scholarly journals Quantification and Stability Indicating Method Development and Validation of Vismodegib in Bulk and Pharmaceutical Dosage Form by Ultra Performance Liquid Chromatography

2021 ◽  
pp. 858-866
Author(s):  
V. Mohan Goud ◽  
M. Harini ◽  
CH. B. Praveena Devi ◽  
M. Meghana Goud
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Wave Length ◽  
Accurate Method ◽  
Ultra Performance Liquid Chromatography ◽  
Routine Analysis ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Stability Indicating Method

Background: Vismodegib (VMD) is a drug of choice for the treatment of basal-cell carcinoma. Present studies carried out to estimate VMD by RP-UPLC technique and to develop a simple, précised, accurate method for routine analysis. Methods: For this purpose Chromatographic conditions used were stationary phase STD BEH C18  column (100 mm x 2.1 mm, 1.8m), a mixture of Methanol:KH2PO4 taken in the ratio 50:50%v/v as a mobile phase with a pH 7.4 and flow rate was maintained at 0.3ml/min, detection wave length was Acquity TUV 254nm, column temperature was set to 30oC and diluent was mobile phase, Conditions were finalized as optimized method. Results: System suitability parameters were studied by injecting the standard six times. Linearity study was carried out between 25% to150% (37.5-225µg/ml) levels, R2 value was found to be as 0.9992. Precision was found to be 0.6 for repeatability and 0.4 for intermediate precision. LOD and LOQ are 0.33 µg/ml and 0.99 µg/ml respectively and results were well under the acceptance criteria. Conclusion: By using above method assay of marketed formulation was carried out and was found 100.12%. Degradation studies of VMD were done, in all conditions purity threshold was more than purity angle and within the acceptable range. The developed method was simple and can be used for routine analysis.

scholarly journals Stability Indicating Method Development and Validation of Cenobamate in Bulk and Dosage form by Liquid Chromatography

2021 ◽  
pp. 120-131
Author(s):  
K. Athulya Damodharan ◽  
. Nuaman ◽  
M. Archana ◽  
Mariya Palathingal ◽  
P. Ashisha ◽  
...  
Keyword(s):  
Method Development ◽  
Wave Length ◽  
Accurate Method ◽  
Intermediate Precision ◽  
Column Temperature ◽  
Stability Indicating Method ◽  
System Suitability ◽  
Method Development And Validation ◽  
Phase Symmetry ◽  
Development And Validation

A simple, Precise, Accurate method was developed for the estimation of Cenobamate   by RP-HPLC technique. Chromatographic conditions used are stationary phase symmetry C18 (150 mm* 4.6 mm 5 µm), mobile phase Acetonitrile: 0.01NKH2PO4in the ratio of 55:45 and flow rate was maintained at 1.0ml/min, detection wave length was 272.0 nm; column temperature was set to 30oC. Retention time was found to be 2.908 min. System suitability parameters were studied by injecting the standard six times and results were well under the acceptance criteria. Linearity study was carried out between 25% to150 % levels, R2 value was found to be as 0.999.Precision was found to be 0.5 for repeatability and 0.8 for intermediate precision. LOD and LOQ are 0.01µg/ml and 0.03µg/ml respectively. By using above method assay of marketed formulation was carried out 100.32% was present. Degradation studies of Cenobamate were done, in all conditions purity threshold was more than purity angle and within the acceptable range.

FORCED INDICATING UPLC-DAD METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF APALUTAMIDE IN BULK AND IN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (09) ◽  
pp. 73-75
Author(s):  
China Babu D ◽  
Madhusudhana Chetty C ◽  
Mastanamma S. K ◽  
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Uv Light ◽  
Accurate Method ◽  
Pharmaceutical Dosage Form ◽  
Good Ability ◽  
Acquity Uplc ◽  
Development And Validation

A new analytical method was developed for the estimation of apalutamide in bulk and its pharmaceutical formulation. The sensitive, précise and accurate method was developed by using Waters Acquity UPLC system equipped with quaternary gradient pump. The column used was Waters C18 150 X 2.1 mm X 1.7 µm and mobile phase was 0.2 % OPA buffer in water : acetonitrile in the ratio of 25:75 V/V. The buffer pH was maintained at 4.5. The fl ow rate of mobile phase was 0.5 mL min-1 and detection was at 272 nm by using PDA detector. The method was performed at ambient temperature. The retention time of the apalutamide was 1.27 min. The % RSD value in precision was >2 %. The accuracy of the method was found to be between 99.54 % - 100.01 %. The limit of detection and limit of quantifi cation values were found to be 0.14 µg mL-1 and 0.48 µg mL-1, respectively. The linearity concentration range was found to be 11.25 - 67.5 µg mL-1, it show wide linearity concentration range. The method was proved to have good robustness after changing parameters of fl ow rate, temperature and mobile phase composition. The method showed good ability towards different stress conditions of acidity, alkalinity, peroxide and UV-light. The method can be used for the routine analysis of apalutamide in bulk and its pharmaceutical dosage form by using UPLC.

