scholarly journals Optimization of a spectrofluorimetric method based on a central composite design for the determination of potassium losartan in pharmaceutical products

2014 ◽  
Vol 50 (3) ◽  
pp. 611-619 ◽  
Author(s):  
Fatma Demirkaya-Miloglu ◽  
Mehmet Emrah Yaman ◽  
Yucel Kadioglu
Keyword(s):  
Central Composite Design ◽  
Reference Method ◽  
Pharmaceutical Products ◽  
Critical Parameters ◽  
Fluorescent Intensity ◽  
Spectrofluorimetric Method ◽  
Acid Molarity ◽  
Development And Validation ◽  
Central Composite

Here, a spectrofluorimetric method for the determination of potassium losartan (PL) in pharmaceutical products is described. The effects of critical parameters, pH, acid molarity, and temperature, on the fluorescence intensity of PL were analyzed, and these parameters were optimized using a central composite design (CCD). The highest fluorescent intensity at excitation (λex) and emission (λem) wavelengths of 248 nm and 410 nm, respectively, was achieved using 0.01 M sulfurous acid (pH 2) at 21.6 °C. Under optimum conditions, the method was linear from 0.025-0.5 µg/mL, with a reasonably high correlation coefficient (0.9993). Furthermore, the method was very sensitive (LOQ, 0.006), accurate (RE, ≤7.06), and precise (%RSD, ≤6.51). After development and validation of the method, samples containing PL were analyzed with this method, and the obtained data were statistically compared with those obtained with a previously published reference method using a two one-sided equivalence test (TOST). According to the data, the results from the proposed and reference assays were equivalent.

Development and validation of RP-UPLC method for the determination of betamethasone dipropionate impurities in topical formulations using multivariate central composite design approach.

2021 ◽  
Author(s):  
Siva Krishna Muchakayala ◽  
Kommera Pavithra ◽  
Naresh Kumar Katari ◽  
Vishnu Murthy Marisetti ◽  
THIRUPATHI DONGALA ◽  
...  
Keyword(s):  
Central Composite Design ◽  
Method Development ◽  
Betamethasone Dipropionate ◽  
Design Approach ◽  
Topical Formulations ◽  
Development And Validation ◽  
Central Composite ◽  
Determination Of Impurities

Current study portrays a specific, accurate, simple and rapid UPLC method development for the determination of impurities present in two different topical formulations (Cream and Ointment) of betamethasone dipropionate. The...

scholarly journals Development and validation of spectrophotometric and spectrofluorimetric methods for determination of cilnidipine

2020 ◽  
Vol 19 (7) ◽  
pp. 1503-1509
Author(s):  
Safwan M. Fraihat ◽  
Hatim S. Al Khatib
Keyword(s):  
Quantitative Methods ◽  
Quantitative Measurement ◽  
Pharmaceutical Preparation ◽  
Fluorescence Emission ◽  
Reference Method ◽  
Drug Formulation ◽  
Pharmaceutical Dosage Form ◽  
Spectrofluorimetric Method ◽  
Development And Validation

Purpose: To develop simple and reliable quantitative methods for the determination of cilnidipine (CLD) in pharmaceutical tablets.Methods: Two simple and sensitive methods (spectrophotometric and spectrofluorimetric) were developed for the determination of cilnidipine (CLD) in pure form and in a pharmaceutical preparation. Spectrophotometric method (A) is based on oxidation of CLD with a known excess amount of Nbromosuccinamide (NBS) in acidic medium, followed by addition of methyl orange indicator and absorbance measurement at 510 nm. The spectrofluorimetric method (B) is based on oxidation of CLD to cerium (IV), followed by measurement of fluorescence emission of Ce (III) at 350 nm. Factors that affect the performance of the two methods were studied and optimized.Results: The spectrophotometric and spectrofluorimetric procedures were successfully used for measuring CLD levels in pharmaceutical dosage form, in the ranges of 2.0 - 25.0 and 0.25 - 11.2 μg/mL, at detection limits of 1.05 and 0.13 μg/mL, respectively. There were no significant differences between the proposed methods and a standard reference method (p < 0.05).Conclusion: The developed methods provide simple and reliable procedures for quantitative measurement of CLD in bulk and tablet forms. Keywords: Cilnidipine, Oxidation, Spectrophotometric, Spectrofluorimetric, Drug formulation

