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.

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.

DEVELOPMENT AND VALIDATION OF A UV SPECTROPHOTOMETRIC Q-ABSORBANCE RATIO METHOD FOR SIMULTANEOUS ESTIMATION OF EPERISONE HYDROCHLORIDE AND ACECLOFENAC IN BULK AND TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (11) ◽  
pp. 50-56
Author(s):  
M. Simoes ◽  
◽  
L. Almeida
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Ratio Method ◽  
Simultaneous Estimation ◽  
Absorbance Ratio ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Development And Validation ◽  
Tablet Dosage

A simple, sensitive, rapid, accurate, precise and economical Q-absorbance ratio method has been developed for the simultaneous estimation of eperisone hydrochloride and aceclofenac in combined dosage form. The solvent used was methanol:water (70:30 v/v). The iso-absorptive point was found to be 269.5 nm. Calibration curves were linear over a concentration range of 6-21 μg/ml for eperisone hydrochloride and 8-28 μg/mL for aceclofenac, respectively. The developed method was validated as per International Conference on Harmonization (ICH) guidelines for various parameters such as linearity, precision, accuracy, limit of detection and limit of quantitation. Accuracy of method was determined through recovery studies which were found to be 99.0% - 100.89 % for eperisone hydrochloride and 98.67% - 100.44 % for aceclofenac. Method was found to be reproducible with relative standard deviation (RSD) for intra-and inter-day precision less than 2% over the concentration range. The proposed method can be used for routine analysis of eperisone hydrochloride and aceclofenac in bulk and tablet dosage form.

scholarly journals A NEW ROBUST ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF RIBOCICLIB AND LETROZOLE IN SOLID DOSAGE FORM (TABLET)

2021 ◽  
pp. 129-134
Author(s):  
BHAGYALATA SATAPATHY ◽  
CHAITANYA BANGARI
Keyword(s):  
Analytical Method ◽  
Dosage Form ◽  
Method Development ◽  
Simultaneous Estimation ◽  
Solid Dosage Form ◽  
Solid Dosage ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

Objective: The objective of the study was to develop a new robust, sensitive, precise, accurate RP-HPLC analytical method and validate for simultaneous estimation of ribociclib and letrozole in solid dosage form (tablet). Methods: The chromatographic separation was carried out on Waters, symmetry C18 (150 mm×4.6 mm with 3.5 μm), mobile phase used was a mixture of buffer and acetonitrile in the ratio of 80:20, with flow rate of 1ml/min and injection volume of 10 μL for the assay. The detection was done using PDA at 260 nm, with run time of 5 min. The retention time for the drugs ribociclib and letrozole was detected to be 2.648 min and 3.151 min, respectively. The method was validated according to ICH guidelines. Results: The linearity of letrozole and ribociclib was observed to be in the range of 0.50–7.50 and 40.01–600.15, Correlation coefficient (r2) 0.999 and 0.9983, respectively. Accuracy for ribociclib and letrozole is carried out by repeatable concentrations of 50%, 100%, and 150. Validation factors of robustness and ruggedness were detected to be in limits. Conclusion: The developed method was simple, rapid, and consistent; it can be used for the simultaneous estimation of ribociclib and letrozole tablet dosage form in routine analysis.

scholarly journals Development and Validation of UV-Spectrophotometric Method for Estimation of Metformin Hydrochloride and Pioglitazone in Tablet Dosage Form

2019 ◽  
Vol 9 (4-A) ◽  
pp. 381-384
Author(s):  
Rupali S. Joshi ◽  
Ajit K. Nangare ◽  
Deepali S. Sanap ◽  
Surekha M. Sase
Keyword(s):  
Dosage Form ◽  
Estimation Method ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
Dual Wavelength ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

Simple, sensitive, rapid and accurate UV spectroscopic methods have been developed for the estimation of metformin hydrochloride and pioglitazone in tablet dosage forms. Simultaneous estimation and dual-wavelength methods were developed and validated using solvent methanol. Both drugs show linearity at 5-40 µg/ml for both methods. The suggested techniques have been effectively implemented in pharmaceutical formulations to the evaluation of quoted drugs. Recovery research was conducted to verify the method's accuracy, precision. The techniques have been validated under ICH guidelines. Keywords: Metformin hydrochloride, Pioglitazone, Simultaneous estimation method and Dual wavelength method.

Development and Validation of Stability Indicating Assay Method for Simultaneous Estimation of Glibenclamide and Metformin

2017 ◽  
Vol 8 (03) ◽  
Author(s):  
Waje M. K. ◽  
Barge V. U. ◽  
Talole B. B.
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Chromatographic Procedure ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A high performance reverse phase liquid chromatographic procedure is developed for simultaneous estimation of Metformin and Glibenclamide in combined tablet dosage form. The method was carried out on Agilent Hypersil ODS (4.6 x 250 mm) column with a mobile phase used consisting of Methanol: Water (0.1 % OPA) OPA= Ortho Phosphoric acid (80:20) and the pH of buffer was adjusted to 3 using 2M Orthophosphoric acid. The detection of the combined dosage form was carried out at 228 nm and a flow rate employed was 1 ml/min and column oven temperature at 300C. The retention times of Metformin andGlibenclamide were 3.4667 and 7.3500 minutes respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantification as per ICH norms. The proposed method can be used for the estimation of these combined drugs.

Development and Validation of the Analytical method for the estimation of a combination of 5-fluorouracil and Imiquimod by RP-HPLC

2021 ◽  
pp. 3313-3318
Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.

scholarly journals Application of RP-HPLC for the Estimation of Allopurinol and Its Related Substances in Bulk and Tablet Dosage Form

2021 ◽  
pp. 11-20
Author(s):  
Ch. Jaswanth Kumar ◽  
Prachet Pinnamaneni ◽  
Siva Prasad Morla ◽  
K. N. Rajini Kanth ◽  
Rama Rao Nadendla
Keyword(s):  
Drug Testing ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Related Substance ◽  
Related Substances ◽  
Rp Hplc ◽  
Relative Standard ◽  
Tablet Dosage

Aims: The main aim of the present study was to develop and validate a simple and cost- effective method for the estimation of allopurinol and its related substances by using RP-HPLC. Study Design:  Estimation of Allopurinol and its related substance in bulk and tablet dosage forms by RP-HPLC. Place and Duration of Study: Chalapathi Drug Testing Laboratory, Chalapathi Institute of Pharmaceutical Sciences, Chalapathi Nagar, Lam, Guntur-522034 between October 2020 to January 2021. Methodology: Method development was carried out by using Schimadzu, Prominence-i series LC 3D-Plus autosampler embedded with lab solutions software, equipped with PDA detector using YMC column (150 mm X 4.6 mm, 3 μm) and 0.1M Ammonium acetate buffer as a mobile phase in the ratio of 100% at a flow rate of 1.0 ml/min at a wavelength of 255nm. The developed method was validated according to ICH guidelines. Results:  The linearity was observed in the range of 20-100 µg/ml with a regression (R2) value of 0.999. Developed method was specific with no interactions and accurate with 100.11% for allopurinol and 99.54% for its related substance. The limit of detection for allopurinol was 2 µg/ml and for related substance was 0.0.1 µg/ml. The limit of quantification for allopurinol was 6 µg/ml and for related substance was 0.03 µg/ml respectively. The percentage relative standard deviation was found to be NMT 2 which indicates that the proposed method was precise and robust. Conclusion:  The developed method was simple, precise and accurate and can be successfully employed for the estimation of allopurinol in bulk and tablet dosage form.

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.

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