Stability indicating assay method for determination of Febuxostat by RP-HPLC

2021 ◽  
Vol 01 ◽  
Author(s):  
Ramanlal N. Kachave ◽  
Pragati B. Mandlik ◽  
Akshay G. Mundhe
Keyword(s):  
Limit Of Detection ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
Limit Of Quantitation

Objective: A simple, rapid, precise and accurate RP-HPLC stability indicating method was developed and validated for estimation of Febuxostat in bulk drug and marketed tablet formulation. Methods: The chromatographic separation was achieved on Agilent C18 (250 x 4.6mm, 5 µm) using solvent 15 mM ammonium acetate buffer (pH 4.8) and acetonitrile (30:70 v/v) as a mobile phase at flow rate of 1 mL/min and at ambient column temperature analysis were carried out at detection wavelength 315nm. Result: The method was validated for linearity, precision, accuracy, specificity, LOD and LOQ, and robustness. The linearity was studied in the concentration range of 5-25 µg/mL and correlation coefficient was found to be 0.999. The limit of detection and limit of quantitation were found to be 0.37 µg/mL and 1.13 µg/mL. Febuxostat was subjected to stress condition of degradation including acidic, alkaline, oxidation, photolytic and thermal degradation. Febuxostat is more sensitive toward acidic condition than oxidation and less sensitive towards alkaline, thermal and photolytic degradation. Conclusion: The method is simple, reliable, sensitive and precise which could separate the drug and their degraded product formed under various stress conditions, thus it can be employed as stability indicating method for the determination of FBX in bulk and pharmaceutical dosage form.

scholarly journals STABILITY INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF VILDAGLIPTIN AND METFORMIN IN PHARMACEUTICAL DOSAGE FORM

2017 ◽  
Vol 9 (3) ◽  
pp. 150
Author(s):  
Ramesh Jayaprakash ◽  
Senthil Kumar Natesan
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The present study was aimed to develop a rapid, accurate, linear, sensitive and validate stability-indicating high performance liquid chromatographic [RP-HPLC] method for determination of vildagliptin and metformin in pharmaceutical dosage form.Methods: The chromatographic separation was performed on kromasil-C18 column [4.5 x 250 mm; 5 µm] using a mobile phase consisting of 0.05 mmol potassium dihydrogen phosphate buffer: acetonitrile [80:20 v/v], [pH adjusted to 3.5 using orthophosphoric acid]. The flow rate is 0.9 ml/min and the detection was carried out at 263 nm.Results: The chromatographic condition, the peak retention time of metformin and vildagliptin were found to be 2.215 min and 2.600 min respectively. Stress testing was performed in accordance with an international conference on harmonization [ICH] Q1A R2 guidelines. The method was validated as per ICH Q2 R1 guidelines. The calibration curve was found to be linear in the concentration range of 5-17.5 µg/ml and 50-175 µg/ml for vildagliptin and metformin. The limit of detection and quantification was found to be 0.0182 µg/ml and 0.0553 µg/ml for vildagliptin and 0.4451 µg/ml and 1.3490 µg/ml for metformin respectively.Conclusion: A new sensitive, simple and stability indicating reverse-phase high-performance liquid chromatography [RP-HPLC] method has been developed and validated for the determination of vildagliptin and metformin. The proposed method can be used for routine determination of vildagliptin and metformin.

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE DETERMINATION OF BAMIFYLLINE HYDROCHLORIDE IN TABLET DOSAGE FORM

2017 ◽  
Vol 9 (4) ◽  
pp. 76
Author(s):  
Panchumarthy Ravisankar ◽  
Shaheem Sulthana ◽  
Inturi Mary Thanuja ◽  
A. Dihitha Chowdary ◽  
J. Vyshnavi
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Array Detector ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Limit Of Quantitation ◽  
Tablet Dosage

Objective: The objective of the current study was to develop and validate a novel RP-HPLC method for determination of bamifylline hydrochloride in pharmaceutical dosage form.Methods: Chromatographic separation was conducted on Agilent technologies-1260 series with the G1311C quaternary pump, eclipse XDB C18 column (4.6 mm i.d. X 250 mm, 5 µm particle sizes) and equipped with photodiode array detector G1315D. Mobile phase consisted of methanol and acetonitrile were mixed in the ratio of 90:10 v/v, was used at a flow rate of 1 ml/min and detection wavelength was set at 263 nm.Results: The retention time for bamifylline hydrochloride was found to be 2.913 min. The calibration was linear (r2= 0.9996) in the concentration range of 2-10 µg/ml. The limit of detection and the limit of quantitation were found to be 0.4825 μg/ml and 1.4621 µg/ml respectively. Recovery of bamifylline hydrochloride in tablet formulation was observed in the range of 99.6-99.8 %. Percentage assay of bamifylline hydrochloride (Bamifix) was found to be 99.4 % w/w.Conclusion: Thus the novel proposed method for bamifylline hydrochloride was found to be feasible for the estimation of bamifylline hydrochloride in bulk as well as a pharmaceutical dosage form. 