scholarly journals STABILITY INDICATING METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF PANOBINOSTAT LACTATEIN PHARMACEUTICAL DOSAGE FORMS BY UPLC

2018 ◽  
Vol 10 (11) ◽  
pp. 60
Author(s):  
Ashok Gorja ◽  
Sumanta Mondal
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Thermal Conditions ◽  
Ultra Performance Liquid Chromatography ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stability Indicating Method

Objective: The present study aimed to develop a stability indicating ultra-performance liquid chromatography (UPLC) method for the estimation of panobinostat lactate in pharmaceutical dosage form and validate the method in accordance with ICH guidelines.Methods: The optimized conditions for the developed UPLC method are acquity UPLC hibar C18 (100 mm × 2.1 mm, 1.8µ) column maintained at 30°C with mobile phase consisting of 0.1% ortho phosphoric acid and acetonitrile in the ratio 50:50%v/v on isocratic mode at flow rate 0.3 ml/min. The sample was detected at 266 nm.Results: The retention time for panobinostat was found to be 1.6 min. The developed method was validated for accuracy, precision, specificity, ruggedness, robustness and solution stability. The method obeyed Beer’s law in the concentration range of 50µg/ml and 300µg/ml with correlation coefficient of 0.9998. Forced degradation studies were conducted by exposing the drug solution to various stress conditions such as acidic, basic, peroxide, neutral, photolytic and thermal conditions. The net degradation was found to be within the limits, indicating that drug is stable in stressed conditions.Conclusion: The developed method for the estimation ofpanobinostat can be utilized for the routine analysis of pharmaceutical dosage form.

scholarly journals RAPID ANALYTICAL METHOD FOR ASSAY DETERMINATION FOR PROCHLORPERAZINE EDISYLATE DRUG SUBSTANCES BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY

2017 ◽  
Vol 9 (4) ◽  
pp. 118 ◽  
Author(s):  
Kishorkumar L. Mule
Keyword(s):  
Liquid Chromatography ◽  
Trifluoroacetic Acid ◽  
Analytical Method ◽  
Mobile Phase ◽  
Ultra Performance Liquid Chromatography ◽  
Drug Substance ◽  
Assay Method ◽  
Column Temperature ◽  
Drug Substances

Objective: To develop and validate new, simple and rapid assay method for Prochlorperazine edisylate drug substance by UPLC as per ICH guidelines.Methods: Ultra performance liquid chromatographic method was developed, optimized and validated on Acquity UPLC by using Acquity BDH300 C4 (100 x 2.1 mm) 1.7µ column. 3.85g ammonium acetate in 1000 ml of water add 0.5 ml trifluoroacetic acid and 1 ml triethylamine (Mobile phase A): 0.5 ml trifluoroacetic acid in 1000 ml acetonitrile mobile phase (Mobile phase B) with gradient program. Detector wavelength 254 nm and column temperature 30 °C.Results: Linearity study was carried out for prochlorperazine edisylate, linearity was calculated from 80 % level to 120% with respect to specification level. The correlation coefficient (r) = 0.999 was proved that the method is robust. The resolution between known impurities and Prochlorperazine edisylate found more than 2.5, it was evident from specificity test that Prochlorperazine edisylate peak are well separated from its related impurities, hence the method is specific. Prochlorperazine edisylate sample solution and mobile phase were found to be stable for at least 3 d.Conclusion: A new, simple and rapid method has been developed and validated for assay determination of prochlorperazine edisylate in drug substance by Ultra Performance Liquid Chromatography (UPLC). The analytical method was developed and validated as per ICH guidelines. The developed method can be used for the fast assay determination of prochlorperazine edisylate drug substances in research laboratories and in the pharmaceutical industry. 

