scholarly journals DEVELOPMENT AND VALIDATION OF A UV SPECTROPHOTOMETRIC METHOD FOR DETERMINATION OF AGOMELATINE IN BULK AND A TABLET DOSAGE FORM

2021 ◽  
Vol 10 (1) ◽  
pp. 22-25
Author(s):  
Firake Bhushan M. ◽  
Pathak Pranjalee V. ◽  
Dorik Pallavi K. ◽  
Siddaiah M.
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Spectroscopic Method ◽  
Uv Spectrophotometry ◽  
Analytical Method Validation ◽  
Analytical Technique ◽  
International Conference ◽  
Validation Parameters ◽  
Limit Of Quantitation

UV spectrophotometry is an analytical technique used routinely for qualitative and quantitative assay due the low cost and reliability during analysis. An simple, efficient, rapid, sensitive, precise and economical UV Spectrophotometric method has been developed for estimation of agomelatine from bulk and pharmaceutical formulation. The method was developed and validated according to International Conference on Harmonization (ICH Q2 R1) guidelines.  The λmax of agomelatine in acetonitrile was found to be 229.6 nm. The analytical method validation parameters linearity, precision, accuracy, robustness were studied according to International Conference on Harmonization guidelines. Pure drug concentration was prepared in the range of 1-10 μg/ml and the linear regression analysis data showed good linear relationship with correlation coefficient value 0.9937. The precision of the method was studied as an intra- day, inter-day variations with value less than 2 % RSD. The limit of detection and limit of quantitation were found to be 0.577 and 1.248 μg/ml, respectively. Recoveries were found to be in the range of 100.815 to 101.744 % and % RSD was less than 2 %. This proposed UV spectroscopic method is simple and suitable for routine analysis. Keywords: Keywords: Agomelatine, Validation, UV Spectrophotometric method

DEVELOPMENT AND VALIDATION OF NOVEL STABILITY INDICATING UV SPECTROPHOTOMETRIC METHOD FOR THE ESTIMATION OF CINACALCET HYDROCHLORIDE IN BULK AND TABLET DOSAGE FORMS

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (12) ◽  
pp. 31-36
Author(s):  
N Mallikarjuna Rao ◽  
◽  
D. Gowrisankar
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Dosage Forms ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Cinacalcet Hydrochloride ◽  
Tablet Dosage

A novel stability indicating UV spectrophotometric method for the quantitative determination of cinacalcet hydrochloride, a calcimimetic, in bulk and tablet dosage forms was developed in the present work. The parameters linearity, precision, accuracy, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. UV spectroscopic determination was carried out at an absorption maximum of 281 nm using methanol as solvent. In the UV spectroscopic method, linearity over the concentration range of cinacalcet hydrochloride was found to be 15-35 μg/mL with a correlation coefficient of 0.9992. Results of the analysis were validated statistically and by recovery studies. Forced degradation studies were conducted under various conditions. The proposed method is simple, rapid, precise and accurate and can be used for the reliable quantitation of cinacalcet hydrochloride in commercial pharmaceutical dosage forms.

scholarly journals VALIDATION OF CYCLAMATE ANALYSIS METHOD WITH SPECTROPHOTOMETRY AND TURBIDIMETRY

2016 ◽  
Vol 4 (1) ◽  
Author(s):  
Regina Tutik Padmaningrum ◽  
Siti Marwati
Keyword(s):  
Detection Limit ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Spectrophotometric Analysis ◽  
Linear Range ◽  
Uv Spectrophotometry ◽  
Good Precision ◽  
Analysis Method ◽  
Limit Of Quantitation ◽  
Precision And Accuracy

