RP-HPLC Method Development and Validation for the Determination of Pemigatinib using Design of Experiments Approach

Aim: To develop and validate a simple, precise, accurate and robust RP-HPLC method for the determination of Pemigatinib by using Design of Experiments (DoE) approach. Study Design: A 23 Factorial design consisting of three factors at two levels was considered for the experimental plan initially to select the initial chromatographic conditions and optimization was done using Box-Behnken Design. The critical method parameters selected for optimization were % Organic phase composition, pH of the buffer and flow rate. The critical quality attributes investigated were retention time, theoretical plates and tailing factor. Methodology: Chromatographic separation was achieved on Agilent Zorbax XDB C18 (250×4.6 mm, 5 µm) column maintained at ambient temperature and PDA-UV detection set at 262nm. The optimized and predicted data from the Design Expert® (12.0.12.0) modelling software (Stat-Ease Inc., Minneapolis, MN, USA) consisted of mobile phase 0.1% OPA pH 2.5 buffer (60%): Acetonitrile (40%) pumped at a flow rate of 1.06ml/min gave the highest desirability. Results: The retention time of the drug was found to be 3.258 min. The developed method was linear over the concentration range of 25-150 µg/mL with correlation coefficient of 0.999. The optimized method was validated as per ICH Q2 (R1) guidelines. Conclusion: Based on the ANOVA results, the selected models for the responses retention time and tailing factor were found to be significant with P=0.05. 2D Contour plots were used to visualize the effect of factors and their interactions on the responses. Design validation was done using predicted vs. actual plots for the responses. The results of the validation parameters were within the acceptable limit. The stability of the drug was examined under different stress conditions forcibly and significant degradation was found in reductive condition.

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RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

E-Journal of Chemistry ◽

10.1155/2006/713569 ◽

2006 ◽

Vol 3 (1) ◽

pp. 60-64 ◽

Cited By ~ 6

Author(s):

P. Venkata Reddy ◽

B. Sudha Rani ◽

G. Srinu Babu ◽

J. V. L. N. Seshagiri Rao

Keyword(s):

Flow Rate ◽

Retention Time ◽

Mobile Phase ◽

Dosage Forms ◽

Hplc Method ◽

Reverse Phase Hplc ◽

Reverse Phase ◽

Pharmaceutical Dosage Forms ◽

Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

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APPLICATION OF VALIDATED RP-HPLC METHOD FOR THE DETERMINATION OF ARMODAFINIL IN BULK AND FORMULATION

International Journal of Current Pharmaceutical Research ◽

10.22159/ijcpr.2017v9i5.22162 ◽

2017 ◽

pp. 158-161

Author(s):

Devi Ramesh ◽

Mohammad Habibuddin

Keyword(s):

Retention Time ◽

Mobile Phase ◽

Hplc Method ◽

Reverse Phase Hplc ◽

Reverse Phase ◽

Rp Hplc ◽

Ich Guidelines ◽

Validation Parameters ◽

Isocratic Mode

Objective: The objective of the present study is to develop and validate a simple, rapid, sensitive reverse phase HPLC method for the determination of Armodafinil present in bulk and its pharmaceutical formulations.Methods: The chromatographic separation was achieved by using Hypersil ODS C-18 (150 x 4.6 mm, 5Âµ) in an isocratic mode with mobile phase methanol: phosphate buffer 3.0 (60:40 %v/v) was used. The flow rate was 1 ml/min and effluent was monitored at 225 nm. The method was validated for validation parameters i.e. linearity, accuracy, precision and robustness according to ICH guidelines.Results: The retention time of Armodafinil was 4.2 min and the linearity range of the method was 500-20000ng/ml with regression (r2) coefficient 0.9998. The method was validated for precision, accuracy, robustness and which were found to be within the acceptable limits according to the ICH guidelines. Also, the method was successfully applied for the estimation of Armodafinil in the marketed formulation of Nuvigil and the recovery was found to be>98%.Conclusion: The developed method possess good selectivity, specificity, there is no interference found in the blank at a retention time of ARM and good correlation between the peak area and concentration of the drugs under prescribed conditions. Hence, the method can be applied for routine analysis of Armodafinil.Â

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RP-HPLC Method Development and Validation for the Estimation of Lansoprazole in Presence of Related Substances by QbD Approach

Journal of Pharmaceutical Research International ◽

10.9734/jpri/2021/v33i36a31936 ◽

2021 ◽

pp. 138-150

Author(s):

Sachin B. Gholve ◽

Jaiprakash N. Sangshetti ◽

Omprakash G. Bhusnure ◽

Ram S. Sakhare ◽

Pratap H. Bhosale ◽

...