HPLC METHOD DEVELOPMENT, VALIDATION, AND FORCED DEGRADATION FOR SIMULTANEOUS ANALYSIS OF OXYCODONE AND NALTREXONEIN PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (02) ◽  
pp. 31-38
Author(s):  
R. S. Ch Phani ◽  
◽  
K. R. S. Prasad ◽  
R. M Useni
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Degradation Study ◽  
Ich Guidelines ◽  
Hplc Method Development

A simple, precise and stability-indicating RP-HPLC method was developed for simultaneous quantification of oxycodone (OXCD) and naltrexone (NTRX) in combined dosage form. The developed method was validated with respect to precision, linearity, accuracy, robustness, ruggedness, sensitivity and solution stability. The method was developed with ammonium di hydrogen phosphate buffer (pH 5.0) and acetonitrile in a ratio of 55:45 (v/v) as mobile phase at a flow rate of 1.0 mL/minute over Intersil ODS C18 column (250 mm × 4.6 mm×5μ).The UV detection wavelength was fixed at 235 nm. The column temperature was maintained at ambient temperature. The method showed good linearity with correlation coefficient values of 0.9990 and 0.9994 for OXCD and NTRX. The percent recoveries of the two drugs found within the limits of 98.0–102.0%. The LOQ concentrations of OXCD and NTRX are 0.625 μg/ mL and 0.075 μg/mL, respectively. The LOD concentrations of OXCD and NTRX are 0.3125 μg/mL and 0.0375 μg/mL, respectively. According to ICH guidelines forced degradation study was validated.

scholarly journals Simultaneous and Trace Level Determination of Six Potential Impurities by UPLC-ESI-MS/MS in Antiarrhythmic Drug: Dronedarone Hydrochloride

2020 ◽  
Vol 32 (5) ◽  
pp. 1183-1190
Author(s):  
K. Durga Raja ◽  
V. Saradhi Venkata Ramana ◽  
K. Raghu Babu ◽  
B. Kishore Babu ◽  
V. Jagadeesh Kumar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Solvent Mixture ◽  
Column Temperature ◽  
Esi Ms ◽  
Quantitation Limit ◽  
Ich Guidelines ◽  
Validation Tests ◽  
Development And Validation

Development and validation of six potential impurities by ultra performance liquid chromatography electro spray ionization tandem mass (UPLC-ESI-MS/MS) method for dronedarone hydrochloride drug was accomplished coherent with ICH guidelines. Successful chromatographic separation of dronedarone with its six impurities was attained by using gradient elution mode on RP-UPLC column using three pump mode system of 0.1 % formic acid in water as mobile phase A, methanol as the mobile phase B and solvent mixture of methanol, acetonitrile and water in the ratio of 65:30:5 v/v/v as the mobile phase C. Chromatographic conditions were set as 0.3 mL min-1 flow rate at the column temperature of 45 °C with the injection volume 2 μL. Briefly, the method enabled quantitation of six impurities with high accuracy (recovery > 90 %) and precision (% RSD < 5.0),within the ranges of 0.18-2.82 μg g-1. The regression (r) for each impurity over a range was > 0.99. The detection limit and quantitation limit of impurities were set at 0.09 and 0.18 μg g-1, respectively. The performed validation tests proved the suitability of the method for its intended purposes.

scholarly journals BIOEQUIVALENCE STUDIES OF MARKETED CLOZAPINE TABLETS BY USING OPTIMIZED VALIDATED LIQUID CHROMATOGRAPHIC METHOD

2018 ◽  
Vol 10 (3) ◽  
pp. 47
Author(s):  
Udayasree Konikuru ◽  
Rajavel P. ◽  
Vijitha S.
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Accurate Method ◽  
Stability Studies ◽  
Column Temperature ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Dissolution Apparatus ◽  
Liquid Chromatographic ◽  
Interday Precision

Objective: A simple, selective, precise and accurate method was developed for the estimation of Clozapine by RP-HPLC technique.Methods: Chromatographic conditions used are stationary phase, Phenomenex BDS (150 mm x 4.6 mm, 5µ), Mobile phase was methanol and water in (80:20) ratio and flow rate was maintained at 1.0 ml/min, column temperature was set at 25 °C, detection wavelength was 240 nm, and diluent was mobile phase. These conditions were finalized for the optimized method.Results: Linearity study was carried out between 10-60 µg/ml, the R2 value was found to be as 0.995. Precision was found to be as follows for system precision 1.052, method precision 1.662, and intraday precision 1.02 and for interday precision 0.93. The % Recovery was found to be 98.60%. LOD and LOQ were found to be 2.7 µg/ml and 8.4 µg/ml respectively. By using the above method assay of the marketed formulation was carried out and the % purity was found to be 99.28 %. Stability studies of Clozapine were done, in all conditions degradation was found to be within the acceptable range.Conclusion: The current validated method was finally applied in bioequivalence studies of four different brands of Clozapine by using dissolution apparatus and percentage drug release was found to be 99.48%, it was within the acceptable limit (NLT 85 %) as per USP.

