scholarly journals Method Development and Validation of Quantitative Estimation of Vilazodone Hydrochloride by UV and RP-HPLC

2020 ◽  
Vol 13 (4) ◽  
pp. 362-373
Author(s):  
Gayathri Nallathambi ◽  
V Sekar ◽  
Surendra kumar.M
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Potassium Hydrogen ◽  
Method Development And Validation ◽  
Development And Validation ◽  
High Degree

The aim of the study is to develop some new analytical method development and Validation of Quantitative Estimation of Anti-depressant Drug Vilazodone by UV and HPLC was found to be simple, specific, precise, accurate, rapid and economical. The method was developed and validated as per ICH guidelines, concerning accuracy, precision, linearity, ruggedness, limit of detection, limit of quantification and robustness and forced degradation studies. The GRACE ODS phenyl column (4.6 x 150mm,5μm) column was maintained at an ambient temperature and 232 nm λ max conditions. The mixture of di-potassium hydrogen phosphate with buffer (pH 7.4) and methanol in proportion 60:40v/v mobile phase was used in the flow rate of 1 ml/min. All validation methods shows good reproducibility and good recovery. The mean recoveries was found in the range between 99.6-99.9%. with % RSD values were within 2. The limit of detection and limit of quantification were found to be 0.05 μg/ml and 0.01 μg/ml respectively. The method was found to be having suitable application in routine laboratory analysis with high degree of accuracy and precision.

Key Aspects of Analytical Method Development and Validation

2019 ◽  
Vol 31 (1) ◽  
pp. 32-39
Author(s):  
Suman Shrivastava ◽  
Pooja Deshpande ◽  
S. J. Daharwal
Keyword(s):  
Method Validation ◽  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Key Aspects ◽  
Development And Validation

Development of a method is crucial for discovery, development, and analysis of medicines in the pharmaceutical formulation. Method validation could also be thought to be one in all the foremost well-known areas in analytical chemistry as is reproduced within the substantial variety of articles submitted and presented in peer review journals every year. Validation of an analytical procedure is to demonstrate that it's appropriate for its intended purpose. Results from method validation are often wont to decide the quality, reliability and consistency of analytical results. Analytical methods need to be validated or revalidated. This review describes general approach towards validation process and validation parameters to be considered during validation of an analytical method. It also refers to various regulatory requirements like WHO, USFDA, EMEA, ICH, ISO/IEC. The parameters described here are according to ICH guidelines which include accuracy, precision, specificity, limit of detection, limit of quantification, linearity range and robustness.

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 Method Development and Validation of A Novel Anti-Depressant Bupropion by RP-HPLC

2020 ◽  
Vol 8 (3) ◽  
pp. 211-224
Author(s):  
Anil Kumar ◽  
Dilip Agarwal ◽  
Mukesh Bansal
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Antidepressant Drug ◽  
Ammonium Hydroxide ◽  
Ammonium Bicarbonate ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
High Degree

A speedy, simple and precise RP-HPLC process was developed for the estimation of novel antidepressant drug bupropion with Waters X – Bridge C-18 5µm, 4.6 X 150 mm columnusing mobile phase Acetonitrile: Ammonium bicarbonate (5mM) pH-9 adjusted with 1% Ammonium hydroxide (50:50, %v/v).The flow rate was 1 ml/min and quantification was done by PDA detector at wavelength254nm.The Bupropion eluted from the column in 5.194 min. The validation was carried out in the light of ICH guidelines with respect to parameters linearity, specificity, accuracy, limit of detection (LOD) and limit of quantification (LOQ). The proposed method showed linearity in the concentration range of 50 to 250 ppm for Bupropion. The linear regression equation of Bupropion was found to be y = 6E+06x + 91344 and correlation coefficient value was found to be 0.997 indicating a high degree of linearity for the drug. The limit of detection (LOD) of bupropion was 0.5 ppm and limit of quantification (LOQ) was 2.0 ppm. The low values of %recovery and %C.V. showed that the method is precise within the acceptance limit of 5% (according to ICH guidelines).      

scholarly journals UV Method Development and Validation of Ellagic Acid for its Rapid Quantitative Estimation

2019 ◽  
Vol 7 (1) ◽  
pp. 1-5
Author(s):  
Harsheen Kaur ◽  
Arti Thakkar ◽  
Kalpana Nagpal
Keyword(s):  
Ellagic Acid ◽  
Method Development ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Uv Spectroscopy ◽  
Entrapment Efficiency ◽  
Good Recovery ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation

Development and validation of a simple UV- Spectroscopy method was done for the quantitative analysis of Ellagic Acid (EA). The stock solution of 50μg/ml was prepared and scanned, for which absorption maxima was found to be 277nm. Further dilutions to different concentrations (1-5μg/ml) were prepared and analyzed at 277nm. The method so developed was validated as per ICH guidelines for: linearity, robustness, precision, accuracy, limit of detection and quantification. The Lambert- Beer’s law is followed in the range (1-5μg/ml) with correlation coefficient value 0.9994. It was observed that the method is precise and accurate for EA analysis with good recovery percent of 94.47% to 106.83%. The method developed was further employed for determining the entrapment efficiency of ellagic acid and its release from its nanoparticle dosage form. The method may be utilized for determining the concentration of EA when present as formulation and in combination with other drugs.

scholarly journals Development and Validation of UV Spectrophotometric Method of Mesalamine Using Hydrotropic Solubilizing Agents

