scholarly journals Implementation of Quality by Design for the Development and Validation of Pioglitazone Hydrochloride by RP-UPLC with Application to Formulated Forms

2012 ◽  
Vol 2012 ◽  
pp. 1-11 ◽  
Author(s):  
Cijo M. Xavier ◽  
Kanakapura Basavaiah
Keyword(s):  
Quality By Design ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Process Understanding ◽  
Validation Criteria ◽  
Relative Standard ◽  
Level Of Knowledge ◽  
Bulk Drug ◽  
Development And Validation

Quality by Design (QbD) is a philosophy that refines the level of knowledge associated with a product that uses process understanding to deliver a product with the desired critical quality attributes. The objective of this study was to develop an integrated multivariate QbD approach to develop and quantify the constituent concentrations of pioglitazone hydrochloride (PGZ) drug in its pure and formulated forms. To facilitate studies investigating the determination of PGZ in bulk drug and its pharmaceutical formulations, a rapid UPLC method was developed and validated for the determination of PGZ accompanied by its degradation studies in different stress conditions. The method fulfilled validation criteria and was shown to be sensitive, with limits of detection (LOD) and quantitation (LOQ) of 0.01 and 0.05 μg mL−1, respectively. The percent relative standard deviations for robustness and ruggedness were observed within the range of 0.1–1.74. The calibration graph was linear in the range of 0.05–300 μg mL−1. The applicability of the method was shown by analysis of formulated drug samples and spiked human urine. The proposed method can be used for routine analysis in quality controlled laboratories for its bulk and formulated product and this is the first reported UPLC method for the assay of PGZ.

scholarly journals Quality by Design Approach for the Development and Validation of Glipizide, an Antidiabetic Drug, by RP-UPLC with Application to Formulated Forms and Urine

2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Cijo M. Xavier ◽  
Kanakapura Basavaiah ◽  
K. B. Vinay ◽  
N. Swamy
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
Quality By Design ◽  
Calibration Graph ◽  
Multivariate Approach ◽  
Antidiabetic Drug ◽  
Validation Criteria ◽  
Relative Standard ◽  
Quality By Design Approach ◽  
Development And Validation

Quality by design (QbD) refers to the achievement of certain predictable quality with desired and predetermined specifications. The objective of this study was to develop and demonstrate an integrated multivariate approach to develop and quantify the constituent concentrations of glipizide (GPZ) drug in its pure and tablet forms. The method was developed using Zorbax Extend C-18 (50 mm × 4.6 mm × 1.8 μm) column with mobile phase consisting of a mixture of phosphate buffer of pH 3.5 and acetonitrile (60 : 40 v/v). The method fulfilled validation criteria and was shown to be sensitive, with limits of detection (LOD) and quantitation (LOQ) of 0.001 and 0.005 μg mL−1, respectively. The percentage relative standard deviations for robustness and ruggedness were observed within the range of 0.1 and 0.99. The calibration graph was linear in the range of 0.005–300 μg mL−1. The applicability of the method was shown by the analysis of formulated drug and spiked urine samples. The proposed method can be used for routine analysis in quality control laboratories for its bulk and formulated product, and this is the first UPLC method reported for the assay of GPZ in bulk, formulated form and urine.

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.

scholarly journals Development and Validation of Spectrophotometric, Atomic Absorption and Kinetic Methods for Determination of Moxifloxacin Hydrochloride

2011 ◽  
Vol 6 ◽  
pp. ACI.S8090 ◽  
Author(s):  
Lobna M. Abdellaziz ◽  
Mervat M. Hosny
Keyword(s):  
Atomic Absorption ◽  
Kinetic Method ◽  
Reference Method ◽  
Pharmaceutical Formulations ◽  
Ion Pair ◽  
Relative Standard ◽  
Formed Precipitate ◽  
Development And Validation ◽  
Atomic Absorption Spectrometric

