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.

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 Development and Validation of Spectrophotometric Methods for Simultaneous Estimation of Furosemide and Spironolactone by Vierordt’s Method in Bulk and Combined Tablet Dosage Form

2018 ◽  
Vol 26 (1) ◽  
pp. 74-90 ◽  
Author(s):  
Rohankumar R. Chavan ◽  
Somnath D. Bhinge ◽  
Mangesh A. Bhutkar ◽  
Dheeraj S. Randive
Keyword(s):  
Spectrophotometric Method ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Simultaneous Equation ◽  
Equation Method ◽  
Simultaneous Estimation ◽  
Spectrophotometric Methods ◽  
Bulk Drug

Abstract Anew simple, convenient and suitable spectrophotometric method for simultaneous determination of Furosemide and Spironolactone in combined dosage form has been developed and validated. Simultaneous equation method (Vierordt’s method) was used for determination of Furosemide and Spironolactone in combined dosage form. For spectrophotometric method development double distilled water and ethanol were used as a solvent in the ratio of (20:80). The proposed method was quantitatively evaluated in terms of linearity, precision, accuracy, lower limit of detection (LOD) and quantification (LOQ), recovery and robustness. All the parameters were found to be within the acceptance limit. λmax of Furosemide and Spironolactone was found to be 275 and 237 nm respectively. Beer’s law was obeyed over the concentration ranges of 2-10 μg mL−1 for both Furosemide and Spironolactone respectively. The % assay for commercial formulation was found to be 99.60%±0.0500 for Furosemide and 100.26%±1.17 for Spironolactone by the proposed methods. The overall recovery was observed to be 100.38±0.09% for Furosemide and 100.49±0.4197% for Spironolactone by simultaneous equation method (Vierordt’s method). LOD and LOQ were 0.76 and 2.32 μg mL−1 for Furosemide, 1.99 and 6.04 μg mL−1 for Spironolactone. A new simple, convenient, precise, rapid, accurate and economical and reliable spectrophotometric method was developed and validated for the analysis of Furosemide and Spironolactone in bulk drug and their formulations.

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.

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF THYMOL AND EUGENOL BY USING RP-HPLC IN PURE AND IN EMULGEL FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 59-65
Author(s):  
Vinita C. Patole ◽  
Shilpa P. Chaudhari ◽  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Peak Areas ◽  
80 A 20 ◽  
Development And Validation

An attempt was made to develop a simple, selective, rapid and precise high-performance liquid chromatography (HPLC) method for simultaneous estimation of thymol and eugenol. Analysis was performed on a C18 column with the mobile phase consisting of solvent %A (water) and solvent %B (acetonitrile) with the following gradient: 0–1 min, 80 % A, 20 % B; 1–7 min, 40 % A and 60 % B; 7–12 min, 10 % A and 90 % B; and 12–15min, 80 % A and 20 % B at a flow rate of 0.6 mL/min. The compounds were well separated on a Thermo Scientific Hypersil BDS RP C18 column (4.6 mm × 150 mm, dp = 5 µm) and ultraviolet detection at 280 nm. The retention times of eugenol and thymol were 10.5 min and 11.6 min, respectively. Validation of the proposed method was carried out according to the guidelines of the International Council on Harmonization (ICH). The linearity of the method is good for thymol and eugenol over the concentration range of 1–50 ppm, and the r 2 values were 0.9996 for both thymol and eugenol. The calculated limit of detection (LOD) value was 0.5ppm and the limit of quantification (LOQ) value was 1ppm for both the analytes. The intra and interday relative standard deviation (RSD) of the retention time and peak areas was less than 3 %.The established method was appropriate, and the two markers were well resolved, enabling efficient quantitative analysis of thymol and eugenol.

scholarly journals Method Development and Validation of Stability Indicating RP-HPLC Method for Simultaneous Estimation of Escitalopram Oxalate and Clonazepam in Bulk and its Pharmaceutical Formulations

