scholarly journals Development and validation of RP-HPLC method for estimation of brexpiprazole in its bulk and tablet dosage form using Quality by Design approach

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Amol S. Jagdale ◽  
Nilesh S. Pendbhaje ◽  
Rupali V. Nirmal ◽  
Poonam M. Bachhav ◽  
Dayandeo B. Sumbre
Keyword(s):  
Flow Rate ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Control Analysis ◽  
Uv Detector ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Quality By Design Approach ◽  
Bulk Drug

Abstract Background A new, sensitive, suitable, clear, accurate, and robust reversed-phase high-performance liquid chromatography (RP-HPLC) method for the determination of brexpiprazole in bulk drug and tablet formulation was developed and validated in this research. Surface methodology was used to optimize the data, with a three-level Box-Behnken design. Methanol concentration in the mobile phase, flow rate, and pH were chosen as the three variables. The separation was performed using an HPLC method with a UV detector and Openlab EZchrom program, as well as a Water spherisorb C18 column (100 mm × 4.6; 5m). Acetonitrile was pumped at a flow rate of 1.0 mL/min with a 10 mM phosphate buffer balanced to a pH of 2.50.05 by diluted OPA (65:35% v/v) and detected at 216 nm. Result The developed RP-HPLC method yielded a suitable retention time for brexpiprazole of 4.22 min, which was optimized using the Design Expert-12 software. The linearity of the established method was verified with a correlation coefficient (r2) of 0.999 over the concentration range of 5.05–75.75 g/mL. For API and formulation, the percent assay was 99.46% and 100.91%, respectively. The percentage RSD for the method’s precision was found to be less than 2.0%. The percentage recoveries were discovered to be between 99.38 and 101.07%. 0.64 μg/mL and 1.95 μg/mL were found to be the LOD and LOQ, respectively. Conclusion The developed and validated RP-HPLC system takes less time and can be used in the industry for routine quality control/analysis of bulk drug and marketed brexpiprazole products. Graphical abstract

VALIDATED RP-HPLC METHOD FOR DETERMINATION OF ENZALUTAMIDE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (11) ◽  
pp. 46-50
Author(s):  
Z. G Khan ◽  
◽  
S. S. Patil ◽  
P. K. Deshmukh ◽  
P. O. Patil
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detector ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Bulk Drug

Novel, isocratic reversed phase high performance liquid chromatography method was developed and validated for the determination of enzalutamide (EZA) in bulk drug and pharmaceutical formulation. Efficient separation was achieved on PrincetonSPHER C18 100A, 5μ (250×4.6 mm) under the isocratic mode of elution using acetonitrile: water (80:20) % V/V as a mobile phase pumped in to the column at flow rate 1.0 mL/min. The effluent was monitored at 237.0 nm using UV detector. EZA was eluted in the given mobile phase at retention time (tR) of 3.2 minutes. The standard calibration curve was linear over the concentration range 10 - 60 μg/mL with correlation coefficient 0.997. The method was validated for accuracy, precision, sensitivity, robustness, ruggedness and all the resulting data treated statistically. The system suitability parameters like retention time, theoretical plates, tailing factor, capacity factor were found within the limit.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR ESTIMATION OF EDOXABAN TOSYLATE IN TABLET DOSAGE FORMS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (07) ◽  
pp. 47-51
Author(s):  
B. Anupama ◽  
P. Tejaswi ◽  
KNV. Chenchu Lakshmi ◽  
A. Vishwanadh
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Control Analysis ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Isocratic Mode

A rapid, simple and precise reversed phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of edoxabantosylate in tablets. The quantification was carried out using a Phenomenex C-18 column (250×4.6 mm i.d., 5µm particle size) in isocratic mode with mobile phase comprising of ammonium acetate buffer andacetonitrile in the ratio of 50:50 (V/V) at a flow rate 1 mL/min. The eluent was monitored at 240 nm. The retention time of the drug was 3.486 min. The calibration curve was linear in the concentration range of 5-25 µg/mL and per cent recovery ranged from 98.25-101.6.The developed method was validated as per ICH guidelines and the results obtained were satisfactory.The method can be applied for routine quality control analysis of edoxabantosylate in tablet dosage forms.