Keyword(s):

Flow Rate ◽

Mobile Phase ◽

Method Development ◽

Hplc Method ◽

Drug Substance ◽

Gastric Ulcers ◽

Mobile Phase Flow Rate ◽

Column Temperature ◽

Rp Hplc

A rapid specific RP-HPLC method has been developed for the determination of Lansoprazole impurities in the drug substance. The control of pharmaceutical impurities is currently a critical issue in the pharmaceutical industry. The International Council for Harmonization (ICH) has formulated a workable guideline regarding the control of impurities. The objective of the recent study was to develop and validate a HPLC method for the quantitative determination of process-related impurities of Lansoprazole in pharmaceutical drug substance. Lansoprazole, 2-[[[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridinyl] methyl]-sulfinyl]- 1H-benzimidazole is an proton pump inhibitor used in the management of gastric ulcers. Chromatographic identification of the impurities was carried out by response surface methodology, applying a three-level Box Behnken design with three center points. Three factors selected were a mobile phase, flow rate, column temperature. Evaluation of the main factor, their interaction, and the quadric effect on peak resolution were done on Waters Symmetry C8, 250 x 4.6mm, 5µm column is used for the development of the method. The mobile phase consists of buffer and acetonitrile. The flow rate of the mobile phase was 1.0 ml/min with gradient elution. The column temperature is ambient and the detection wavelength is 235 nm. The injection volume was 10 µL. The method was validated as per ICH guidelines for linearity in the range of 50-150 µg/ml and the LOD & LOQ values obtained were 0.437×10-4 and 0.1325×10-3 µg/ml respectively which specifies the method's sensitivity. The proposed method was successfully used to determine the Lansoprazole impurities in drug substances.

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Method Development and Validation of Degradation Studies of Lenalidomide by RP-HPLC

Research Journal of Pharmacy and Technology ◽

10.52711/0974-360x.2021.00744 ◽

2021 ◽

pp. 4281-4286

Author(s):

Punna Venkateshwarlu ◽

Mehul M. Patel

Keyword(s):

Retention Time ◽

Mobile Phase ◽

Method Development ◽

Hplc Method ◽

Mobile Phase Flow Rate ◽

Pharmaceutical Dosage Forms ◽

Rp Hplc ◽

System Suitability ◽

Wide Range

A simple, accurate, RP HPLC method was developed by this study determination of lenalidomide. This method is developed by Shimadzu LC -2010 HT by using C18 (250 X 4.6 X mm X 5µ) column in solvents Phosphate buffer: Acetonitrile (55:45) v/v as mobile phase and the temperature was maintained at 25°C. The mobile phase flow rate 1ml/min was pumped and sample wavelength was detected at 242nm by ultraviolet -visible spectrophotometer. The retention time was found 2.5 min. The number of theoretical plates and tailing factor for lenalidomide was observed 16199.817 (NLT 2000) and 1.128 (NMT 2). The method was validated for analytical standards such as linearity, accuracy, precision, system suitability and robustness. LOD and LOQ values obtained from regression of lenalidomide 0.058 and 0.174µg/ml. The regression equation of validated method for lenalidomide is Y=5223x+183075. In wide range of 25 to 150 (µg/ml) the linearity was observed. The method was validated and a recovery study indicates accuracy of this method. The Retention time less compared to established methods. The method was validated by determining its accuracy, precision and system suitability. The results of the study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate, which is useful for the routine determination of Lenalidomide in bulk drug and in its pharmaceutical dosage forms.

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ANALYTICAL QUALITY BY DESIGN APPROACH IN RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF DUVELISIB

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2021.v14i2.40181 ◽

2021 ◽

pp. 99-108

Author(s):

SRUJANI CH ◽

ANNAPURNA P ◽

NATARAJ KS ◽

KRISHNA MANJARI PAWAR A

Keyword(s):

