Analytical Method Development and Validation of UV-visible Spectrophotometric Method for the Estimation of Vildagliptin in Gastric Medium

Drug Research ◽  
2020 ◽  
Vol 70 (09) ◽  
pp. 417-423
Author(s):  
Beena Kumari ◽  
Aparna Khansili
Keyword(s):  
Melting Point ◽  
Spectrophotometric Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Scanning Calorimetry ◽  
Limit Of Quantification ◽  
Double Beam ◽  
Uv Visible ◽  
Development And Validation

Abstract Background Vildagliptin is an antidiabetic agent, belongs to the dipeptidyl peptidase IV (DPP-4) inhibitors. Objective The aim of investigation was to develop a simple UV-visible Spectrophotometric method for the determination of vildagliptin in its pure form and pharmaceutical formulations, further to validate the developed method. Material and Methods Vildagliptin was estimated using UV-Visible double beam spectrophotometer at the wavelength of maximum absorption (210 nm) in acidic medium containing 0.1N HCl. The drug was characterized by melting point, Differential Scanning Calorimetry (DSC), and Fourier Transform Infra-Red (FTIR) techniques. The analysis of the drug was carried out by novel UV-Visible method which was validated analytical parameters like linearity, precision, and accuracy as per guidelines laid down by International Conference on Harmonization (ICH). Result Melting point of drug was found 154°C which is corresponds to its actual melting range. Similarly by the interpretation of spectra the drug was confirmed. The linear response for concentration range of 5–60 µg/ml of vildagliptin was recorded with regression coefficient 0.999. The accuracy was found between 98–101%. Precision for intraday and interday was found to be 1.263 and 1.162 respectively, which are within the limits. To establish the sensitivity of the method, limit of detection (LOD) and limit of quantification (LOQ) were determined which were found to be 0.951 µg/ml and 2.513 µg/ml respectively. Conclusion The UV method developed and validated for vildagliptin drug was found to be linear, accurate, precise and economical which can be used for the testing of its pharmaceutical formulations.

scholarly journals DEVELOPMENT AND VALIDATION OF UV-SPECTROPHOTOMETRIC METHOD FOR ESTIMATION OF HYDROQUINONE IN BULK, MARKETED CREAM AND PREAPARED NLC FORMULATION

2017 ◽  
Vol 9 (5) ◽  
pp. 102
Author(s):  
Sukhjinder Kaur ◽  
Taranjit Kaur ◽  
Gurdeep Kaur ◽  
Shivani Verma
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Pure Form ◽  
Nanostructured Lipid Carrier ◽  
Limit Of Quantification ◽  
Double Beam ◽  
Uv Visible ◽  
Development And Validation

Objective: The aim of the present work was to develop a simple, rapid, accurate and economical UV-visible spectrophotometric method for the determination of hydroquinone (HQ) in its pure form, marketed formulation as well as in the prepared nanostructured lipid carrier (NLC) systems and to validate the developed method.Methods: HQ was estimated at UV maxima of 289.6 nm in pH 5.5 phosphate buffer using UV-Visible double beam spectrophotometer. Following the guidelines of the International Conference on Harmonization (ICH), the method was validated for various analytical parameters like linearity, precision, and accuracy robustness, ruggedness, limit of detection, quantification limit, and formulation analysis.Results: The obtained results of the analysis were validated statistically. Recovery studies were performed to confirm the accuracy of the proposed method. In the developed method, linearity over the concentration range of 5-40 μg/ml of HQ was observed with the correlation coefficient of 0.998 and found in good agreement with Beer Lambert’s law. The precision (intra-day and inter-day) of the method was found within official RCD limits (RSD<2%).Conclusion: The sensitivity of the method was assessed by determining the limit of detection and limit of quantification. It could be concluded from the results obtained that the purposed method for estimation of HQ in pure form, in the marketed ointment and in the prepared NLC-formulation was simple, rapid, accurate, precise and economical. It can be used successfully in the quality control of pharmaceutical formulations and for the routine laboratory analysis.