DEVELOPMENT AND VALIDATION OF NEW RP-HPLC METHOD FOR QUANTITATIVE ESTIMATION OF VITAMIN-D3 IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (06) ◽  
pp. 40-45
Author(s):  
T Mohan ◽  
◽  
S Prabhakara ◽  
K Anbazhagan ◽  
Krishnan Pavithra ◽  
...  
Keyword(s):  
Vitamin D3 ◽  
Dosage Form ◽  
Quantitative Estimation ◽  
Hplc Method ◽  
Control Analysis ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Bulk Drug

An accurate, simple, rapid, sensitive and cost effective method for the determination of Vitamin-D3 in pharmaceutical dosage form was developed and validated by RP-HPLC method. Chromatographic separation was achieved on phenomenex C18 column (150 mm X 4.6 mm, 5μm) using methanol: acetonitrile: water (90:5:5 V/V/V) as mobile phase, at a flow rate of 1.5 mL/min. The retention time of Vitamin-D3 was found to be 8.3 minutes; the detection was monitored at 265 nm by using UV detector. The developed method was validated according to International Conference on Harmonization (ICH) guidelines. The linearity of Vitamin-D3 was in the range of 2.50 ppm to 6.00 ppm. This method showed an excellent linear response with the correlation coefficient (R2) value of 0.999 for the Vitamin-D3. The recovery of the drug ranged from 99.59% to 103.83% with an average of 101.34%. The percentage RSD was found to be less than two, indicating high degree of accuracy and precision of the proposed RPHPLC method. Due to simplicity, cost effectiveness, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis of Vitamin-D3 in bulk drug and pharmaceutical dosage forms.

scholarly journals Development and Validation of a Simple RP-HPLC Method for Determination of Naproxen in Pharmaceutical Dosage Forms

2015 ◽  
Vol 16 (2) ◽  
pp. 137-141 ◽  
Author(s):  
Saleha Tanjin ◽  
Farhana Islam ◽  
Md Zakir Sultan ◽  
Asma Rahman ◽  
Sharmin Reza Chowdhury ◽  
...  
Keyword(s):  
High Performance ◽  
Pharmaceutical Formulations ◽  
Pharmaceutical Journal ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Uv Detector ◽  
Allowable Limit ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A simple, sensitive and precise reversed phase high performance liquid chromatographic (RP-HPLC) method has been developed for the estimation of naproxen in pharmaceutical dosage forms. The method was developed using the mobile phase comprising of dibasic sodium phosphate buffer (Na2HPO4) at pH 7.80 (adjusted by sodium hydroxide) and acetonitrile in the ratio of 70:30 (v/v) over C-18 column (250 x 4.6 mm, 5?m, Phenomenex Inc.) at ambient temperature. The flow rate was at 0.7 ml/min and the column washing was monitored by UV detector at 225 nm. The retention time of naproxen was 4.8 ± 0.1 min. The recovery was found to be >97% which is demonstrative of accuracy of the protocol. Inter-day and intra-day precision of the newly developed method were less than the maximum allowable limit (RSD% ? 2.0) according to ICH, USP and FDA guidelines. The method showed linear response with correlation coefficient (r2) value of 0.9991. Therefore, the method was found to be accurate, reproducible, sensitive and less time consuming and can be successfully applied for routine analysis of naproxen in pharmaceutical formulations. DOI: http://dx.doi.org/10.3329/bpj.v16i2.22295 Bangladesh Pharmaceutical Journal 16(2): 137-141, 2013

scholarly journals A SIMULTANEOUS ESTIMATION, VALIDATION AND FORCED DEGRADATION STUDIES OF 5-FLUOROURACIL AND TEGAFUR IN A PHARMACEUTICAL DOSAGE FORM USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD

2018 ◽  
Vol 11 (12) ◽  
pp. 132
Author(s):  
Vaishali Mistry ◽  
Akshay Yelwe ◽  
Amey Deshpande
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Uv Detector ◽  
Stability Indicating ◽  
Rp Hplc ◽  
The Stability

