scholarly journals Development and validation of a microbiological assay for determination of chlorhexidine digluconate in aqueous solution

2013 ◽  
Vol 49 (2) ◽  
pp. 351-358 ◽  
Author(s):  
Flávia Angélica Másquio Fiorentino ◽  
Marcos Antonio Corrêa ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Aqueous Solution ◽  
Pharmaceutical Formulations ◽  
Parallel Line ◽  
Inhibitory Effect ◽  
Microbiological Assay ◽  
Diffusion Method ◽  
Chlorhexidine Digluconate ◽  
Relative Standard ◽  
Pharmaceutical Industries ◽  
Development And Validation

Chlorhexidine (CHX) is a broad-spectrum antiseptic that is used in many topical pharmaceutical formulations. Because there is no official microbiological assay reported in the literature that is used to quantify CHX, this paper reports the development and validation of a simple, sensitive, accurate and reproducible agar diffusion method for the dosage of chlorhexidine digluconate (CHX-D) in an aqueous solution. The assay is based on the inhibitory effect of CHX-D upon the strain of Staphylococcus aureus ATCC 25923, which is used as the test microorganism. The design 3x3 parallel-line model was used. The results were treated statistically by analysis of variance (ANOVA), and they were excellent in terms of linearity (r = 0.9999), presenting a significant regression between the zone diameter of growth inhibition and the logarithm of the concentration within the range of 0.5 to 4.5%. The results obtained were precise, having relative standard deviations (RSD) for intra-day and inter-day precision of 2.03% and 2.94%, respectively. The accuracy was 99.03%. The method proved to be very useful and appropriate for the microbiological dosage of CHX-D in pharmaceutical formulations; it might also be used for routine drug analysis during quality control in pharmaceutical industries.

Development and Validation of a Microbiological Agar Assay for Determination of Thiamphenicol in Soft Capsules

2020 ◽  
Vol 16 (7) ◽  
pp. 806-813
Author(s):  
Yugo Araújo Martins ◽  
Reginaldo dos Santos Sousa ◽  
Cristiani Lopes Capistrano Gonçalves de Oliveira
Keyword(s):  
Pharmaceutical Formulations ◽  
Inhibitory Effect ◽  
Diffusion Method ◽  
Test Microorganism ◽  
Pharmaceutical Sample ◽  
Alternative Methodology ◽  
Reliable Quantification ◽  
Development And Validation ◽  
Kocuria Rhizophila

Background: Thiamphenicol belongs to the amphenicol class of antibiotic and possesses a broad-spectrum antimicrobial activity. An alternative microbiological assay for quantification of thiamphenicol in pharmaceutical formulations has not yet been reported in the literature. Objective: This study aimed to develop and validate an agar diffusion method for quantification of thiamphenicol in soft capsules. Methods: The assay was based on the inhibitory effect of thiamphenicol on the following: a strain of Kocuria rhizophila ATCC 9341, used as the test microorganism, Antibiotic 1culture medium, phosphate buffer pH 6, 0, inoculum at a concentration of 1%, as well as standard and sample solutions at the concentrations of 20.0, 40.0 and 80.0 μg mL-1. Results: The method validation yielded good results for the parameters of linearity, precision, accuracy, robustness and selectivity. The experimental statistic results were analyzed using analysis of variance (ANOVA). The method was found to be linear (r2 = 0.9992) in the range of 20-80 μg mL-1, precise (inter-assay R.S.D = 0.09%), accurate (R.S.D. = 4.65%), specific, and robust. Conclusion: The results demonstrated the validity of the proposed bioassay, which allows for reliable quantification of thiamphenicol in a pharmaceutical sample. An alternative methodology for thiamphenicol determination in routine quality control has been reported herein.

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.

Development and Validation of Stability Indicating UPLC Method for Simultaneous Estimation of Phenylephrine and Fexofenadine in Suspension Dosage Form

2020 ◽  
Vol 13 (5) ◽  
pp. 5069-5074
Author(s):  
Rajitha G ◽  
Geetha Susmita Adepu
Keyword(s):  
Quality Control ◽  
Dosage Form ◽  
Orthophosphoric Acid ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Relative Standard ◽  
Pharmaceutical Industries ◽  
Acquity Uplc ◽  
Development And Validation ◽  
Liquid Chromatographic