scholarly journals ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF NORFLOXACIN PRESENT IN TASTE MASKED DRUG RESIN COMPLEX

2018 ◽  
Vol 11 (4) ◽  
pp. 244
Author(s):  
Ayya Rajendra Prasad ◽  
Jayanthi Vijaya Ratna
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Development And Validation

 Objective: The objective of this study was developed and validated a novel, specific, precise, and simple ultraviolet (UV)-spectrophotometric method for the estimation of norfloxacin present in taste masked drug-resin complex.Methods: UV-spectrophotometric determination was performed with ELICO SL 1500 UV-visible spectrophotometer using 0.1 N HCl as a medium. The spectrum of the standard solution was run from 200 to 400 nm range for the determination of absorption maximum (λ max). λ max of norfloxacin was found at 278 nm. The absorbance of standard solutions of 1, 2, 3, 4, and 5 μg/ml of drug solution was measured at an absorption maximum at 278 nm against the blank. Then, a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, limit of detection (LOD) and limit of quantification (LOQ), accuracy, precision, and robustness were evaluated as per the International Conference on Harmonization (ICH) guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 1–5 μg/ml with a correlation coefficient of 0.9995. The LOD and LOQ for norfloxacin were found at 0.39 μg/ml and 1.19 μg/ml, respectively. Accuracy was in between 99.00% and 99.17%. % relative standard deviation for repeatability, intraday precision, and interday precision was found to be 0.600, in between 0.291 and 0.410, and in between 0.682 and 1.439, respectively. The proposed UV spectrophotometric method is found to be robust.Conclusion: The proposed UV-spectrophotometric method was validated according to the ICH guidelines, and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable, and simple for the estimation of norfloxacin present in taste masked drug-resin complex.

scholarly journals UV-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF LORNOXICAM IN MICROSPONGES

2018 ◽  
Vol 10 (1) ◽  
pp. 74 ◽  
Author(s):  
Ayya Rajendra Prasad ◽  
Bannaravuri Thireesha
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Straight Line ◽  
Validation Parameters ◽  
Development And Validation

Objective: To develop and validate a novel, specific, precise and simple UV-spectrophotometric method for the estimation of lornoxicam present in microsponges.Methods: UV-spectrophotometric determination was performed with Thermo Scientific Evolution 201 UV-Vis spectrophotometer using methanol as a medium. The spectrum of the standard solution was run from 200-400 nm range for the determination of absorption maximum (λ max). λ max of lornoxicam was found at 353 nm. The absorbance of standard solutions of 3, 6, 9, 12 and 15, µg/ml of drug solution was measured at an absorption maximum at 353 nm against the blank. Then a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, LOD and LOQ, accuracy, precision and robustness were evaluated as per ICH guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 3.0-15.0 µg/ml with a correlation coefficient of 0.9995. The limit of detection (LOD) and limit of quantification (LOQ) for lornoxicam was found at 1.26 μg/ml and 3.82 μg/ml respectively. Accuracy was in between 99.21 and 99.60%. % RSD for repeatability, intraday precision and interday precision were found to be 0.473, in between 0.478 and 0.619 and in between 0.855 and 1.818 respectively. The proposed UV method is found to be robust.Conclusion: The proposed UV-Visible spectrophotometric method was validated according to the ICH guidelines and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable and simple for the estimation of lornoxicam present in microsponges.

scholarly journals DEVELOPMENT OF SPECTROPHOTOMETRIC AND FLUOROMETRIC METHODS FOR ESTIMATION OF DARUNAVIR USING QBD APPROACH

2018 ◽  
Vol 10 (1) ◽  
pp. 13 ◽  
Author(s):  
R. D. Godambe ◽  
J. I. Disouza ◽  
C. M. Jamkhandi ◽  
P. S. Kumbhar
Keyword(s):  
Experimental Work ◽  
Spectrophotometric Method ◽  
Method Development ◽  
Regression Coefficient ◽  
Limit Of Detection ◽  
Fluorometric Method ◽  
Limit Of Quantification ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Testing Criteria