Objective: The present study describes the stability indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous estimation of 5-fluorouracil and tegafur in pharmaceutical dosage forms.Method: 5-fluorouracil and tegafur the propose RP-HPLC method were developed by using Shimadzu Prominence-i LC-2030 HPLC system equipped with UV detector and chromatographic separation was carried on shim-pack gist c18 (250 × 4.6 mm, 5 μ) column at a flow rate of 1 ml/min and the run time was 10 min. The mobile phase consisted of methanol and water in the ratio of 50:50% v/v and elements were scanned using a UV detector at 271 nm.Result: The retention time of 5-fluorouracil and tegafur was found to be 2.74 and 3.66 min, respectively. A linearity response was observed in the concentration range of 13.4 μg/ml–31.3 μg/ml for 5-fluorouracil and 6 μg/ml–14 μg/ml for tegafur, respectively. Limit of detection and limit of quantification of 5-fluorouracil were 10.97 μg/ml and 33.26 μg/ml and for tegafur are 4.89 μg/ml and 14.83 μg/ml, respectively.Conclusion: The stability indicating that the method was developed by subjecting drugs to stress conditions such as acid and base hydrolysis, oxidation, photo and thermal degradation, and degraded products formed were resolved successfully from samples.

scholarly journals RP-HPLC Determination of Atomoxetine Hydrochloride in Bulk and Pharmaceutical Formulations

2011 ◽  
Vol 8 (4) ◽  
pp. 1958-1964 ◽  
Author(s):  
H. R. Prajapati ◽  
P. N. Raveshiya ◽  
J. M. Prajapati
Keyword(s):  
Flow Rate ◽  
High Performance ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Liquid Chromatographic

A reversed phase high performance liquid chromatographic (RP–HPLC) method was developed and subsequently validated for the determination of atomoxetine hydrochloride in bulk and pharmaceutical formulation. The separation was done by a PerkinElmer Brownlee analytical C8 column (260 mm x 4.6 mm, 5 µm) using methanol: 50 mM KH2PO2buffer (PH adjusted to 6.8 with 0.1 M NaOH), 80:20 v/v as an eluent. UV detection was performed at 270 nm at a flow rate 1.0 mL/min. The validation of the method was performed, and specificity, reproducibility, precision accuracy and ruggedness were confirmed. The correlation coefficient was found to be 0.997 for atomoxetine hydrochloride. The recovery was in the range of 99.94 to 100.98% and limit of quantification was found to be 5.707 µg/mL. The method is simple, rapid, selective and economical too and can be used for the routine analysis of drug in pharmaceutical formulations.

scholarly journals ANALYTICAL QUALITY-BY-DESIGN (AQBD) APPROACH FOR THE DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF LAMOTRIGINE IN BULK AND TABLET FORMULATION

2021 ◽  
Vol 10 (5) ◽  
pp. 3591-3596
Author(s):  
Manisha P. Puranik
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Quality By Design ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Analytical Technique ◽  
Rp Hplc ◽  
Ich Guideline

The current analytical exploration illustrated developing a reversed-phase high-performance liquid chromatography (RP-HPLC) technique and consequent substantiation for analyzing lamotrigine (LAM) active pharmaceutical ingredient (API) using a Quality-by-design (QbD) approach (Central Composite Design), in bulk product as well as in the tablet formulations. In this experiment, based on systematic scouting, four key components (viz., mobile phase, column, flow-rate, and wavelength) were studied by the RP-HPLC method. 13 experimental runs were done with acetonitrile (ACN) (40-60% v/v) having flow-rate in the range 0.8 mL/min to 1.2 mL/min. The proposed analytical method was thoroughly corroborated in terms of ruggedness linearity, robustness, accuracy, and precision in accordance with ICH guideline Q2A and ICH guideline Q2B. Under the optimum chromatographic environment; Intersil C8 column of 250 mm length, 4.6 mm (i.d.); 20 μL injection volume; and mobile phase ACN: Methanol (60:40 v/v), a retention time of 2.542 min was noticed at 220 nm detection wavelength. The method was found to be extremely reproducible, accurate, linear, precise, robust, and economically adequate to execute the estimation. The intended analytical technique was thoroughly assessed through statistical tools and could be an imperative concern for the habitual scrutiny of LAM in bulk products and its formulation.

