scholarly journals Development and Validation of RP-HPLC Assay Method for Vildagliptin Using Qbd Approach and Its Application to Forced Degradation Studies

2016 ◽  
Vol 8 (03) ◽  
Author(s):  
Meetali M. Chaphekar ◽  
Purnima Hamrapurkar
Keyword(s):  
Method Development ◽  
Accurate Determination ◽  
Interaction Effects ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies

The concept of Quality by design (QbD) has recently gained importance in the area of analytical method development and involves understanding of the critical factors and their interaction effects by a desired set of experiments. So, the present work describes the development of Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) method by QbD approach using Design of Experiments and subsequent validation for analysis of Vildagliptin in bulk drug and its pharmaceutical formulation. An efficient experimental design based on systematic scouting of all three key components of the RP‐HPLC method (Buffer pH, Organic Phase-% acetonitrile, Organic Modifier-Methanol) is presented. The significance and interaction effects of these parameters on the response variables (Retention time and tailing factor) were evaluated through statistical analysis tools like Analysis of Variance (ANOVA) and plots which revealed the final chromatographic conditions of the method. The developed method was validated and Forced degradation studies were also carried out in order to determine the stability-indicating nature of the method. The chromatographic separation was achieved on Jasco CrestPack RP C18 (250 × 4.6 mm, 5μ) column using Buffer (pH 6): Acetonitrile: Methanol (70:10:20 v/v) as mobile phase and detection was done using Photo-Diode Array (PDA) detector at 210 nm. The developed method of Vildagliptin is linear over a range of 5-15μg/ml having correlation coefficient R2 value as 0.999. The %RSD for precision and accuracy of the method was found to be less than 2%. Forced Degradation studies revealed that the method was found to be stability-indicating. The results showed that the proposed method is suitable for the precise and accurate determination of Vildagliptin in bulk and its formulation.

scholarly journals STABILITY INDICATING RP-HPLC ASSAY METHOD FOR ESTIMATION OF DIMETHYL FUMARATE IN BULK AND CAPSULES

2017 ◽  
Vol 9 (5) ◽  
pp. 121 ◽  
Author(s):  
Hemant K. Jain ◽  
Archana A. Gunjal
Keyword(s):  
Dimethyl Fumarate ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies

Objective: To develop an accurate, simple, precise and specific stability indicating RP-HPLC method for estimation of dimethyl fumarate in bulk and capsules.Methods: An Inertsil ODS (150x4.6 mm, 5µ) column and a mobile phase containing acetonitrile: potassium dihydrogen phosphate buffer pH 6.8 (50:50% v/v) was used for this study. The flow rate was maintained at 1.0 ml/min; column temperature was fixed at 35 °C and UV detection was carried out at 210 nm. The forced degradation studies were performed and method was validated with as per ICH guidelines.Results: The retention time of dimethyl fumarate was found to be 3.3±0.02 min. The value of correlation coefficient between peak area and concentration was found to be 0.9993. The mean percent recovery of dimethyl fumarate in capsules was found in the range of 99.65 to 101.64%. The results of forced degradation studies indicated that the drug was found to be stable in basic, oxidative and thermal conditions while degraded in acidic conditions.Conclusion: It can be conducted from results that the developed HPLC method is simple, accurate, precise and specific. Results of stress testing study revealed that the method is stability indicating. Thus, this method can be used for routine analysis of dimethyl fumarate capsules and check their stability.  

scholarly journals RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANIOUS ESTIMATION AND FORCED DEGRADATION STUDIES OF LAMIVUDINE AND RALTEGRAVIR IN SOLID DOSAGE FORM

2018 ◽  
Vol 10 (6) ◽  
pp. 242
Author(s):  
Juluri Krishna Dutta Tejaswi ◽  
R. Govinda Rajan
Keyword(s):  
Correlation Coefficient ◽  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies

Objective: A stability indicating reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the estimation of the combined tablet formulation of lamivudine (LAM) and raltegravir (RAL) in dosage forms and its API.Methods: Chromatographic separation was achieved on inertsil ODS C18 5 µm (4.6 X 150 mm) using a mobile phase (MP) consisting of a mixture of mixed orthophosphoric acid (OPA): acetonitrile (ACN) in the ratio 50:50 v/v which was determined at 242 nm respectively. Results: The assay of LAM and RAL was performed with tablets, and the % assay was found to be 100.12 and 99.89 which shows that the method is useful for routine analysis. The linearity of LAM and RAL was found to be linear with a correlation coefficient of 0.998 and 0.999, which shows that the method is capable of producing good sensitivity. The retention time of LAM and RAL was 1.99 min and 4.34 min respectively; linearity range was found to lie from 15 µg/ml to 75 µg/ml for LAM, 30 µg/ml to 150 µg/ml for RAL with a correlation coefficient of 0.999 respectively. Forced degradation studies were conducted in acidic, basic, thermal, photolytic and peroxide where all the degradation peaks were monitored.Conclusion: The proposed HPLC method was found to be simple, specific, precise, accurate, rapid and economical for simultaneous estimation of LAM and RAL in bulk and tablet dosage form. Thus the validated economical method was applied for forced degradation study of LAM and RAL tablet.

scholarly journals Stability Indicating RP-HPLC Method Development and Validation for Dexamethasone

2020 ◽  
Vol 32 (3) ◽  
pp. 587-591
Author(s):  
Pankaj N. Kulkarni ◽  
C.K. Jadhav ◽  
A.S. Nipate ◽  
Alaknanda M. Dodake-Supekar ◽  
C.H. Gill
Keyword(s):  
Method Development ◽  
Reversed Phase ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Phase Water ◽  
Hplc Method Development ◽  
Development And Validation

