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.

Method Development and Validation of Spectrophotometric Methods for The Estimation of Rizatriptan Benzoate in Pure and Pharmaceutical Dosage Form

2021 ◽  
pp. 6003-6006
Author(s):  
Pushpa Latha E. ◽  
Sailaja B.
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rizatriptan Benzoate ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

Analytical UV derivative spectrophotometric method was developed and validated to quantify Rizatriptan Benzoate in pure drug and tablet dosage form. Based on the spectrophotometric characteristics of Rizatriptan Benzoate, a signal of zero (225nm), first (216nm), second (237nm), third (233nm), fourth (231nm) order derivative spectra were found to be adequate for quantification. The methods obeyed Beer's law in the concentration range of (0.1-360µg/ml) with square correlation coefficient (r2) of 0.999. The mean percentage recovery was found to be 100.01 ± 0.075. As per ICH guidelines the results of the analysis were validated in terms of linearity, precision, accuracy, limit of detection and limit of quantification, and were found to be satisfactory.

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.

Quantification and Stability Indicating UPLC Method Development and Validation of Acalabrutinib in Bulk and Pharmaceutical Dosage Form

2021 ◽  
Vol 11 (5) ◽  
Author(s):  
V Mohan Goud ◽  
N Pooja Singh
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Dosage Form ◽  
Method Development ◽  
Theoretical Plate ◽  
Lymphocytic Leukemia ◽  
Plate Count ◽  
Pharmaceutical Dosage Form ◽  
Method Development And Validation ◽  
Development And Validation

Acalabrutinib (ABN) is a Bruton tyrosine kinase inhibitor used to treat mantle cell lymphoma, chronic lymphocytic leukemia and small lymphocytic lymphoma. It has been used in the treatment of Hodgkin lymphoma, multiple myeloma and ovarian cancer. It is available in capsule dosage form, usually prescribed twice a day. The objective of the present study describes the ultra-performance liquid chromatography (UPLC) method development and validation for the estimation of the ABN in Capsule dosage form by following ICH guidelines because no methods were reported in this category. The column and Mobile phase were selected based on trial and error methods. For the estimation, the chromatogram BEH C18 (50 mm x 2.1 mm, 1.7µm) column was run through with Mobile phase 0.01N KH2PO4 : Methanol in the ratio of 50:50 at a flow rate of 0.3 ml/min. Temperature was maintained at 30°C. Optimized wavelength selected for the separation was 234nm. Retention time was achieved 1.148minute in optimized chromatogram. Theoretical plate count and tailing factor were obtained “as per recommendations of ICH limits”. The % RSD precision obtained was 0.7% and Intermediate precision obtained was 0.7% as the limit of Precision was less than 2. %Recovery obtained for marketed formulation was 99.23%. LOD, LOQ values obtained from the regression equation (y=9128.5x + 14854) of ABN were 0.18µg/ml and 0.55µg/ml respectively. Proposed method was linear over the concentration range25-150µg/ml. Different degradation studies (acid, alkali, oxidation, thermal, UV, water) were performed and all these samples passed the limits of degradation. Retention time and run time was decreased, so the method developed was simple and economical that can be adopted in regular quality control tests in Industries.

scholarly journals Analytical Method Development and Validation and Forced Degradation Stability-Indicating Studies of Favipiravir by RP-HPLC and UV in Bulk and Pharmaceutical Dosage Form

2021 ◽  
pp. 254-271
Author(s):  
Sayyed Nazifa Sabir Ali ◽  
Lajporiya Mobina ◽  
Manjra Mehfuza ◽  
Patel Seema ◽  
Aejaz Ahmed ◽  
...  
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Development And Validation