Objective: The main objective of the present study is to develop newer simple, precise spectrophotometric and fluorometric methods of estimation for Darunavir using coupling agent O-pthaladehyde.Methods: The experimental work was designed for both spectroscopic and fluorometric method development and validation. The method is based on formation complex of Darunavir with O-pthaladehyde. QbD approach was applied by varying different parameters. These parameters were designed into Ishikawa diagram.Results: The complex Darunavir-Phthalaldehyde in methanol with 0.1 N HCl showed linearity for both spectrophotometric and fluorometric methods. The calibration curve by spectrophotometry is linear in concentration range of 2-22 µg/ml with regression coefficient (R2) = 0.998 at 355 nm and for fluorometry it is linear in concentration range of 0.5-5.0 ng/ml with regression coefficient (R2) = 0.999. This method was found to be rugged and robust in different testing criteria with % RSD less than 2. The limit of detection and limit of quantification was found to be 0.2 μg/ml and 0.8 μg/ml for a spectrophotometric method and 0.12 μg/ml and 0.43 μg/ml for fluorometric method respectively.Conclusion: Both methods were found to be precise with % RSD of less than 2. The % recovery of the spectrophotometric and fluorometric methods was found to be 101.04 %, 98.15 % respectively. In this way, the results of all validation parameter were within the limits as per International Conference on Harmonization guideline. 

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF CEFIXIME AND OFLOXACIN IN TABLETS BY RP-HPLC METHOD

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (08) ◽  
pp. 33-37
Author(s):  
T. Venkatachalam ◽  
◽  
K. G. Lalitha
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Development And Validation

A chromatographic method has been developed as per ICH norms for the simultaneous estimation of cefixime and ofloxacin from pharmaceutical formulations. The method was carried out on a column -Gemini (250 x. 4.6, 5 mc) with a mobile phase consisting of 0.2 M potassium dihydrogen phosphate buffer (adjusted to pH 7 with 1 % w/w triethylamine), acetonitrile and methanol in 70:20:10 ratio and filtered through 0.45 mc cellulose nitrate filters. The flow rate 1.0 mL/min. Detection was carried out at 288 nm. The retention time of CEF and OFL was 2.16 and 7.86 min respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantification and solution stability. The proposed method can be used for the estimation of these drugs in combined dosage forms.

scholarly journals A novel spectrophotometric method development and validation of Tenagliptin in its Tablet dosages form

2019 ◽  
Vol 9 (5) ◽  
pp. 95-98
Author(s):  
Poulami Patra ◽  
Somsubhra Ghosh ◽  
Tathagata Roy ◽  
B. V. V. Ravi kumar
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Ultra Violet ◽  
Range Limit ◽  
Limit Of Quantification ◽  
International Conference ◽  
Validation Parameters ◽  
Insulin Dependent ◽  
Uv Visible ◽  
Development And Validation

The aim of present work was to develop a new, economical & simple analytical method of Teneligliptin & its validation as per International Conference on Harmonization (ICH) guideline, which is a new antidiabetic drug that is used to treat Non-Insulin Dependent Diabetis Melitus (NIDDM) patients. A sensitive and specific Ultra Violet (UV) Visible method was developed & the analysis was carried out by using Shimazdu 1800 Spectrophotometer, 0.1(N) NaOH was used as a solvent. The UV- Visible Spectrophotometric estimation was carried out at a λ max of 242 nm using 1cm thick quartz cell. Validation of the newly developed method was performed as per International Conference on Harmonization (ICH) Q2R1 guideline in the following parameters: Calibration curve, Accuracy, Precision etc.  Newly developed method obeys Beer’s-Lambert’s law in the concentration range of 5 - 25 μg / ml, whereas correlation coefficient value is less than 1. The percent amount of drug estimated by this developed method was 100.91 %, which is very close to 100 %. The validation parameters like Accuracy, Precision, Linearity, Range, Limit of detection (LOD) & Limit of Quantification (LOQ) were studied for the developed method and was found to be within the limits. Keywords: Teneligliptin, Validation, Method, Spectroscopy etc.