This research aims to validate methods of analysis by spectrophotometry and turbidimetry cyclamate in the sample drink mango-flavored jelly drink  by spectrophotometry with hypochlorite reagent, ultraviolet spectrophotometry (without reagent) and turbidimetry. The object of research was the validity parameters spectrophotometric method were linearity, linear range, the limit of detection, limit of quantitation, precision, and accuracy. The calibration curve of standard solution of sodium cyclamate in the spectrophotometric method with hypochlorite reagent, UV spectrophotometry (without reagent), and turbidimetry are linear. Linear range each method respectively at a concentration were (211.36-747.08); (16.000-146.434); and (1.8521-6.1717) ppm. The detection limit of each method successively were 53.6028; 0.5833; and 0.2723 ppm. Limit of quantitation each method successively were 66.9948; 1.9443; and 0.8068 ppm. Spectrophotometric analysis method cyclamate with hypochlorite reagent had good precision and accuracy. Ultra violet  spectrophotometric analysis method of cyclamate have a good precision but the accuracy was not good. Turbidimetric methods  analysis of cyclamate had  precision and accuracy were not good.Keywords:   method validation, spectrophotometry, turbidimetry, cyclamate

SPECTROPHOTOMETRIC ESTIMATION AND VALIDATION OF CANAGLIFLOZIN AND METFORMIN HYDROCHLORIDE IN BINARY MIXTURE

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (05) ◽  
pp. 68-72
Author(s):  
Vivek Nalawade ◽  
◽  
Mohammad A. Shaikh ◽  
Vidula Ghodke ◽  
Keyword(s):  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Uv Visible ◽  
Metformin Hcl

The purpose of the work was to establish a UV spectroscopic method for the simultaneous estimation of canagliflozin and metformin hydrochloride in a binary mix. This method involves interpretation of simultaneous equations based on measurement of absorbance at two wavelengths, 237 nm and 290 nm, using UV-visible spectrophotometer with 1cm matched quartz cells. Methanol solvent was employed in this method. The developed method obeyed Beer’s-Lambert’s law in the concentration range of 2-12 µg/mL, having correlation coefficient 0.9998 and 0.9994 for canagliflozin and metformin hydrochloride, respectively. Different validation parameters like accuracy, precision, limit of detection and limit of quantitation were examined and found to be within the limits. The results of the method were validated as per ICH guidelines. A novel, simple, sensitive, rapid, accurate and economical spectrophotometric methods have been developed for simultaneous estimation of canagliflozin and metformin HCl. The technique can be used to determine the amount of canagliflozin and metformin HCl in a mixture containing canagliflozin and metformin. The absorptivities of canagliflozin and metformin HCl are 0.0481 and 0.0921, respectively. Sandell’s sensitivity (mg/cm2 /0.001 absorbance unit) for canagliflozin and metformin HCl was found to be 0.025 and 0.02931, respectively.

scholarly journals A REVIEW ON ANALYTICAL METHOD DEVELOPMENT AND VALIDATION

2018 ◽  
Vol 10 (6) ◽  
pp. 8 ◽  
Author(s):  
Shivani Sharma ◽  
Swapnil Goyal ◽  
Kalindi Chauhan
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Good Manufacturing Practice ◽  
Raw Material ◽  
Analytical Technique ◽  
Effective Manner ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Development And Validation

The top objective of any pharmaceutical industry is to produce products of necessary characteristic and quality reliably, in a cost-effective manner. Development of a method is essential for discovery, development, and evaluation of medicines in the pharmaceutical formulation. The main aim of this review article was to check the development and validation of the procedure employed for the medication from the starting of the formulation to the complete commercial batch of product. At the point when an analytical technique is applied to produce outcomes for the quality of medicine associated samples, it is necessary that the outcomes are reliable. In the pharma industry, validation policy is documented for how to perform validation, types of validation and validation policy are complied with the necessities of good manufacturing practice (GMP) regulations. Validation is very important for the effective running of the pharmaceutical firms. At every stage from raw material to the finished, stability, everywhere validation was performed. The method was developed properly, and validation parameters are explained in terms of accuracy, specificity, precision, limit of detection (LOD), limit of quantitation (LOQ), ruggedness, robustness, and system suitability testing with the example of certain drugs. All validation parameters are used in the routine and stability analysis.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

Method of Validation for Residual Solvents in Bisoprolol Fumarate by GC Technique

2021 ◽  
pp. 147-155
Author(s):  
Sandip A Telavane ◽  
Seema Kothari ◽  
Manohar V. Lokhande
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Technique ◽  
Range Limit ◽  
Column Temperature ◽  
Residual Solvent ◽  
Residual Solvents ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Chromatographic Condition ◽  
Methylene Dichloride