Development and Validation of an Eco-Friendly and Low-Cost Method for the Quantification of Cefepime Hydrochloride in Powder for Injectable Solution Using Infrared (IR) Spectroscopy

2020 ◽  
Vol 16 (4) ◽  
pp. 456-464
Author(s):  
Danilo F. Rodrigues ◽  
Hérida R.N. Salgado
Keyword(s):  
Ir Spectroscopy ◽  
Low Cost ◽  
Pharmaceutical Preparations ◽  
Potassium Bromide ◽  
Pharmaceutical Products ◽  
Injectable Formulation ◽  
Ich Guidelines ◽  
Lactam Ring ◽  
Development And Validation

Background: A simple, eco-friendly and low-cost Infrared (IR) method was developed and validated for the analysis of Cefepime Hydrochloride (CEF) in injectable formulation. Different from some other methods, which employ organic solvents in the analyses, this technique does not use these types of solvents, removing large impacts on the environment and risks to operators. Objective: This study aimed at developing and validating a green analytical method using IR spectroscopy for the determination of CEF in pharmaceutical preparations. Methods: The method was validated according to ICH guidelines and the quantification of CEF was performed in the spectral region absorbed at 1815-1745 cm-1 (stretching of the carbonyl group of β- lactam ring). Results: The validated method showed to be linear (r = 0.9999) in the range of 0.2 to 0.6 mg/pellet of potassium bromide, as well as for the parameters of selectivity, precision, accuracy, robustness and Limits of Detection (LOD) and Quantification (LOQ), being able to quantify the CEF in pharmaceutical preparations. The CEF content obtained by the IR method was 103.86%. Conclusion: Thus, the method developed may be an alternative in the quality control of CEF sample in lyophilized powder for injectable solution, as it presented important characteristics in the determination of the pharmaceutical products, with low analysis time and a decrease in the generation of toxic wastes to the environment.

scholarly journals Carbon dots as absorbance promoter probes for detection of Cu(ii) ions in aqueous solution: central composite design approach

2018 ◽  
Vol 17 (2) ◽  
pp. 245-255 ◽  
Author(s):  
S. A. R. Shahamirifard ◽  
M. Ghaedi ◽  
M. Montazerozohori ◽  
A. Masoudiasl
Keyword(s):  
Aqueous Solution ◽  
Central Composite Design ◽  
Carbon Dots ◽  
Design Approach ◽  
Complexing Agent ◽  
Vis Spectroscopy ◽  
First Time ◽  
Central Composite ◽  
Determination Of Copper

In this work, the use of carbon dots (CDs) as a complexing agent and sensitizer in a polymeric matrix for determination of copper(ii) by UV-vis spectroscopy is reported for the first time.

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 Microtitrimetric determination of a drug content of pharmaceuticals containing olanzapine in non-aqueous medium

2009 ◽  
Vol 15 (2) ◽  
pp. 77-81 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagaraju Rajendraprasad ◽  
Basavaiah Vinay
Keyword(s):  
Standard Deviation ◽  
Aqueous Medium ◽  
Reference Method ◽  
Standard Addition ◽  
Cost Effective ◽  
Pharmaceutical Products ◽  
Relative Standard ◽  
Bulk Drug ◽  
Point Detection

Two simple, rapid, reliable and cost-effective methods based on titrimetry in non-aqueous medium are described for the determination of olanzapine in pharmaceuticals. In these methods, the drug dissolved in the glacial acetic acid was titrated with the acetous perchloric acid with visual and potentiometric end point detection, crystal violet being used as the indicator for visual titration. The methods are applicable over 1-15 mg range of olanzapine. The procedures were applied to determine olanzapine in pharmaceutical products and the results were found to be in a good agreement with those obtained by the reference method. Associated pharmaceutical materials did not interfere. The precision results, expressed by inter-day and intra-day relative standard deviation values, were satisfactory, higher than 2%. The accuracy was satisfactory as well. The methods proved to be suitable for the analysis of olanzapine in bulk drug and in tablets. The accuracy and reliability of the methods were further ascertained by recovery studies via a standard addition technique with percent recoveries in the range 97.51-103.7% with a standard deviation of less than 2%.

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