2019 ◽  
Vol 9 (1-s) ◽  
pp. 265-274
Author(s):  
Bindusar Kalia ◽  
Uttam Singh Baghel
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Plot ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Rp Hplc

This article refers to simple isocratic reverse-phase high-performance liquid chromatographic method (RP-HPLC) developed for the simultaneous quantification of Escitalopram Oxalate (EST) and Clonazepam (CZP) in active pharmaceutical ingredient and pharmaceuticals. The separation of the two drugs was attained using a C₁₈ column (250mm×4.6mm, 5µ) as a stationary phase. The mobile phase was used as a mixture of methanol; acetonitrile; and 0.05M potassium dihydrogen orthophosphate buffer (pH 4 adjusted by orthophosphoric acid) with an isocratic ratio of 40:20:40 v/v. Detection was made by using PDA detector at 210 nm. Escitalopram Oxalate (RT= 4.428 minutes) and Clonazepam (RT= 6.532 minutes) were separated in a single chromatographic run with resolution of 8.719. The calibration plot indicated good linear relationship with r2 = 0.998 for Escitalopram Oxalate in concentration range of 32 µg/ml - 48 µg/ml and r2 = 0.999 for Clonazepam in concentration range of 16 µg/ml - 24 µg/ml. The retrievals for Escitalopram Oxalate and Clonazepam were found to be 99.75% and 99.00%, respectively. The established analytical method was validated and found acceptable as per ICH guidelines for linearity, precision, accuracy, specificity, limit of detection, limit of quantification, robustness and stability. Escitalopram Oxalate and Clonazepam individually as well as in combination were exposed to different stress conditions like acid, base, thermal, photolytic and oxidation degradation and peaks of a degraded product were well determined from peaks of pure drug. This method is modest, quick and appropriate for routine quality control analysis. Keywords: Reverse Phase – HPLC; Escitalopram Oxalate; Clonazepam; Validation; Degradation study.

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Mirabegron in Bulk and Dosage Form

2020 ◽  
Vol 10 (1) ◽  
pp. 31-38
Author(s):  
Rahul Suryawanshi ◽  
Siddiqua Shaikh ◽  
Snehal Patil
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Hplc Method Development ◽  
Tablet Dosage

A new, simple, precise, accurate and reproducible Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method for Simultaneous estimation of bulk and pharmaceutical formulations. Separation of Mirabegron was successfully achieve , C18, 250X4.6mm, 5µm or equivalent in an isocratic mode utilizing methanol water (70:30) at pH 5.0 Adjusted to OPA at a flow rate of 1.0ml/min and eluate was monitored at 243nm, with a retention time of 2.584 minutes for Mirabegron. The method was validated and the response was found to be linear in the drug concentration range of 50µg/ml to150 µg/ml for Mirabegron. The values of the correlation coefficient were found to 0.999for Mirabegron. The Limit of Detection(LOD) and Limit of Quantification (LOQ) for Mirabegron were found to be 0.149 and 0.498 respectively. This method was found to be good percentage recovery were found to be 99 indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample so, the method specifically determines the analyte in the sample without interference from excipients of tablet dosage forms. The method was extensively validated according to International Council for Harmonisation(ICH) guidelines for Linearity, Accuracy, Precision, Specificity and

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.

Development and Validation of UV Spectroscopic Method for Simultaneous Estimation of Pantoprazole and Cinitapride in Bulk and in Capsule Dosage FormC

2018 ◽  
Vol 9 (4) ◽  
Author(s):  
Gaur A ◽  
Yashwant .
Keyword(s):  
Dosage Form ◽  
Spectroscopic Method ◽  
Pharmaceutical Formulations ◽  
Simultaneous Equation ◽  
Equation Method ◽  
Routine Analysis ◽  
Simultaneous Estimation ◽  
Development And Validation

