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.

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 Method Development and Validation of Metformin Hydrochloride in Tablet Dosage Form

2011 ◽  
Vol 8 (3) ◽  
pp. 1309-1313 ◽  
Author(s):  
Kaushelendra Mishra ◽  
Himesh Soni ◽  
Govind Nayak ◽  
Sita Sharan Patel ◽  
A. K. Singhai
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Wave Length ◽  
Metformin Hydrochloride ◽  
Limit Of Quantification ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

A simple, reproducible and efficient method for the determination of metformin hydrochloride (MET) was developed and validated. The analysis complied with Beer's law in the concentration range of 8-13 μg/mL at 233 nm for MET. In our study the validation of analytical method for determination of MET by UV in tablets formulation was performed in accordance the parameters including-system suitability, specificity, limit of quantification, limit of detection, linearity of response, accuracy, precision (reproducibility & repeatability), robustness (change of wave length±2 nm).

A NEW METHOD DEVELOPMENT AND VALIDATION FOR RELATED SUBSTANCES OF GRANISETRON IN ACTIVE PHARMA INGREDIENT BY HPLC

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (07) ◽  
pp. 52-59
Author(s):  
T. N Rao ◽  
◽  
Y. Prasanthi ◽  
Parvatamma Botsa ◽  
G. Kumara ◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Column Temperature ◽  
Related Substances ◽  
System Suitability ◽  
Method Development And Validation ◽  
Development And Validation

A simple and inexpensive method was developed using high performance liquid chromatography with PDA detection for determination of granisetron hydrochloride and related impurities (2-methyl-N- [(1R,3r,5S)-9-methyl-9-azabicyclo[3.3.1]non-3-yl]-2H-indazole-3-carboxamide, 1-Methyl-N-[(1R,3r,5S)- 9-methyl-9-azabicyclo[3.3.1]non-3-yl]-1H-indazole-3-carboxamide hydrochloride, N-[(1R,3r,5S)-9- azabicyclo[3.3.1]non-3-yl]-1-methyl-1H-indazole-3-carboxamide and 1-methyl-1H-indazole-3-carboxylic acid. The chromatographic separations were achieved on (250×4.6 mm), 5.0 μm make: Waters, Symmetry Shield C8 column employing acetonitrile: 2% V/V H3PO4 in MilliQ water + 0.1% V/V hexylamine in water, 800:200 V/V (pH adjusted to 7.5 using triethylamine) mobile phase with isocratic programme. A flow rate of 1.5 mL/min was chosen. Four impurities were eluted within 20 minutes. The column temperature was maintained at 40°C and a detector wavelength of 300 nm was employed. The method was successfully validated by establishing system suitability, specificity, linearity, accuracy, limit of detection and limit of quantification.

scholarly journals Analytical Method Development and Validation of Rp-Hplc Method for Simultaneous Estimation of Pyridoxamine Dihydrochloride and Acetylcysteine in Tablet Dosage Form.

2021 ◽  
Vol 23 (06) ◽  
pp. 992-1000
Author(s):  
Sneha S. Ghule ◽  
◽  
Ashpak M. Tamboli ◽  
Snehal D. Patil ◽  
◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
System Suitability ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

A reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of Pyridoxamine dihydrochloride and Acetylcysteine in the marketed formulation is developed. Chromatography carried out at 30oc temperature on Agilent Zorbax Bonus-RP (250 x 4.6 mm, 5 µ) coloum. Coloum using a mobile phase 0.1% trifluroacetic acid in water: acetonitrile (80:20v/v) with flow rate 1ml/min (DAD scan at 210nm). Validation parameters such as system suitability, linearity, precision, accuracy are considered as reported International Conference on Harmonization guidelines. The retention times for Pyridoxamine dihydrochloride and Acetylcysteine are 2 min and 3.4 min. The linearity range for Pyridoxamine dihydrochloride and Acetylcysteine is 30-70 µg/ml and 180-420 µg/ml. The %RSD for accuracy was found to be less than 2%. Hence the proposed method was found to be accurate, precise, reproducible, and specific and can be used for simultaneous analysis of these drugs in tablet formulation.

scholarly journals LC-MS/MS METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF CARDIAZOL IN HUMAN PLASMA

2019 ◽  
pp. 380-385
Author(s):  
IRYNA DRAPAK ◽  
BORYS ZIMENKOVSKY ◽  
LINA PEREKHODA ◽  
SERGIY KOVALENKO ◽  
Liliya Logoyda
Keyword(s):  
Formic Acid ◽  
Human Plasma ◽  
Method Development ◽  
Accurate Method ◽  
Sample Volume ◽  
Ich Guidelines ◽  
Coefficients Of Variation ◽  
Method Development And Validation ◽  
Development And Validation

Objective: The main purpose of this study was to develop a simple, precise, rapid and accurate method for the quantification of cardiazol in human plasma. Methods: Chromatography was achieved on Discovery C18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile-water–formic acid, 5: 95: 0.1 v/v), eluent B (acetonitrile–formic acid, 100: 0.1 v/v)). The initial content of the eluent B of 8%, which increases linearly to 1.0 min to 100%, is maintained up to 1.5 min and returned to the original 8% to 1.51 min. The mobile phase was delivered at a flow rate of 0.400 ml/min into the mass spectrometer ESI chamber. The sample volume was 300 μl. Results: The total chromatographic run time was 2.5 min and the elution of cardiazol and IS (difenoconazole) occurred at ~2.15 and 1.98 min, respectively. A linear response function was established at 1-100 ng/ml for cardiazol and difenoconazole in human plasma. The % mean recovery for cardiazol in LQC, MQC and HQC was 102.8 %, 100.3 % and 95.9 %. The lowest concentration with the RSD<20% was taken as LLOQ and was found to be 1.10 ng/ml for cardiazol. The % accuracy of LLOQ samples prepared with the different biological matrix lots was found 109.7 %, which were found within the range of 80.00-120.00 % for the seven different plasma lots. % CV for LLOQ samples was observed as 11.9 %, which are within 20.00% of the acceptance criteria. The within-run coefficients of variation ranged between 0.311 % and 0.601 % for cardiazol. The within-run percentages of nominal concentrations ranged between 99.80 % and 100.41 % for cardiazol. The between-run coefficients of variation ranged between 0.332 % and 0.615 % for cardiazol. The between-run percentages of nominal concentrations ranged between 98.18 % and 101.21 % for cardiazol. Conclusion: A rapid method was developed for simultaneous determination of cardiazol in human plasma. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that the proposed strategy can be effortlessly and advantageously applied for routine examination of cardiazol in human plasma.

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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