Aims: To develop and validate a new, simple, rapid, precise, and accurate An Eco-friendly RP-HPLC and UV-Method Development and Validation for an estimation of Favipiravir in Bulk and pharmaceutical dosage form followed by Forced Degradation Studies. Study Design: This was employed for UV-visible (200-400 nm and 400-800 nm respectively) and RP-HPLC method development using C 18 inertsil column and optimization of variables for Favipiravir estimation in bulk and formulations. Place and Duration of the Study: The present work was carried out at Ali-allana College of Pharmacy, Akkalkuwa between the duration of November-2020 to February-2021. Methodology: UV-Spectroscopic method was developed for the estimation of Favipiravir in the bulk and pharmaceutical dosage form. The solvent selected for the Favipiravir UV analysis was water, the solution in a range of 2-10µg/ml was scanned in the UV region from 200-400 nm and the λmax value was determined. The RP-HPLC method was developed on inertsil ODS-3V C18 150 mm x 4.6mm x 5μ column using buffer pH 3.5: acetonitrile [90:10] as mobile phase at flow rate 1.0 ml/min and PDA detection at 358 nm. Results: The maximum absorbance was observed at 358 nm. The wavelength 358 nm was selected for further analysis of Favipiravir. The calibration curve was determined using drug concentrations ranging from 2-10 µg/ml. The % recovery for accuracy was 100.50-100.76%. The method was to be precise with a % RSD value 0.51-1.37 and 0.77-1.78 for intraday and Interday respectively. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 0.0723 &0.219 µg/ml respectively by UV method. The RP-HPLC method was shown to be linear in the 50-250 μg/ml concentration range. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 2.186 & 6.626 μg/ml respectively. The method was to be precise with a % RSD value 0.25-1.53 and 0.86-1.68 for intraday and inter-day respectively. Conclusion: Here we conclude that the developed UV and RP-HPLC methods are precise, accurate, sensitive, and reproducible for the quantitative estimation of Favipiravir bulk and its formulation. The developed method can be used by the pharmaceutical industries for the routine analysis of Favipiravir, in particular by UV and RP-HPLC. The main features of the proposed method are economic and eco-friendly with less retention time around 5.0 min.

scholarly journals Analytical Method Development and Validation for Estimation of Mifepristone in Pure and Pharmaceutical Dosage Form

2021 ◽  
pp. 120-130
Author(s):  
Sheetal Bastia ◽  
Vaibhav Gawade ◽  
Vitthal Chopade ◽  
Rahul Jagtap ◽  
Vishal Modi
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Development And Validation ◽  
High Degree ◽  
Tablet Dosage

Mifepristone structurally belongs to the class of anti-progesterone steroids, which are used as an oral contraceptive. The reverse phase HPLC method was designed in a simplified and rapid way for the estimation of Mifepristone in bulk as well as tablets. The method was established using a Kromasil C18 column of dimensions of 250mm×4.6mm and a particle size of 5m.The used mobile phase was Acetonitrile: Water (70:30, v/v). The pump was pumped at 1 ml/min at a temperature of about 30 ± 2 °C and the eluted analyte was identified at 305 nm. Mifepristone eluted with a mean retention time of 6.27 minutes. The intended method was validated as per ICH (International Council for Harmonisation) guidelines, indicating a high degree of specificity, system suitability, accuracy, precision, and robustness. The LOD (Limit of detection) was found to be 0.7238 ppm and the limit of measurement was 0.9562 ppm. The method linearity was found to be between 1-6µg/ml, with an R2 of 0.9923. In accuracy studies, the percent recovery was found to be between 99.39% - 100.50%. The method was discovered to be precise as the values of the percent RSD were found to be less than 2.0% for both intraday and interday. The method was discovered to be reliable and robust. Mifepristone in marketed pharmaceutical tablet dosage form was effectively quantified using the established Reverse Phase HPLC method.

scholarly journals A novel high performance liquid chromatography method development and validation of fluconazole by ezchrom software

2020 ◽  
Vol 11 (2) ◽  
pp. 2399-2409
Author(s):  
Vikrant Verma ◽  
Manish Pathak ◽  
Amit Kumar ◽  
Amit Kumar
Keyword(s):  
Standard Deviation ◽  
Mobile Phase ◽  
Method Development ◽  
Limit Of Detection ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation

The current research explains the development of a new method and its subsequent validation by a novel HPLC method in fluconazole tablets. Inertsil Octadecyl silica C18 column having dimensions of length 150 mm, diameter 4.6 mm, particle size 5 μm was exploited for the method development, and the mobile phase embodies buffer pH 4 and acetonitrile in the combo of 40:60. Wavelength exploited for the segregation was 289 nm. The volume of injection was preserved at 20 µl. The new developed method has been established to demonstrate linearity in the range of 10 to 30 µg /ml correspondingly. Average recovery established to be 101.571, 100.315, and 99.021, the standard deviation was established to be 0.93834, 0.986418, and 0.989741, and % R.S.D was established to be 0.92382, 0.98331, and 0.999526. The percentage recovery was established to be within prescribed restrictions. The limit of detection was established to be 0.0080. The limit of quantitation was established to be 0.0051. In assay studies, an average assay was found to be 95.966, and standard deviation and % RSD of the assay was found to be 0.6021  and  0.6274, respectively. The method was found to be specific as there was no intrusion from impurities and excipients. Extensive diversity of mobile phase combos was utilized for the research and flow rate preserved at 1.3 ml/min all through the process. After carefull and systemic investigation of various research articles and review articles, it is observed that H.P.L.C method development and validation of fluconazole has been done in various pharmaceutical dosage forms, but till now a smaller amount of work is executed on dosage forms of solid nature, and hence there is huge prospective for research to be done in this area for new methodology to be developed in pharmaceutical dosage form of solid nature by means of dissimilar mobile phase combos and different strategy adopted by use of chromatography software which avoids the problems and demerits associated with present methods

RP-HPLC Method Development and Validation for the Estimation of Sacubitril and Valsartan in Pharmaceutical Dosage Form

2021 ◽  
pp. 5797-5802
Author(s):  
G.M. Kadam ◽  
A.L. Puyad ◽  
T.M. Kalyankar
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Content Uniformity ◽  
Phase Detection ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Hplc Method Development

A new, economical, simple, accurate, and precise RP-HPLC method was developed for simultaneous assay and content uniformity determination of Sacubitril and Valsartan in bulk and pharmaceutical dosage form. The separation of Sacubitril and Valsartan was achieved within 6 minutes on Phenomenex Luna C18 250 mm x 4.6mm and 5µm Particle Size, column using Acetonitrile: Methanol: Water (30:55:15% v/v/v) as the mobile phase. Detection was carried out at 250 nm wavelength. The retention time of Sacubitril and Valsartan was found to be 2.361 and 3.304 min, respectively. The validation of the developed method was performed in terms of specificity, accuracy, precision, linearity, the limit of detection, the limit of quantification as mentioned in International Conference on Harmonization (ICH) guidelines. The method showed adequate sensitivity concerning linearity, accuracy, and precision over the range 12-36 μg/ml and 13-39 μg/ml for Sacubitril and Valsartan, respectively. The percentage recoveries obtained for Sacubitril and Valsartan were found to be in the range of 98.00 – 102.00 %. The proposed method is suitable for use in quality-control laboratories for quantitative analysis.

scholarly journals UPLC Method Development and Validation for the Determination of Chlophedianol Hydrochloride in Syrup Dosage Form

2017 ◽  
Vol 2 (02) ◽  
pp. 25-31
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Calibration Plot ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation

A specific, precise, accurate ultra pressure liquid chromatography (UPLC) method is developed for estimation of chlophedianol hydrochloride in bulk drug and syrup dosage form. The method employed with Hypersil BDS C18 (100 mm x 2.1 mm, 1.7 μm) in a gradient mode, with mobile phase of methanol and acetonitrile in the ratio of 65:35 %v/v. The flow rate was 0.1 ml/min and effluent was monitored at 254 nm. Retention time was found to be 1.130±0.005 min. The method was validated in terms of linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ)in accordance with ICH guidelines. Linear regression analysis data for the calibration plot showed that there was good linear relationship between response and concentration in the range of 20-100 μg/ml respectively. The LOD and LOQ values were found to be 2.094(μg/ml)and 6.3466(μg/ml)respectively. No chromatographic interference from syrup excipients and degradants were found. The proposed method was successfully used for estimation of chlophedianol hydrochloride in syrup dosage form.

Sign in / Sign up

Export Citation Format

Share Document