Validation is important technique for detection, progress and estimation of drugs for pharmaceutical analysis. Aim of this article was to check the progress and validation of the method employed for the Residual Solvents in Bisoprolol Fumarate by Gas Chromatographic technique. The objective of this protocol is to validate a GC method of analysis for detection and Quantification of Residual Solvents Methanol, Acetone and Methylene dichloride in Bisoprolol Fumarate. In the pharmaceutical industry, validation policy is more important for documented of validation, types of validation and validation policy. The method was developed accurately and validation parameters are explained. Chromatographic condition was GC- 2014, gas chromatograph equipped with FID detector, column: 30 m x 0.32 mm ID x 1.8 µm DB - 624 capillary column or equivalent and column temperature was 45°C (hold 7 minutes) to 250°C @ 40°C/minutes, hold at 250°C for 3 minutes. The parameters such as Accuracy, Specificity, Precision, Linearity and Range, Limit of detection (LOD), Limit of quantitation (LOQ), ruggedness, robustness and system suitability testing with residual solvent such as Methanol, Acetone and methylene dichloride. All validation parameters are used in the routine and stability analysis.

scholarly journals Spectrophotometric Determination of Olmutinib in Bulk by Area under Curve and First Order Derivative Methods and its Validation as per ICH guidelines

2019 ◽  
Vol 9 (4-A) ◽  
pp. 349-354
Author(s):  
BALU KHANDARE ◽  
Atish C. Musle ◽  
Sanket S. Arole ◽  
Pravin V. Popalghat
Keyword(s):  
Area Under Curve ◽  
Limit Of Detection ◽  
Order Derivative ◽  
Spectrometric Method ◽  
First Order ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract: A simple, precise and economical UV-spectrophotometric method has been developed for the estimation of Olmutinib from bulk. Two methods were developed First method (A) applied was area under curve (AUC) in which the area was integrated in wavelength from 262-272nm. Second method (B) was first order derivative spectrometric method. In this method absorbance at λmin=256.57nm, λmax=282.83nm and zero cross=267.68nm was measured. Calibration curves were plotted for the method by using instrumental response at selected wavelength and concentration of analyte in the solution. In both the methods, linearity was observed in the concentration range of 2-12µg/ml at the λmax=267.68nm. Accuracy and precision studies were carried out and results were satisfactorily obtained. The drug at each of the 80 %, 100 % and 120 % levels showed good recoveries that is in the range of 98.00 to 99.00% for both methods, hence it could be said that the method was accurate. Limit of detection (LOD) and limit of quantitation (LOQ) were determined for the method. The method was validated as per International Conference on Harmonization. All validation parameters were within the acceptable limit. The developed method was successfully applied to estimate the amount of Olmutinib in pharmaceutical formulation.

SIMULTANEOUS ESTIMATION OF DOXORUBICIN AND HYDROXYCHAVICOL IN BULK AND PHARMACEUTICAL FORMULATION BY Q-ABSORPTION RATIO METHOD

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (02) ◽  
pp. 51-58
Author(s):  
Sachin Bhusari ◽  
Bharti Gotmare ◽  
Pravin Wakte
Keyword(s):  
Quality Control ◽  
Standard Deviation ◽  
Spectrophotometric Method ◽  
Pharmaceutical Formulation ◽  
Ratio Method ◽  
Simultaneous Estimation ◽  
Calibration Standards ◽  
Analytical Method Validation ◽  
Relative Standard ◽  
Validation Parameters