Three simple spectrophotometric and atomic absorption spectrometric methods are developed and validated for the determination of moxifloxacin HCl in pure form and in pharmaceutical formulations. Method (A) is a kinetic method based on the oxidation of moxifloxacin HCl by Fe3+ ion in the presence of 1,10 o-phenanthroline (o-phen). Method (B) describes spectrophotometric procedures for determination of moxifloxacin HCl based on its ability to reduce Fe (III) to Fe (II), which was rapidly converted to the corresponding stable coloured complex after reacting with 2,2’ bipyridyl (bipy). The formation of the tris-complex formed in both methods (A) and (B) were carefully studied and their absorbance were measured at 510 and 520 nm respectively. Method (C) is based on the formation of ion- pair associated between the drug and bismuth (III) tetraiodide in acidic medium to form orange—red ion- pair associates. This associate can be quantitatively determined by three different procedures. The formed precipitate is either filtered off, dissolved in acetone and quantified spectrophotometrically at 462 nm (Procedure 1), or decomposed by hydrochloric acid, and the bismuth content is determined by direct atomic absorption spectrometric (Procedure 2). Also the residual unreacted metal complex in the filtrate is determined through its metal content using indirect atomic absorption spectrometric technique (Procedure 3). All the proposed methods were validated according to the International Conference on Harmonization (ICH) guidelines, the three proposed methods permit the determination of moxifloxacin HCl in the range of (0.8-6, 0.8-4) for methods A and B, (16-96, 16-96 and 16-72) for procedures 1-3 in method C. The limits of detection and quantitation were calculated, the precision of the methods were satisfactory; the values of relative standard deviations did not exceed 2%. The proposed methods were successfully applied to determine the drug in its pharmaceutical formulations without interference from the common excipients. The results obtained by the proposed methods were comparable with those obtained by the reference method.

scholarly journals Extractive Spectrophotometric Determination of Nortriptyline Hydrochloride Using Sudan II, IV and Black B

2001 ◽  
Vol 69 (2) ◽  
pp. 151-160
Author(s):  
A. Amin ◽  
H. Saleh
Keyword(s):  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Calibration Graph ◽  
Official Method ◽  
Spectrophotometric Methods ◽  
Sudan Black B ◽  
Relative Standard ◽  
Nortriptyline Hydrochloride

A simple spectrophotometric methods has been developed for the determination of nortriptyline hydrochloride in pure and in pharmaceutical formulations based on the formation of ion-pair complexes with sudun II (SII), sudan (IV) (SIV) and sudan black B (SBB). The selectivity of the method was improved through extraction with chloroform. The optimum conditions for complete extracted colour development were assessed. The absorbance measurements were made at 534, 596 and 649 nm for SII, SIV and SBB complexes, respectively. The calibration graph was linear in the ranges 0.5- 280. 0.5- 37.5 and 0.5 – 31.0 μg ml−1 of the drug usiny the same reagents, respectively. The precision of the procedure was checked by calculating the relative standard deviation of ten replicate determinations on 15 μg ml−1 of nortriptyline HCI and was found to be 1.7, 1.3 and 1.55% using SII, SIV, and SBB complexes, respectively. The molar absorptivity and Sandell sensitivity for each ion-pair were calculated. The proposed methods were successfully applied to the deterniination of pure nortriptyline HCI and in pharmaceutical formulations, and the results demonstrated that the method is equally accurate, precise and reproducible as the official method.

scholarly journals Development and Validation of New Chromatographic Method for the Determination of Enantiomeric and Diastereomeric Purity of Solifenacin Succinate: An Antimuscarinic Agent

2011 ◽  
Vol 2011 ◽  
pp. 1-7 ◽  
Author(s):  
Shashikant B. Landge ◽  
Sanjay A. Jadhav ◽  
Sunil B. Dahale ◽  
Navanath C. Niphade ◽  
Ch. Lakshmi Narayana ◽  
...  
Keyword(s):  
Pharmaceutical Formulations ◽  
Antimuscarinic Agent ◽  
Column Temperature ◽  
Solifenacin Succinate ◽  
Drug Manufacturing ◽  
Phase Liquid ◽  
Bulk Drug ◽  
Development And Validation ◽  
Liquid Chromatographic

