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 In-house Validation of a Microbiological Assay for Determination of Cefepime in Injectable Preparations

2006 ◽  
Vol 89 (5) ◽  
pp. 1367-1372 ◽  
Author(s):  
Marinês J Souza ◽  
Rosecler R Kulmann ◽  
LucÊlia M Silva ◽  
Daniele R Nogueira ◽  
Estevan S Zimmermann ◽  
...  
Keyword(s):  
Micrococcus Luteus ◽  
Inhibitory Effect ◽  
Fourth Generation ◽  
Intermediate Precision ◽  
Test Microorganism ◽  
Relative Standard ◽  
Significant Difference ◽  
Accurate Comparison ◽  
Alternative Methodology

Abstract Cefepime is a new parenteral cephalosporin that has been described as a fourth-generation, broad-spectrum antibiotic. This paper reports the development and in-house validation of an agar diffusion bioassay using a cylinder-plate method for the determination of cefepime in powder for injection. The validation performed yielded good results in terms of linearity, precision, accuracy, and robustness. The assay is based on the inhibitory effect of cefepime upon the strain of Micrococcus luteus ATCC 10240 used as the test microorganism. The results of assays were treated statistically by analysis of variance (ANOVA) and were found to be linear (r = 0.99993) in the selected range of 8.032.0 g/mL; precise [repeatability: relative standard deviation (RSD) = 1.39%, intermediate precision: between-day RSD = 1.77%, and between-analyst RSD = 1.97%] and accurate. Comparison of bioassay and liquid chromatography by ANOVA showed no significant difference between methodologies. The results demonstrated the validity of the proposed bioassay, which is a simple and useful alternative methodology for cefepime determination in routine quality control.

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 Application of Liquid Chromatography to the Simultaneous Determination of Acetylsalicylic Acid, Caffeine, Codeine, Paracetamol, Pyridoxine, and Thiamine in Pharmaceutical Preparations

2001 ◽  
Vol 84 (3) ◽  
pp. 676-683 ◽  
Author(s):  
Natividad Ramos-Martos ◽  
Francisco Aguirre-Gómez ◽  
Antonio Molina-Díaz ◽  
Luis F Capitán-Vallvey
Keyword(s):  
Salicylic Acid ◽  
Acetylsalicylic Acid ◽  
Simultaneous Determination ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract This paper describes a rapid reversed-phase liquid chromatographic method, with UV detection, for the simultaneous determination of acetylsalicylic acid, caffeine, codeine, paracetamol, pyridoxine, and thiamine in pharmaceutical preparations. A reversed-phase C18 Nucleosil column is used. The mobile phase consists of 2 successive eluants: water (5 min) and acetonitrile–water (75 + 25, v/v; 9 min), both adjusted to pH 2.1 with phosphoric acid. Before determination acetylsalicylic acid is completely converted to salicylic acid by alkaline hydrolysis. Salicylic acid, caffeine, paracetamol, pyridoxine, and thiamine are all detected at 285 nm, whereas codeine is detected at 240 nm. Calibration curves were linear for salicylic acid, caffeine, paracetamol, and pyridoxine in the range of 50–500 mg/L, and for codeine and thiamine in the range of 50–1000 mg/L. The method was applied to the analysis of 13 fortified commercial pharmaceutical preparations. Recoveries ranged from 92.6 to 105.5%, with relative standard deviations of 1.1–5.8%.

scholarly journals Development and Validation of a Liquid Chromatographic Method for the Simultaneous Determination of Estradiol, Estriol, Estrone, and Progesterone in Pharmaceutical Preparations

2009 ◽  
Vol 92 (3) ◽  
pp. 846-854 ◽  
Author(s):  
Phyllis Wilson
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Pharmaceutical Preparations ◽  
Men And Women ◽  
Naturally Occurring ◽  
Vital Functions ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract Progesterone and estrogens are hormones produced in the human body that are essential for regulating many vital functions. The three major estrogens produced by women are estriol, estradiol, and estrone. Progesterone is a naturally occurring hormone in both men and women. Pharmaceuticals containing estrogens alone or estrogens in combination with progesterone are commonly used in therapy. Patients requiring unique combinations of the drugs rely on pharmacies to compound the ingredients. In order to assess the potency of drugs containing combinations of estrogens and progesterone, a method was developed to determine all four ingredients simultaneously. The liquid chromatographic method utilized a Bondapak C18 column with an isocratic mobile phase of acetonitrilewater (50 + 50, v/v) at a flow rate of 1.0 mL/min and temperature of 30C. Under these conditions, the order of elution was estriol, estradiol, and estrone, followed by progesterone. UV detection was at 205 nm to monitor elution of the estrogens, then switched to 270 nm to monitor progesterone. The method was applied to the analysis of pharmacy-compounded drugs containing combinations of the hormones. Validation studies demonstrated that the method is accurate and precise.

scholarly journals Development and Validation of a Chiral HPLC Method for Quantitative Analysis of Enantiomeric Escitalopram