A simple, rapid, accurate, precise and economical UV-spectrophotometric method has been developed and validated for simultaneous estimation of doxorubicin hydroxychavicol (DOXO) and OH-CHV in a pharmaceutical formulation. It is based on the Q-analysis UV Spectrophotometric method. The absorption spectra of DOXO and OH-CHV were obtained over the range of 200-800 nm, and the absorption maxima were determined. Multiple calibration standards were prepared for both the drugs separately and absorbances were recorded at respective absorption maxima. Calibration curves were plotted and the linear responses were studied. Various analytical method validation parameters viz. accuracy, precision, LOD, LOQ, robustness and ruggedness were calculated using quality control standards. The absorbance maxima of DOXO and OH-CHV were found to be 477 nm and 284 nm, respectively in methanol. In Q-analysis, the isoabsorptive point for both the drugs was found at 297 nm. The linearity range was between 5-40 μg/ml for DOXO and 5-40 μg/ml for OH-CHV at their respective wavelengths. The intra-day and inter-day study shows percent relative standard deviation in the range of 0.9991 to 0.9993. LOD and LOQ were found to be 0.024 µg/ml and 0.075µg/ml for DOXO and 0.228μg/ml and 0.692μg/ml for OH-CHV. The total percent recoveries of DOXO and OH-CHV were found to be 98.75 and 99.41, respectively.

scholarly journals Determination of Tianeptine in Tablets by High-Performance Liquid Chromatography with Fluorescence Detection

2007 ◽  
Vol 90 (3) ◽  
pp. 720-724
Author(s):  
Sevgi Tatar Ulu
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Linear Calibration ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract A sensitive and selective high-performance liquid chromatographic method has been developed for the determination of tianeptine (Tia) in tablets. The method is based on derivatization of Tia with 4-chloro-7-nitrobenzofurazan (NBD-Cl). A mobile phase consisting of acetonitrile10 mM orthophosphoric acid (pH 2.5; 77 + 23) was used at a flow rate of 1 mL/min on a C18 column. The Tia-NBD derivative was monitored using a fluorescence detector, with emission set at 520 nm and excitation at 458 nm. Gabapentin was selected as an internal standard. Linear calibration graphs were obtained in the concentration range of 45300 ng/mL. The lower limit of detection (LOD) was 10 ng/mL at a signal-to-noise ratio of 4. The lower limit of quantitation (LOQ) was 45 ng/mL. The relative standard values for intra- and interday precision were &lt;0.46 and &lt;0.57%, respectively. The recovery of the drug samples ranged between 98.89 and 99.85%. No chromatographic interference from the tablet excipients was found. The proposed method was validated in terms of precision, robustness, recovery, LOD, and LOQ. All the validation parameters were within the acceptance range. The proposed method was applied for the determination of Tia in commercially available tablets. The results were compared with those obtained by an ultraviolet spectrophotometric method using t- and F-tests.

scholarly journals DEVELOPMENT AND VALIDATION OF ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD FOR DETERMINATION OF FEBUXOSTAT FOR CONDUCTING IN-VITRO QUALITY CONTROL TESTS IN BULK AND PHARMACEUTICAL DOSAGE FORMS

2018 ◽  
Vol 11 (9) ◽  
pp. 115
Author(s):  
Jaspreet Kaur ◽  
Daljit Kaur ◽  
Sukhmeet Singh
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Development And Validation

Objective: A simple, accurate, and selective ultraviolet-spectrophotometric method has been developed for the estimation of febuxostat in the bulk and pharmaceutical dosage forms.Method: The method was developed and validated according to International Conference on Harmonization (ICH Q2 R1) guidelines. The developed method was validated statistically with respect to linearity, range, precision, accuracy, ruggedness, limit of detection (LOD), limit of quantitation (LOQ), and recovery. Specificity of the method was demonstrated by applying different stressed conditions to drug samples such as acid hydrolysis, alkaline hydrolysis, oxidative, photolytic, and thermal degradation.Results: The study was conducted using phosphate buffer pH 6.8 and λmax was found to be 312 nm. Standard plot having a concentration range of 1–10 μg/ml showed a good linear relationship with R2=0.999. The LOD and LOQ were found to be 0.118 μg/ml and 0.595 μg/ml, respectively. Recovery and percentage relative standard deviations were found to be 100.157±0.332% and <2%, respectively.Conclusion: Proposed method was successfully applicable to the pharmaceutical formulations containing febuxostat. Thus, the developed method is found to be simple, sensitive, accurate, precise, reproducible, and economical for the determination of febuxostat in pharmaceutical dosage forms.

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