2021 ◽  
Vol 12 (3) ◽  
pp. 2291-2296
Author(s):  
Bhavani N. L. D. ◽  
Gowtham Reddy Cheruku ◽  
Bhargava Sri Harsha Polina ◽  
Dheeraj Kotagiri ◽  
Jnanendra Kumar Korukollu
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Regression Equations ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Technical Requirements ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Method Development And Validation ◽  
Development And Validation

The work was proposed to discuss method development and validation of the drug Mesalamine by using hydrotropic solubilizing agents. An uncomplicated, accurate, and precise method was developed for the drug Mesalamine in bulk as well as Pharmaceutical dosage form. 5M Urea was used as the hydrotropic solubilizing agent to enhance the solubility of the drug. The maximum wavelength (ʎ max) for Mesalamine was found to be 241nm. The validation was performed as per International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines for Accuracy, linearity, precision, Limit of detection (LOD) and Limit of quantification (LOQ). Percentage recovery (%) of Mesalamine was ascertained to be between 95 to 98%. Linearity for Mesalamine was observed between 2-10 µg/ml. Regression equation y=0.0571x-0.0186, regression coefficient (r²) is 0.9996 for Mesalamine. Inter day and intraday precision were checked, % relative standard deviation values were less than 2 for both the methods. Limit of detection (LOD) and Limit of quantification (LOQ) values were derived using regression equations. LOD value was found to be 0.55 µg/ml. LOQ value was found to be 1.67 µg/ml. The assay of the marketed formulation was performed and the results of the assay were obtained by the proposed method. The results are in between 98-102%. So, the method developed was simple and economical that can be adopted for routine tests.

RAPID RP-HPLC METHOD DEVELOPMENT AND VALIDATION OF LURASIDONE HYHROCHLORIDE IN BULK AND TABLET FORM

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (01) ◽  
pp. 28-34
Author(s):  
K. Vijaya Sri ◽  
M. Shiva Kumar ◽  
A. Sravani ◽  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Tablet Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation

The RP-HPLC were developed and validated for the estimation of lurasidone HCl as per ICH guidelines. A simple, fast, accurate and precise RP-HPLC method was developed by using methanol: water containing 0.01% ortho phosphoric acid in the ratio of 70:30 (V/V). The method was developed in Eclipse C18 column (100 mm × 4.6 mm, 3.5 μm particle size). The method was found to be linear in the range of 2.5- 15µg/mL with a correlation coefficient value of 0.999. The accuracy studies of RP-HPLC method was performed at three different levels, i.e., 50%, 100%, and 150% and recovery was found to be in the range of 100.1-100.6% .The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.30-0.92. Satisfactory validation was also obtained from recovery (99.8%) studies, intra-day and interday precision and robustness 2%. The proposed method was found to be accurate, precise and rapid for the analysis of lurasidone.

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 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.

Analytical Method Development and Validation of Glipizide to Determine Residual solvents by head Space-Gas Chromatography

2021 ◽  
pp. 2440-2444
Author(s):  
Sanapala Srinivasa Rao ◽  
A. Vijayalakshmi
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Dimethyl Formamide ◽  
Analytical Methodology ◽  
Residual Solvents ◽  
Flame Ionization ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation

Residual solvents in Pharmaceuticals are termed as organic volatile impurities. These are the chemicals that are used in the manufacture of drug substance or excipients or use in the preparation of final formulation. Most of the available methods use liquid chromatography which could be expensive and time consuming. Hence, an analytical methodology was developed for the quantification of residual solvents in Glipizide using a headspace gas chromatography (HSGC) with the help of flame ionization detector (FID). Methanol, acetone and dimethyl formamide as residual solvents were determined in Glipizide. Analysis was performed by headspace GC/FID method on Auto system- HS40. Nitrogen was used as a carrier gas and the separation of residual solvents was achieved by DB-Wax 0.25mm, 0.3mcm column. The thermostat temperature was 115 °C for 40 minutes for each vial. % RSD for nine injections obtained are in acceptance criteria. The correlation coefficient R2 obtained greater than 0.99. The method parameters were validated includes specificity, limit of detection and quantification, accuracy, linearity, precision, and robustness. According to the International Conference on Harmonization (ICH) guidelines, a new simple, specific, accurate and precise method was developed and validated.

scholarly journals A Stability Indicating Assay Method Development and Validation for the Frovatriptan Succinate Monohydrate by Using UV: A Spectrophotometric Technique

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Hitesh Verma ◽  
Surajpal Verma ◽  
Harmanpreet Singh
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Assay Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Experimental Conditions ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Relative Standard

A new simple, reliable, inexpensive, and accurate method was developed for the quantification of Frovatriptan Succinate Monohydrate in different physiological media at 244 nm in bulk and in tablet dosage forms. The developed method is an attempt to surpass the disadvantages associated with the reported methods, namely, less sensitive and tedious in usage for routine purposes. Beer’s law was followed over the range of 1.0 µg/mL to 4.5 µg/mL. Stability indicating assay method was developed and validated as per the ICH guidelines using various parameters, for example, accuracy, precision, limit of quantification, limit of detection, robustness, ruggedness, solution stability, recovery, forced degradation (hydrolysis, photo degradation, thermal degradation, and oxidation), and so forth. Percent relative standard deviation associated with all the parameters was less than 2, showing compliance with the acceptance criteria of ICH guidelines. The developed method was very sensitive as limit of quantification and limit of detection were found to be 0.025 µg/mL and 0.00625 µg/mL, respectively. Forced degradation studies of drug reveal good stability under the chosen experimental conditions.

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