Development and Validation of a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) Method for Identification, Assay and Estimation of Related Substances of Ivermectin in Bulk Drug Batches of Ivermectin Drug Substance

2021 ◽  
Author(s):  
Daoli Zhao ◽  
Rasangi M Wimalasinghe ◽  
Lin Wang ◽  
Abu M Rustum
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Drug Substance ◽  
Related Impurities ◽  
Rp Hplc ◽  
Bulk Drug

Abstract A reversed-phase high-performance liquid chromatography (RP-HPLC) method has been developed and validated for the identification and assay of Ivermectin, including the identification and estimation of its process-related impurities and degradation products in bulk drug substance of Ivermectin. Analytes were separated on a HALO C18 column (100 mm × 4.6 mm I.D., 2.7 μm particle size) maintained at 40 °C (column temperature) with gradient elution. All analytes of interests were adequately separated within 25 min. All degradation products, process-related impurities and assay were monitored by ultraviolet detection at 254 nm. The new HPLC method described here successfully separated an isomer peak of the active pharmaceutical ingredient (API) from the major API peak. This newly separated isomer peak is around 1.2 to 1.5% (peak area) in typical API samples, and coelutes with the major API peak by all current HPLC methods. Quantitation limit of the HPLC method is 0.1% of target analytical concentration (~1.0 μg/mL). This method has been demonstrated to be accurate, robust, significantly higher degree of selectivity compared to the HPLC methods of Ivermectin drug substance reported in the literature and in the compendial HPLC methods prescribed in the current USA and European Pharmacopeia.

scholarly journals Development and Validation of a Reversed-Phase HPLC Method for the Estimation of Zolpidem in Bulk Drug and Tablets

2013 ◽  
Vol 2013 ◽  
pp. 1-6
Author(s):  
E. Konoz ◽  
A. H. Mohsen Sarrafi ◽  
R. Abdolahnejad ◽  
M. Bahrami-Zonoz
Keyword(s):  
High Performance ◽  
Dynamic Range ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Bulk Drug

In the present study an isocratic reversed-phase high-performance liquid chromatography method was developed for the estimation of zolpidem in bulk drug and pharmaceutical dosage forms. The quantification was carried out on C18columns. A mixture of acetonitrile-ammonium acetate (pH=8.0, 0.02 M) (60 : 40 v/v) was used as the mobile phase, at flow rate of 1.0 mL/min and the determination wavelength at 245 nm. The retention time of zolpidem was found to be 3–5 min. The validation of the proposed method was carried out for specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness. The linear dynamic range was from 2.5 to 30 μg mL−1. Regression equation was found to bey=0.1416x+0.0183with correlation coefficientr=0.9996. The percentage recovery obtained for zolpidem was greater than 96.5%. Limit of quantification and limit of detection were found to be 2.5 μg mL−1and 0.83 μg mL−1, respectively. The developed method can be used for routine quality control analysis of zolpidem in tablet formulations.

Development and Validation of Stability Indicating RP-HPLC Method For Estimation of Clofazimine in Soft Gelatine Capsule

2017 ◽  
Vol 8 (1) ◽  
Author(s):  
Patel H. A. ◽  
Patel K. G. ◽  
Pathak D. S. ◽  
Patel D. J. ◽  
Meshram D. B.
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Control Analysis ◽  
Uv Detector ◽  
Citrate Buffer ◽  
Chromatography Method ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Liquid Chromatography Method ◽  
Bulk Drug

Stability indicating reverse phase high performance liquid chromatography method was developed for the estimation of Clofazimine in bulk drug and soft gelatin capsules. The chromatographic separation was achieved on ODS C18 column using mobile phase comprising 10 mM citrate buffer : acetonitrile, in which pH of buffer is adjusted with 1N HCL solution in ratio of (70:30 v/v), flow rate was 1.0 ml/min and eluents were detected by UV detector at 283 nm. Retention time of Clofazimine was found to be 5.205 min. Linearity range was found over the concentration range 25-75 μg/ml. Clofazimine was subjected to various stress conditions i.e. Acid, Base, Oxidative, Thermal and Photolytic degradation. The degradation peak of formulation of Clofazimine were well resolved from the pure peak. The proposed method were validated according to the ICH guidelines and it can be suitable for quality control analysis of Clofazimine in soft gelatin capsule

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