A new, simple, reliable and reproducible stability indicating RP-HPLC assay method has been developed for quantitative analysis of dexamethasone from dexamethasone tablets. This developed method has been validated according to ICH guideline with respect to system suitability, specificity, precision, linearity, accuracy and robustness. An isocratic condition of mobile phase water (0.1% orthophosphoric acid):acetonitrile in a ratio of 60:40, v/v at a flow rate of 1.0 mL/minute over RP 2.5 Fortis C18, 100 × 4.6 mm, 2.5 μm, column was at 27 ºC maintained. This method is specific and showed excellent linear response with correlation coefficient (R2) values of 0.999. In forced degradation, the proposed method has been investigated with different stress conditions as hydrolytic, oxidative, thermal and humid as recommended by ICH guidelines. An accurate and reliable reversed-phase HPLC method for the analysis of dexamethasone in dexamethasone tablets was developed and validated successfully.

scholarly journals FORMULATION DEVELOPMENT AND STABILITY INDICATING HPLC ASSAY OF TABLETS OF APIXABAN

2017 ◽  
Vol 9 (10) ◽  
pp. 24
Author(s):  
Hemant K. Jain ◽  
Vishal K. Nikam
Keyword(s):  
Immediate Release ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Direct Compression ◽  
Formulation Development ◽  
Disintegration Time ◽  
Stability Indicating ◽  
Forced Degradation Studies ◽  
Degradation Studies

Objective: Cost effective formulation development and stability indicating HPLC method for estimation of apixaban in bulk and tablets dosage form.Methods: 32 factorial design was applied to formulate the immediate release tablets of apixaban by using direct compression method. The chromatographic separation was performed on Purospher Star RP-18e (5 µm, 250x4, 6 mm) column and a stability indicating assay method was developed by using HPLC. The mobile phase consists of water: acetonitrile (60:40 v/v) was delivered at a flow rate of 1 ml/min and UV detection at 280 nm. The method was validated with forced degradation studies as per ICH guidelines.Results: Prepared batches were evaluated for all pre-compression parameters and post-compression parameters. Formulation batch F5 prepared by direct compression shows highest dissolution release of 90.97 % over the period of 60 min while disintegration time was found to be 136 seconds. The retention time of developed HPLC method was found to be 5.66 min. This method was found to be linear in a concentration range of 5-30 μg/ml of the drug (r2= 0.999). The low value of % RSD in the precision study indicates reproducibility of the method. The low value of LOD and LOQ suggests the sensitivity of the method. The results of forced degradation studies indicated that the drug was less stable in thermal and photolytic condition and degraded in acidic, basic, oxidative conditions.Conclusion: On the basis of formulation evaluation, batch F5 was found to be promising formulation suitable for the immediate release of apixaban. Results obtained by validation studies suggested that the developed stability indicating assay method is simple, accurate, specific, sensitive and precise. Thus, this method can be used for routine analysis of apixaban formulation and to check the stability testing. 

scholarly journals STABILITY INDICATING RP-HPLC ASSAY METHOD FOR ESTIMATION OF MIDODRINE HYDROCHLORIDE IN BULK AND TABLETS

2016 ◽  
Vol 8 (9) ◽  
pp. 283 ◽  
Author(s):  
Hemant K. Jain ◽  
Kishor N. Gujar ◽  
Varsha A. Randhe
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Assay Method ◽  
Forced Degradation ◽  
Hplc Assay ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies ◽  
The Stability

<p><strong>Objective: </strong>To develop an accurate, simple, sensitive and precise stability indicating reverse phase-high performance liquid chromatographic (RP-HPLC) assay method for estimation of Midodrine hydrochloride (MD) in bulk and tablets.</p><p><strong>Methods: </strong>The chromatographic separation was performed on enable C<sub>18</sub>, (250 mm X 4.6 mm, 5 μm) column. The mobile phase consists of triethylamine buffer 0.02%, pH-3: acetonitrile (38:62 v/v) was delivered at a flow rate of 0.6 ml/min and UV detection at 289 nm. The method was validated with forced degradation studies as per ICH guidelines.</p><p><strong>Results: </strong>The retention time of the drug was found to be 3.56 min. The developed method was found to be linear in a concentration range of 19.98-99.9μg/ml of the drug (r<sup>2</sup>= 0.9998). The low value of % RSD indicates reproducibility of the method. The low value of LOD and LOQ suggests the sensitivity of the method. The results of forced degradation studies indicated that the drug was stable in acidic condition and degraded in basic, oxidative and hydrolytic conditions.</p><strong>Conclusion: </strong>The present study represents first stability-indicating HPLC assay method that deals with the estimation of midodrine hydrochloride. It can be concluded from the results that the developed method is simple, rapid, accurate, specific, sensitive and precise. Thus, this method can be used for routine analysis of midodrine hydrochloride formulation and to check the stability of bulk samples.<p> </p>

Forced Degradation Studies of Sofosbuvir with a Developed and Validated RP-HPLC Method as per ICH Guidelines

2021 ◽  
Author(s):  
Abderrazaq Hamdache ◽  
Lamia Grib ◽  
Celia Grib ◽  
Lydia Adour ◽  
Hakim Zatout ◽  
...  
Keyword(s):  
Hplc Method ◽  
Forced Degradation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Forced Degradation Studies ◽  
Degradation Studies
Sign in / Sign up

Export Citation Format

Share Document