A new, simple, and rapid stereoselective normal phase-liquid chromatographic (NP-LC) method was developed to separate and quantify the solifenacin succinate and its three stereoisomers. The stereoisomeric separation was achieved on Chiralpak IC ( mm ID) column. The mobile phase was consisting of n-hexane, ethanol, isopropyl alcohol, and diethylamine in the ratio (60 : 15 : 25 : 0.1, v/v/v/v), and the flow rate was maintained at 1.0 mL min−1. UV detection was carried out at 220 nm. In addition, chiroptical detection was carried out using laser polarimeter to understand the elution orders. Resolution between all the stereoisomers was not less than 3. Effect of column temperature on resolution between the stereoisomers was studied. The method was validated as per ICH guideline and found to be robust. The proposed NP-LC method was successfully applied to the analysis of commercial formulation. The method could be of use not only for routine evaluation of the quality of solifenacin succinate in bulk drug manufacturing unit but also for detection of impurities in pharmaceutical formulations.

scholarly journals Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

scholarly journals Determination of Phenylephrine Hydrochloride by Flow Injection Analysis with Chemiluminescence Detection

2001 ◽  
Vol 84 (1) ◽  
pp. 13-18 ◽  
Author(s):  
Yolanda Fuster Mestre ◽  
Luis Lahuerta Zamora ◽  
José Martínez Calatayud
Keyword(s):  
Flow Injection ◽  
Flow Injection Analysis ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Chemiluminescence Detection ◽  
Phenylephrine Hydrochloride ◽  
Sulfuric Acid Medium ◽  
Sample Throughput ◽  
Relative Standard

Abstract A new method is proposed for the determination of phenylephrine hydrochloride by flow injection analysis with direct chemiluminescence detection. The method is based on the oxidation of the drug by potassium permanganate in sulfuric acid medium at 80°C. The calibration graph is linear over the range 0.03–8 ppm phenylephrine hydrochloride, with a relative standard deviation (n = 51, 0.5 ppm) of 1.1% and sample throughput of 134/h. The influence of 38 different foreign compounds was tested, and the method was applied to the determination of phenylephrine hydrochloride in 8 different pharmaceutical formulations.

scholarly journals Development and validation of UV-spectrophotometric methods for quantitative estimation of Prothionamide in pure and pharmaceutical dosage forms

2015 ◽  
Vol 4 (7) ◽  
pp. 402-404 ◽  
Author(s):  
Sujit Kumar Debnath ◽  
S. Saisivam ◽  
Dillip Kumar Dash ◽  
Monalisha Debnath
Keyword(s):  
Quantitative Estimation ◽  
Pharmaceutical Formulations ◽  
Pharmaceutical Journal ◽  
Routine Practice ◽  
Pharmaceutical Dosage Forms ◽  
Spectrophotometric Methods ◽  
Validation Parameters ◽  
Bulk Drug ◽  
Development And Validation

UV Spectrophotometric method was developed and validated for the quantitative determination of Prothionamide in bulk drug and in pharmaceutical formulations. Prothionamide shows the maximum absorbance at 288 nm in phosphate buffer (pH 7.4). Prothionamide follows Beer’s law in the concentration range of 4-20 µg/ml (r2 = 0.999). The detection limit (DL) and quantitation limit (QL) were 0.406 and 1.229 µg/ml respectively. Accuracy and precision were found to be satisfactory. The developed methods were validated according to ICH guidelines. All the validation parameters were found to be satisfactory accordance with the standard values. Therefore, the proposed method can be used for routine practice for the determination of Prothionamide in assay of bulk drug and pharmaceutical formulations.International Current Pharmaceutical Journal, June 2015, 4(7): 402-404

LC Method Development and Validation for the Determination of Ropivacaine Hydrochloride in Bulk Drug and Pharmaceutical Formulations

2017 ◽  
Vol 51 (1) ◽  
pp. 71-80
Author(s):  
Sridevi Chigurupati ◽  
Raju Nemela Appala ◽  
Kesavanarayanan Krishnan Selvarajan ◽  
Chu How Khaw ◽  
Chun Foo Teoh ◽  
...  
Keyword(s):  
Method Development ◽  
Pharmaceutical Formulations ◽  
Method Development And Validation ◽  
Bulk Drug ◽  
Ropivacaine Hydrochloride ◽  
Development And Validation
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