scholarly journals DEVELOPMENT AND VALIDATION OF SPECTROPHOTOMETRIC METHODS FOR SIMULTANEOUS ESTIMATION OF VILANTEROL AND FLUTICASONE FUROATE IN PHARMACEUTICAL FORMULATIONS

2017 ◽  
Vol 10 (4) ◽  
pp. 302
Author(s):  
Siva Kishore Masimukku ◽  
Rambabu Chintal
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Simultaneous Equation ◽  
Equation Method ◽  
Simultaneous Estimation ◽  
Fluticasone Furoate ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
Development And Validation

Objective:  To develop a simple, rapid,  precise, accurate, sensitive spectrophotometric methods (A&B) were developed for simultaneous estimation and validation of Vilanterol (VTL) and Fluticasone Furoate (FFE) in pure and tablet dosage forms.Method:   Method A is a simultaneous equation method and method B is a first order derivative spectrophotometric method. Pure drug samples of VTL and FFE were dissolved in a mixture of Methanol and Ethanol in the ratio of 1:1 (v/v) and found to have absorbance maxima at 231nm for VTL and 260nm for FFE respectivelyResults:  The linearity lies between 2.5–10µg/ml for VTL and 10–60µg/ml for FFE in these two methods (A&B).  The correlation coefficient (r2) was found to be 0.999 for both VTL and FFE, the limit of detection and limit of quantification were found to be 0.015µg/ml and 0.05µg/ml for VTL and 0.05µg/ml and 0.2µg/ml for FFE respectively. The results of analysis have been validated statistically by recovery studies as per ICH guidelines.Conclusion: The two methods A&B showed good reproducibility and recovery with % RSD less than 2.  Hence both methods were found to be rapid, specific, precise and accurate and can be successfully applied for the routine analysis of VTL and FFE in pure and combined dosage form.Keywords: Fluticasone furoate, Vilanterol, Derivative spectrophotometric, Simultaneous equation method, Method development and validation.

scholarly journals Development and Validation of Ultra Visible Spectrophotometric Method for the Estimation of Thymoquinone

2021 ◽  
pp. 25-30
Author(s):  
Sagar Trivedi ◽  
Veena Belgamwar ◽  
Kamlesh Wadher
Keyword(s):  
Spectrophotometric Method ◽  
Method Development ◽  
Spectroscopic Method ◽  
Pharmaceutical Sciences ◽  
University Campus ◽  
Qualitative And Quantitative Analysis ◽  
Quality Control Tool ◽  
Double Beam ◽  
Uv Visible ◽  
Development And Validation

Aim: The work mainly focuses on developing a robust UV-Visible spectroscopic method for qualitative and quantitative analysis of thymoquinone and this will open to many possibilities in exploiting the wonders of this bioactive molecule. Study Design:  UV-vis Spectrophotometric method development for thymoquinone. Place and Duration of Study: Department of Pharmaceutics, Department of Pharmaceutical Sciences, Rashtrasant Tukadoji Maharaj Nagpur University Campus, Nagpur, India. Methodology: To find out λmax and validate the developed method using Double beam UV – visible spectrophotometer module (JASCO V-630). Results: The thymoquinone was found to be soluble in methanol. The absorption maximum (λmax) was found to be 252 nm. The good linearity was found to be within concentration range of 2-10 μg/ml with correlation coefficient (r2) >0.99 and regression equation of the curve was found to be y = 0.0173x − 0.0394 at 252 nm. The precision (intra-day and inter-day) data represents good reproducibility with % RSD lower than 2.0% which assured that method is précised. Mean recovery value at different concentrations was found to be higher than 90%, indicates accuracy of the method. LOD and LOQ for thymoquinone were reported and were found to be 0.016 μg/ml and 0.0531μg/ ml 252 nm. Conclusion: The developed method was found to be simple, specific, economic, reliable, accurate, precise, and reproducible used as a quality control tool for analysis of pure thymoquinone and thymoquinone in formulations.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

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.

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