Flow Rate ◽

Retention Time ◽

Quality By Design ◽

Hplc Method ◽

Design Approach ◽

Analytical Quality ◽

Column Temperature ◽

Rp Hplc ◽

Validation Parameters ◽

Quality By Design Approach

Objective: A simple, accurate, and robust RP-HPLC method was developed and validated for the estimation of Duvelisib using analytical quality by design approach. Methods: The critical method parameters (CMP) were systematically optimized using box-Behnken design (BBD). The CMP’s selected were % organic phase composition, column temperature, and flow rate. The critical quality attributes investigated were retention time and theoretical plates. Results: Chromatographic separation was accomplished on Agilent Zorbax Eclipse C18 (150×4.6 mm, 5 μm) column. The optimized and predicted data from Design Expert software consist of mobile phase 0.1 % orthophosphoric acid (46.3%): Acetonitrile (53.7%), pumped at a flow rate of 0.91 ml/min at 32.6°C gave the highest desirability function of 1. The retention time of the drug was found to be 2.85 min. The developed method was validated as per the ICH Q2 (R1) guidelines. Conclusion: Based on the analysis of variance values, the selected models were found to be significant with p<0.05. The results of the validation parameters were within the acceptable limit. The stability of the drug was examined under different stress conditions forcibly and significant degradation was found in acidic condition.

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Development and validation of a fast and simple RP-HPLC method for the determination of diosmin and hesperidin in combined tablet dosage form

Macedonian Journal of Chemistry and Chemical Engineering ◽

10.20450/mjcce.2018.1448 ◽

2018 ◽

Vol 37 (2) ◽

Cited By ~ 1

Author(s):

Marjan Piponski ◽

Tanja Bakovska Stoimenova ◽

Marina Topkoska ◽

Stefan Stefov ◽

Magdalena Piponska ◽

...

Keyword(s):

Retention Time ◽

Reversed Phase ◽

Hplc Method ◽

Uv Detector ◽

Rp Hplc ◽

Validation Parameters ◽

Time Cycle ◽

Development And Validation ◽

Tablet Dosage

A fast, simple, accurate and robust reversed phase HPLC method for the simultaneous determination of two flavonoids, hesperidin and diosmin, in combined tablets was developed and validated. This method uses a short C8 column with dimensions of 75 mm × 4 mm with 5 µm particles thermostated at 30 °C, and a mobile phase composed of formic acid (pH 4.1 and 0.05%, V/V) and methanol (58:42, V/V), delivered at a flow rate of 1.2 ml/min, with UV detector signal monitoring at 280 nm and an injection volume of 5 µl. These chromatographic conditions yielded chromatograms with symmetric peaks of hesperidin, eluting at a ~2 min retention time, and diosmin, at a ~4.5 min retention time, with a total run time cycle of 6 min. The method validation parameters confirmed excellent values for accuracy, linearity and reproducibility. This method is suitable for routine analysis in pharmaceutical and food quality control laboratories.

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Application of Elements of Quality by Design to Development and Optimization of HPLC Method for Fingolimod

Journal of Pharmaceutical Research International ◽

10.9734/jpri/2021/v33i46a32872 ◽

2021 ◽

pp. 318-328

Author(s):

Siddique Akber Ansari ◽

Mrinmayee Deshpande ◽

Jaiprakash N. Sangshetti ◽

Sarfaraz Ahmed ◽

Irfan Aamer Ansari

Keyword(s):

Flow Rate ◽

Mobile Phase ◽

Method Development ◽

Quality By Design ◽

Hplc Method ◽

Contour Plots ◽

Target Profile ◽

Quality By Design Approach ◽

Actual Response

Purpose: A HPLC method for Fingolimod was developed using a Quality by Design concept. QbD has gained importance in recent times due to regulatory requirements. Actual study was started after determination of target profile and qualification of instrument. Methods: Separation was carried on a Grace C-8 column (4.6 x 250 mm, 5-μm particle size).The composition of mobile phase was methanol and 20 mM ammonium formate buffer of pH5.8 in gradient mode HPLC method development is affected by critical factors like pH, flow rate and mobile phase composition. Results: To study the effects of these three factors on USP tailing, Box Behnken optimization model was applied. Desirability of the model was set at Tailing less than 1.2.Analysis of results was done using surface diagrams. Verification of Software generated results was done by taking six replicates of the run. Thus developed and optimised method was Finally validated as per ICH guideline. Conclusion: A Quality by Design approach has been successfully utilised in method development of the Fingolimod in bulk. All key aspect of QbD were tried to be implemented in said study. Systematic approach was utilized for method development which includes beginning with determination of target profile characteristics, instrument qualification, risk assessment, design of experiment and validation. Three factors i.e. Ph, flow rate and methanol concentration were analysed for their effect on USP tailing as a responce. Interaction and quadratic effect of the factors were studied with least possible runs by using Box Behnken model. Response surface diagrams and contour plots were studied for coming to conclusion which factors are affecting response and their limits were recorded. Optimum run condition was obtained; Replicates of run having optimized condition were taken to confirm the predicted response with actual response.

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