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF CIPROFLOXACIN AND FLUOCINOLONE ACETONIDE IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 134-138
Author(s):  
MADHAVI KUCHANA ◽  
CHAMUNDESWARI KANDUKURU ◽  
PRASANTHI CHENGALVA
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Fluocinolone Acetonide ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation

Objective: To develop and validate a reverse phase high performance liquid chromatographic method for simultaneous estimation of ciprofloxacin and fluocinolone acetonide in bulk and pharmaceutical dosage form. Methods: The chromatographic separation was achieved on reverse phase Discovery Inertsil ODS3V Column, C18 (250 mm, 4.6 mm, 5 µm). The separation was achieved by employing the mobile phase consists of phosphate buffer (pH 4) and acetonitrile (40:60). The flow rate was 1.0 ml/min, at a detection wavelength of 295 nm. The proposed method was validated as per the International Council for Harmonisation (ICH) guidelines.Results: The retention time for ciprofloxacin and fluocinolone acetonide was found at 3.627 min and 5.037 min respectively. The proposed method was validated for specificity, accuracy, precision, linearity, the limit of detection (LOD), limit of quantitation (LOQ) and robustness. All validation parameters were within the acceptable range. The assay method was linear and found in the range from 12.5–37.25 µg/ml for ciprofloxacin and 0.625–1.875 µg/ml of fluocinolone acetonide. The relative standard deviation (RSD) values for ciprofloxacin and fluocinolone acetonide were 0.25 % and 0.18 %, respectively. Conclusion: A rapid, accurate and precise RP-HPLC method was developed for the simultaneous estimation of ciprofloxacin and fluocinolone acetonide in bulk and ointment formulation. The developed method was validated for specificity, accuracy, precision, linearity, the limit of detection, limit of quantitation and robustness according to ICH guidelines.

Validated Stability Indicating Method for Determination of Indapamide in Pharmaceutical Formulation

2021 ◽  
pp. 3347-3352
Author(s):  
Gopal Prasad Agrawal
Keyword(s):  
Signal To Noise Ratio ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Average Accuracy ◽  
Partical Size ◽  
Analysis Stability

A stability indicating method for Indapamide in an oral antihypertensive tablet and bulk dosage forms was developed and validated by reverse phase HPLC (RP-HPLC). The proposed RP-HPLC Shisheido Capcell Pak C18 column was used and column dimension was 250mm × 4.6mm i.d., 5μm partical size at ambient temperature. The mobile phase Methanol and Phosphate Buffer pH 5.8 (60:40) was run in isocratic mode at a flow rate of 1.0ml/minute. The wavelength of Indapamide was selected at 241nm. Indapamide was found as single peak in the chromatogram at 6.58 min. The different chromatographic conditions were applied to determine the drug in pharmaceutical dosage form. The linearity of the proposed method was found in a range of 0.2-1.2μg/ml with coefficient of correlation (r2) value 0.999, slope 8360 and intercept -77.78. The percent RSD of intraday precision and interday precision were found in range of 0.498 - 1.661 and 0.882 - 1.623 respectively. The average accuracy of the method at three different levels of 50, 100 and 150 % were found to be 100.67, 99.50 and 100.65, respectively. The LOQ and LOD expressed as signal to noise ratio (S/N) were found to be 0.03 and 0.08μg/mL with good accuracy and precision. Indapamide was exposed to different stress conditions like alkaline, acidic, thermal, oxidative and photolytic. The stressed samples were analyzed by the proposed method. The proposed methods can be used for routine analysis stability testing and assay of Indapamide in quality control laboratories.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

scholarly journals A A RAPID AND SENSITIVE RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF EMPAGLIFLOZIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2019 ◽  
pp. 60-65
Author(s):  
MADHURIMA BASAK ◽  
Santhosh Reddy Gouru ◽  
Animesh Bera ◽  
Krishna veni Nagappan
Keyword(s):  
Quantitative Analysis ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Bulk Drug

Objective: The present study aims at developing an accurate precise, rapid and sensitive Reverse Phase High-Performance Liquid Chromatography (RP-HPLC) method for assessing Empagliflozin in bulk drug and in the pharmaceutical dosage form. Methods: The proposed method employs a Reverse Phase Shim Pack C18 column (250 mm × 4.6 mm id; 5 µm) using a mobile phase comprising of acetonitrile and water in the ratio of 60:40 v/v flushed at a flow rate of 1 ml/min. The eluents were monitored at 223 nm. Results: Empagliflozin was eluted at a retention time of 5.417 min and established a co-relation co-efficient (R2>0.999) over a concentration ranging from 0.0495-100µg/ml. Percentage recovery was obtained between 98-102% which indicated that the method is accurate. The Limit of Detection (LOD) and Limit of Quantitation (LOQ) were found at 0.0125µg/ml and 0.0495µg/ml, respectively. Conclusion: An RP-HPLC method which was relatively simple, accurate, rapid and precise was developed and its validation was performed for the quantitative analysis of empagliflozin in bulk and tablet dosage form (10 and 25 mg) in accordance to International Conference of Harmonization (ICH) Q2 (R1) guidelines. The proposed method may aid in routinely analyzing empagliflozin in pharmaceuticals.

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