Phenylephrine and fexofenadine are widely used products for common cold and allergic conditions. In this study, a simple, reliable, sensitive and economical Ultra Performance Liquid Chromatographic (UPLC) method was developed and validated for the simultaneous estimation of phenylephrine and fexofenadine in suspension dosage form. Efficient chromatographic separation was achieved on Acquity UPLC HSS C18 x 1.8μm column with mobile phase consisting of orthophosphoric acid buffer (pH = 2.8) and acetonitrile (55:45% v/v) at a flow rate of 0.3ml.min-1 and 1μl injection volume. TUV detector was used and detection wavelength was 272nm. The retention times of phenylephrine and fexofenadine were found to be 1.347 and 1.536 ± 0.01 mins respectively. The percentage recoveries of phenylephrine and fexofenadine were 99.93% and 99.31% respectively. The relative standard deviation for assay was found to be <2. The detection and quantification limits were found to be 0.04 and 0.13μg/ml for phenylephrine and 0.21 and 0.65μg/ml for fexofenadine respectively. Thus, the developed UPLC method was simple, rapid, sensitive and economical and it can be applied for the routine quality control analysis of combined dosage forms in quality control laboratories and in pharmaceutical industries.

scholarly journals A fully validated microbiological assay to evaluate the potency of ceftriaxone sodium

2013 ◽  
Vol 49 (4) ◽  
pp. 753-762 ◽  
Author(s):  
Maria Luisa Manfio ◽  
Danielle Araújo Agarrayua ◽  
Jaison Carlosso Machado ◽  
Cleber Alberto Schmidt
Keyword(s):  
Low Cost ◽  
Pharmaceutical Formulations ◽  
Microbiological Assay ◽  
Intermediate Precision ◽  
Chromatography Method ◽  
Beta Lactamases ◽  
Pharmaceutical Samples ◽  
Ceftriaxone Sodium ◽  
Relative Standard ◽  
Liquid Chromatography Method

Ceftriaxone (CFTX) sodium is a third-generation, broad-spectrum cephalosporin that is resistant to beta-lactamases. An alternative bioassay for the assessment of the potency of this drug in pharmaceutical formulations has not been previously reported. Thus, this paper reports the development and full validation of a 3 x 3 agar diffusion bioassay using a cylinder-plate method to quantify CFTX sodium in pharmaceutical samples. The strain Staphylococcus aureus ATCC 6538P was used as the test microorganism, and the results of the proposed bioassay displayed high linearity, precision, accuracy, specificity and robustness. All potency results were statistically analyzed using an analysis of variance (ANOVA) and were found to be linear (r=0.99999) in the range of 16-64 µg/mL, accurate (100.5%), and precise [repeatability: relative standard deviation (RSD)=1.4%; intermediate precision: between-day RSD=2.1% and between-analyst RSD=2.5%]. The specificity of the bioassay was determined by evaluating a degraded sample (50 ºC) at 0, 24 and 48 hours as compared against the results from the pharmacopeial liquid chromatography method for CFTX. The results validated the proposed microbiological assay, which allows reliable quantitation of CFTX in pharmaceutical samples. Moreover, it is a useful, simple and low-cost alternative method for monitoring the quality of this medicine.

scholarly journals Development and validation of a rapid turbidimetric assay to determine the potency of norfloxacin in tablets

2015 ◽  
Vol 51 (3) ◽  
pp. 629-635 ◽  
Author(s):  
Lucas Chierentin ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Inhibitory Effect ◽  
Hplc Method ◽  
Assay Method ◽  
Test Microorganism ◽  
Fluoroquinolone Antibiotics ◽  
Relative Standard ◽  
Significant Difference ◽  
Turbidimetric Assay ◽  
Student’S T ◽  
Development And Validation

Norfloxacin is one of the first commercially available (and most widely used) fluoroquinolone antibiotics. This paper reports the development and validation of a simple, sensitive, accurate and reproducible turbidimetric assay method to quantify norfloxacin in tablets formulations in only 4 hours. The bioassay is based on the inhibitory effect of norfloxacin upon the strain ofStaphylococcus epidermidis ATCC 12228 IAL 2150 used as test microorganism. The assay was performed 3x3 parallel lines like, three tubes for each concentration of reference substance and three tubes for each sample concentration. The results were treated statistically by analysis of variance and were found to be linear (r2 = 0.9999) in the selected range of 25-100 μg mL-1; precise (intra-assay: relative standard deviation (RSD) = 1.33%; inter-assay: RSD = 0.21%), accurate (100.74%) and robust with RSD lower than 4.5%. The student's t-test showed no statistically significant difference between the proposed turbidimetric method and an HPLC method previously validated. However the turbidimetric assay can be used as a valuable alternative methodology for the routine quality control of this medicine, complementary to other physical-chemical methods.

scholarly journals Suitability System of Microbiological Method for Nystatin Potency Determination in the Routine Analysis Using Agar Diffusion Method

2021 ◽  
Vol 3 (4) ◽  
pp. 302-315
Author(s):  
Dalia Essam Eissa ◽  
Engy Refaat Rashed ◽  
Mostafa Essam Eissa
Keyword(s):  
Dosage Form ◽  
Parallel Line ◽  
The United States ◽  
Inhibitory Effect ◽  
Raw Material ◽  
Diffusion Method ◽  
Suitability Analysis ◽  
Time Saving ◽  
Pharmaceutical Dosage Form ◽  
Agar Diffusion