scholarly journals Development and validation of novel RP-UPLC method for estimation of atropine sulphate in pharmaceutical dosage form

2013 ◽  
Vol 19 (3) ◽  
pp. 333-337 ◽  
Author(s):  
A.C. Arvadiya ◽  
P.P. Dahivelker
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Atropine Sulphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Development And Validation

A simple, precise, accurate, sensitive and repeatable RP-UPLC method was developed for quantitative determination of atropine sulphate in pharmaceutical dosage form. The method was developed by using C18 column Hiber HR Purospher Star (100mm?2.1mm id, 2?m particle size) as stationary phase with Phosphate Buffer: Acetonitrile (87:13, %v/v) as a mobile phase, pH was adjusted to 3.5 by ortho-phosphoric acid at a flow rate of 0.5 mL/min and column temperature maintained at 30?C. Quantification of eluted compound was achieved with PDA detector at 210 nm. Atropine sulphate followed linearity in concentration range of 2.5-17.5 ?g/mL with r2=0.9998 (n=6). Limit of detection (LOD) and limit of quantification (LOQ) values were 0.0033 and 0.0102 ?g/mL for atropine sulphate. The validation study is carried out as per International Conference on Harmonization (ICH) guidelines. This method was successfully applied for estimation of atropine sulphate in pharmaceutical formulation.

scholarly journals Stability-indicating method development and validation for the concurrent determination of darunavir, cobicistat, emtricitabine and tenofovir alafenamide by UPLC in bulk and tablet dosage forms

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
M. Satya Venkata Sakuntala ◽  
A. Lakshmana Rao ◽  
M. William Carey
Keyword(s):  
Method Development ◽  
Correlation Coefficients ◽  
Dosage Forms ◽  
Forced Degradation ◽  
Cytochrome P450 3A ◽  
Column Temperature ◽  
Stability Indicating Method ◽  
Tenofovir Alafenamide ◽  
Development And Validation ◽  
Tablet Dosage

Abstract Background Tablet dosage forms containing combination of darunavir a protease inhibitor, cobicistat a cytochrome P450 3A inhibitor, emtricitabine and tenofovir alafenamide which were nucleoside reverse transcriptase inhibitors were approved by USFDA on 1st July 2018 to suppress the viral load in HIV patients. It can be used as a complete regimen for the treatment of HIV-1 infection in adults and paediatric patients weighing at least 40 kg. An UPLC method was developed, and separation was done on SB C8 column of dimensions 50 × 2.1 × 1.8 μ with mobile phase 0.01 N potassium dihydrogen ortho phosphate (pH-4.8) and acetonitrile in 60:40 ratio, at a flow rate of 0.3 mL/min and an injection volume of 2 μL. The column temperature was maintained at 30 °C, and detection wavelength was 267 nm. The method was validated according to ICH guidelines. Results The retention times were 1.031, 1.341, 1.630 and 2.153 min, and they were linear in the concentration range of 1.25–7.5 μg/mL, 18.75–112.5 μg/mL, 25–150 μg/mL and 100–600 μg/mL for tenofovir alafenamide, cobicistat, emtricitabine and darunavir, respectively. The intraday and interday precisions were found to be within acceptable limits. LOD was found to be 0.06 μg/mL, 0.51 μg/mL, 1.31 μg/mL and 3.01 μg/mL, and LOQ was 0.19 μg/mL, 1.54 μg/mL, 3.96 μg/mL and 9.13 μg/mL for tenofovir alafenamide, cobicistat, emtricitabine and darunavir. The correlation coefficients were found to be more than 0.999, and recovery was more than 99.52% indicating the method was accurate. Forced degradation studies reveal that the drugs are unstable under acidic conditions. The method was simple, accurate, precise, stable and can be analysed in less runtime of 4 min. Conclusions The flexibility, accuracy and precision of the developed method ensure its applicability in routine analysis of tablet dosage forms. Graphical Abstract

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