated according to the standard guideline. Forced degradation experiments were carried out by exposing sacubitril and valsartan standard and sample for thermal, photolytic, oxidative and acid-base hydrolytic stress conditions.Results: Retention time of sacubitril and valsartan were found to be 4.170 min (minute) and 6.530 min (minute) respectively. The method has been validated for linearity, accuracy, precision, LOD, and LOQ. Linearity observed for sacubitril is 12.25-36.75 μg/ml (microgram per milliliter) and for valsartan is 12.75-38.25 μg/ml (microgram per milliliter). The results showed that sacubitril and valsartan and the other degradation products were fully resolved and thus the proposed method is stability-indicating.Conclusion: The proposed HPLC method was found to be simple, specific, precise, accurate, rapid and economical for simultaneous estimation of valsartan and sacubitril in bulk and tablet dosage form. Thus the validated economical method was applied for forced degradation study of sacubitril and valsartan tablet.

scholarly journals Development and Validation of a Stability-Indicating HPLC Method for the Quantification of α-Mangostin in Dietary Supplements

2019 ◽  
Vol 14 (7) ◽  
pp. 1934578X1986394 ◽  
Author(s):  
Blanca Rivero ◽  
Iliana Garibay
Keyword(s):  
Dietary Supplements ◽  
High Performance ◽  
Degradation Products ◽  
Principal Component ◽  
Hplc Method ◽  
Garcinia Mangostana ◽  
Reverse Phase ◽  
Pharmacological Activities ◽  
Stability Indicating ◽  
Development And Validation

Xanthones are the main active constituents isolated from Garcinia mangostana L. (Hypericaceae). Among these, α-mangostin (1) is reported as the principal component of the species, with remarkable pharmacological activities. In this work, a reverse-phase high-performance liquid chromatography (HPLC) method was developed as a suitable stability-indicating procedure for the quantification of 1 in the presence of degradation products. Chromatographic analysis was performed on a Purospher STAR C18 column with a mobile phase containing 0.1% trifluoroacetic acid in water and ACN (20:80) at a flow rate of 1.0 mL/min. The method was linear over the concentration range of 10 to 100 μg/mL. The limits of detection and quantification were 0.13 and 0.4 μg/mL, respectively. Stability studies were carried out at temperature/relative humidity of 30°C/60% and 40°C/75% during 6 months; and no significant changes were observed. According to the global results, a simple HPLC method was developed and fully validated for quantifying 1 in mangosteen dietary supplements.

scholarly journals Stability-Indicating RP-HPLC Method for Simultaneous Estimation of Enrofloxacin and Its Degradation Products in Tablet Dosage Forms

2015 ◽  
Vol 2015 ◽  
pp. 1-11 ◽  
Author(s):  
V. Ashok Chakravarthy ◽  
B. B. V. Sailaja ◽  
Avvaru Praveen Kumar
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage

The present work was the development of a simple, efficient, and reproducible stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method for simultaneous determination enrofloxacin (EFX) and its degradation products including ethylenediamine impurity, desfluoro impurity, ciprofloxacin impurity, chloro impurity, fluoroquinolonic acid impurity, and decarboxylated impurity in tablet dosage forms. The separation of EFX and its degradation products in tablets was carried out on Kromasil C-18(250×4.6 mm, 5 μm) column using 0.1% (v/v) TEA in 10 mM KH2PO4(pH 2.5) buffer and methanol by linear gradient program. Flow rate was 1.0 mL min−1with a column temperature of 35°C and detection wavelength was carried out at 278 nm and 254 nm. The forced degradation studies were performed on EFX tablets under acidic, basic, oxidation, thermal, humidity, and photolytic conditions. The degraded products were well resolved from the main active drug and also from known impurities within 65 minutes. The method was validated in terms of specificity, linearity, LOD, LOQ, accuracy, precision, and robustness as per ICH guidelines. The results obtained from the validation experiments prove that the developed method is a stability-indicating method and suitable for routine analysis.

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