Nystatin is a polyene macrolide antifungal active which is used for the treatment of candidiasis and obtained from some species of Streptomycesbacteria. The present work describes the statistical suitability analysis for regular monitoring of the agar diffusion bioassay in a simple, inexpensive and time-saving process before potency determination. A balanced (symmetrical) two-dose parallel line assay model was applied using the agar well diffusion method for quantification of Nystatin in raw material and finished medicinal dosage form. The routine inspection methodology yielded good results and included calculations by the linear parallel model and by means of regression analysis and verified using analysis of variance (ANOVA). The assay is based on the inhibitory effect of Nystatin upon a standard strain as described in the United States Pharmacopeia (USP). The results of the post validation regular assays were treated statistically by ANOVA and the deviations (expressed as average ± standard deviation) from both raw and column totals were 0.702 ± 0.476 and 0.865 ± 0.468, respectively. The mean value of the variance ratio for regression and parallelism squares were 534.349 ± 212.546 and 0.596 ± 0.345, respectively. The study of Nystatin's ongoing analysis showed that the microbiological assay design is satisfactory with respect to the limiting values for the determination of the potency. The established balanced parallel line assay is reasonably stable and suitable and can be used for the regular drug analysis in routine quality control testing and the quantitation of Nystatin in pharmaceutical dosage form and raw material. Doi: 10.28991/SciMedJ-2021-0304-2 Full Text: PDF

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 Development and Validation of an Agar Diffusion Assay for Determination of Ceftazidime in Pharmaceutical Preparations

2008 ◽  
Vol 91 (1) ◽  
pp. 59-66 ◽  
Author(s):  
Cleber A Schmidt ◽  
Marcelly Carazzo ◽  
Luciane V Laporta ◽  
Celso F Bittencourt ◽  
Marcos R Santos ◽  
...  
Keyword(s):  
Pharmaceutical Preparations ◽  
Inhibitory Effect ◽  
Intermediate Precision ◽  
Agar Diffusion ◽  
Test Microorganism ◽  
Relative Standard ◽  
Alternative Methodology ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract Ceftazidime (CFZ) is a broad spectrum parenterallactam antibiotic of the cephalosporin family. This paper reports the development and validation of an agar diffusion microbiological assay using the cylinder-plate method for determination of CFZ in powder for injection. The validation carried out yielded good results in terms of linearity, precision, accuracy, selectivity, and robustness. The assay is based on the inhibitory effect of CFZ upon the strain of Pseudomonas aeruginosa ATCC 27853 used as the test microorganism. The results of the assays were treated statistically by analysis of variance and were found to be linear (correlation coefficient = 0.999998) in the selected range of 8.032.0 g/mL; precise [repeatability: relative standard deviation (RSD) = 1.11; intermediate precision: between-day RSD = 1.37 and between-analyst RSD = 1.41]; and accurate. The selectivity of the bioassay was evaluated by analysis of degraded samples at 50C, and the results were compared with a pharmacopeial liquid chromatographic method at the time 0, 24, and 48 h. The results demonstrated the validity of the proposed bioassay, which allows reliable quantitation of CFZ in pharmaceutical samples and can be used as a useful alternative methodology for CFZ analysis in routine quality control.

scholarly journals Development and validation of kinetic spectrophotometric method for herbicide bromfenoxim determination

2016 ◽  
Vol 14 (2) ◽  
pp. 115-123
Author(s):  
Emilija Pecev-Marinkovic ◽  
Zora Grahovac ◽  
Snezana Mitic ◽  
Aleksandra Pavlovic ◽  
Ivana Rasic-Misic ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Detection Limit ◽  
Spectrophotometric Method ◽  
Inhibitory Effect ◽  
Sulfanilic Acid ◽  
Hplc Method ◽  
Optimum Conditions ◽  
Relative Standard ◽  
Kinetic Spectrophotometric ◽  
Development And Validation

A kinetic spectrophotometric method for determining the residues of herbicide bromofenoxim (BrFX) has been developed and validated. The proposed method is based on the inhibitory effect of BrFX on the oxidation of sulfanilic acid (SA) by hydrogen peroxide in the presence of Cu(II) ion, which was monitored at 370 nm. The variables affecting the rate of the reaction were investigated and the optimum conditions were established. BrFX can be measured in the range of 0.041 - 0.46 ?g/ml and 0.46 - 13.86 ?g/ml. The detection limit of the method with 3? criteria is 0.0077 ?g/ml. The relative standard deviations for five replicate determinations of 0.041, 0.24 and 0.46 ?g/ml BrFX are 3.0, 5.32 and 2.85%, respectively. This method can be successfully used to determine BrFX concentration in baby juice samples. The HPLC method is used to verify the results. The results obtained for the same samples by the two methods are quite comparable.

Sign in / Sign up

Export Citation Format

Share Document