2018 ◽  
Vol 16 (2) ◽  
pp. 165-172 ◽  
Author(s):  
Asma Rahman ◽  
Mohammad Rashedul Haque ◽  
M Muhibur Rahman ◽  
Mohammad A Rashid
Keyword(s):  
Pharmaceutical Preparations ◽  
Enantiomeric Separation ◽  
Hplc Method ◽  
Enantiomeric Purity ◽  
Chiral Hplc ◽  
Average Percentage ◽  
Quantitation Limit ◽  
Relative Standard ◽  
Development And Validation

In the present study a rapid, accurate and precise chiral HPLC method was developed and validated for enantiomeric separation of racemate citalopram and escitalopram according to the guidelines of United States of Pharmacopeia (USP) and International Conference on Harmonization (ICH). The chiral chromatographic separation was achieved with ammonium acetate/ ethanol/ 2-propanol/ methylene dichloride (100 : 150 : 70 : 30, v/v) at a flow rate of 0.5 ml/min using a chiral CD-PH column. The HPLC analyses were monitored at 254 nm. The method showed a good linearity with regression coefficient (r2) of 0.998 in the range of 20.0-70.0 μg/ml for escitalopram. The detection limit (LOD), quantitation limit (LOQ) and average percentage of recovery for escitalopram were found to be 2.54, 7.68 μg/ml and 100.28% to 102.86%, respectively. The percentage of relative standard deviation (%RSD) for intra- and inter- day precision were found as 0.16% and 0.09%, respectively. The established method proved as reproducible with a %RSD value of less than 2 and having the robustness within specified limit. The present study also showed the enantiomeric purity or excess (%ee) of seven pharmaceutical preparations of escitalopram. Thus the proposed chiral method can be applied for the enantiomeric purity determination of escitalopram formulations.Dhaka Univ. J. Pharm. Sci. 16(2): 165-172, 2017 (December)

Development and Validation of a Reversed-Phase Column Liquid Chromatographic Method for the Determination of Five Cephalosporins in Pharmaceutical Preparations

2011 ◽  
Vol 94 (5) ◽  
pp. 1440-1446 ◽  
Author(s):  
Ehab F Elkady ◽  
Samah S Abbas
Keyword(s):  
Binary Mixture ◽  
Sodium Benzoate ◽  
Potassium Phosphate ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Column Liquid Chromatographic ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract A new, simple, rapid, and precise RP-HPLC method has been developed and validated for the determination of five cephalosporins, namely, cefalexin, cefoperazone, ceftriaxone, ceftazidime, and cefepime. The method has been applied successfully for simultaneous determination of cefalexin in a binary mixture with sodium benzoate in a suspension, and cefoperazone in a binary mixture with sulbactam in vials. Chromatographic separation was achieved on a Waters μBondapak® C18 column (250 × 4.6 mm id, 10 μm particle size) using the mobile phase monobasic potassium phosphate (50 mM, pH 4.6)–acetonitrile (80 + 20, v/v) with UV detection. A flow rate of 1 mL/min was applied. Linearity, accuracy, and precision were found to be acceptable over the concentration range of 30–300, 3–30, and 15–120 μg/mL for the studied cephalosporins, sodium benzoate, and sulbactam, respectively. The optimized method proved to be specific, robust, and accurate for QC of the cited drugs in their pharmaceutical preparations.

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 Liquid Chromatographic Determination of Cetirizine in Oral Formulations

2005 ◽  
Vol 88 (2) ◽  
pp. 424-427 ◽  
Author(s):  
Lisiane Bajerski ◽  
Simone G Cardoso ◽  
Isabel Fraçao Diefenbach ◽  
Marcelo Donadel Malesuik ◽  
Silvia Helena Miollo Borgmann
Keyword(s):  
Chromatographic Determination ◽  
Reversed Phase ◽  
Control Analysis ◽  
Solution Ph ◽  
Constant Flow Rate ◽  
Oral Formulations ◽  
Relative Standard ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract The development and validation of a reversed-phase liquid chromatographic (LC) method for the determination of cetirizine dihydrochloride in oral formulations are described. An isocratic LC analysis was performed on a reversed-phase C18 column (250 × 4.6 mm id, 5 μm particle size). The mobile phase was 1% orthophosphoric acid solution, pH 3.0–acetonitrile (60 + 40, v/v), pumped at a constant flow rate of 1.0 mL/min. Measurements were made at a wavelength of 232 nm. The calibration curves were linear over the range of 10–30 μg/mL (r2 = 0.9999). The relative standard deviation (RSD) values for intraday precision were 0.94 and 1.43% for tablets and compounded capsules, respectively. The RSD values for interday precision were 0.13 and 0.82% for tablets and compounded capsules, respectively. Recoveries ranged from 97.7 to 101.8% for tablets and from 98.4 to 102% for compounded capsules. No interferences from the excipients were observed. Because of its simplicity and accuracy, the method is suitable for routine quality-control analysis for cetirizine in tablets and compounded capsules.

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