A new, rapid, precise, selective and sensitive Vierodt���s/simultaneous equation method is developed for the simultaneous estimation of pantoprazole (PNT) and cinitapride (CNT) in combined dosage form. In the developed method, absorbance was measured at 289 nm (�� max of Pantoprazole) and 267.2 nm (�� max of Cinitapride). The drugs obeyed the Beer���s law in the concentration range of 13-65��g/ml and 1-5 ��g/ml respectively for pantoprazole and cinitapride. Accuracy of the method was determined by recovery studies and was found to be 101.32 % and 98.9 % for Pantoprazole and Cinitapride respectively. The developed method is simple, precise, rapid and selective. It can be used for routine analysis of both drugs in bulk as well as in pharmaceutical formulations.

scholarly journals Development and Validation of Spectrophotometric Methods for Simultaneous Estimation of Valsartan and Hydrochlorothiazide in Tablet Dosage Form

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Monika L. Jadhav ◽  
Manoj V. Girase ◽  
Shripad K. Tidme ◽  
Manish S. Junagade
Keyword(s):  
Dosage Form ◽  
Pharmaceutical Formulations ◽  
Simultaneous Equation ◽  
Ratio Method ◽  
Simultaneous Estimation ◽  
Spectrophotometric Methods ◽  
Absorbance Ratio ◽  
Standard Additions ◽  
Development And Validation ◽  
Tablet Dosage

Two UV-spectrophotometric methods have been developed and validated for simultaneous estimation of valsartan and hydrochlorothiazide in a tablet dosage form. The first method employed solving of simultaneous equations based on the measurement of absorbance at two wavelengths, 249.4 nm and 272.6 nm, λmax for valsartan and hydrochlorothiazide, respectively. The second method was absorbance ratio method, which involves formation of Q-absorbance equation at 258.4 nm (isoabsorptive point) and also at 272.6 nm (λmax of hydrochlorothiazide). The methods were found to be linear between the range of 5–30 µg/mL for valsartan and 4–24 μg/mL for hydrochlorothiazide using 0.1 N NaOH as solvent. The mean percentage recovery was found to be 100.20% and 100.19% for the simultaneous equation method and 98.56% and 97.96% for the absorbance ratio method, for valsartan and hydrochlorothiazide, respectively, at three different levels of standard additions. The precision (intraday, interday) of methods was found within limits (RSD<2%). It could be concluded from the results obtained in the present investigation that the two methods for simultaneous estimation of valsartan and hydrochlorothiazide in tablet dosage form are simple, rapid, accurate, precise and economical and can be used, successfully, in the quality control of pharmaceutical formulations and other routine laboratory analysis.

METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS ESTIMATION OF PIOGLITAZONE AND GLIMEPIRIDE - A UV SPECTROPHOTOMETRIC APPROACH

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (11) ◽  
pp. 30-35
Author(s):  
P. K Kottu ◽  
◽  
A.P. Gadad ◽  
P. M Dandagi
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Estimation Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
R Value ◽  
Development And Validation ◽  
Tablet Dosage

Objective: The objective of the present work was to design a simple, accurate, economical and reproducible UV spectrophotometric method for the simultaneous estimation of a two-component drug mixture of pioglitazone and glimepiride in the combined tablet dosage form. Methodology: Simultaneous estimation method that involves maximum absorbance (λ max) of Pioglitazone and Glimepiride at 279.0 nm and 238.0 nm, respectively was developed. The proposed method was validated as per ICH guidelines for accuracy, precision, linearity, limit of quantification (LOQ) and limit of detection (LOD). The calibration curves were linear in the concentration range for pioglitazone (r value) and for glimepiride (r value) and were found to obey Beers law in the linear concentration ranges. Statistical analysis and drug recovery data showed that simultaneous estimation method was simple, rapid, economical, sensitive,precise and reproducible. Hence, the proposed method was recommended for routine analysis of pioglitazone and glimepiride in combined tablet dosage form.

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