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 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.

Improved Apparatus for Rapid Mercury Determination by Cold Vapor Atomic Absorption Spectrometry

1983 ◽  
Vol 66 (5) ◽  
pp. 1117-1120
Author(s):  
Lawrence Kupchella ◽  
Augusta Syty ◽  
John J Mahfood
Keyword(s):  
Atomic Absorption ◽  
Analytical Signal ◽  
Absorption Spectrometry ◽  
Water Quality Control ◽  
Injection Port ◽  
Cold Vapor ◽  
Cold Vapor Atomic Absorption ◽  
Relative Standard ◽  
Atomic Absorption Spectrometric

Abstract A glass reaction vessel is described and the convenience and simplicity of its use in cold vapor atomic absorption spectrometric determination of mercury are pointed out. The vessel is easy to construct and requires only 15 s for collection of the analytical signal. It provides for continuous flow of carrier gas, and contains a septum-covered sample injection port, a buret for rapid introduction of reagent, and a drain stopcock. Using this apparatus, the relative standard deviation is 2.9% at the 40 ng Hg/mL level. The detection limit is 1 ng/mL. Applicability of the apparatus is proved by analysis of 3 commercial waste water quality control samples.

scholarly journals Flame Atomic Absorption Spectrometric Determination of Trace Amounts of Nickel after Extraction and Preconcentration onto Natural Modified Analcime Zeolite Loaded with 2-(5-Bromo-2-Pyridylazo)-5-Diethylaminophenol

2005 ◽  
Vol 88 (3) ◽  
pp. 842-846 ◽  
Author(s):  
Darush Afzali ◽  
Mohammad Ali Taher ◽  
Ali Mostafavi ◽  
Mohammad Khayatzadeh Mahani
Keyword(s):  
Atomic Absorption ◽  
Absorption Spectrometry ◽  
Spectrometric Method ◽  
Final Solution ◽  
Flame Atomic Absorption ◽  
Relative Standard ◽  
Analytical Approaches ◽  
Atomic Absorption Spectrometric ◽  
Reference Samples

Abstract Nickel is a moderately toxic element compared with other transition metals. However, inhalation of nickel and its compounds leads to serious problems, including cancer of the respiratory system and a skin disorder, nickel-eczema. Thus, attention has focused on the toxicity of nickel at low concentrations, and the development of reliable, analytical approaches for the determination of trace amounts of nickel is needed. This paper describes a simple, rapid, and sensitive flame atomic absorption spectrometric method for the determination of trace amounts of nickel in various samples after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex on a modified Analcime column in the pH range of 7.5–10.5. The retained analyte on the Analcime is recovered with 5.0 mL 2M nitric acid and determined by flame atomic absorption spectrometry. The detection limit is 20 ng/mL, and the calibration curve is linear for analyte concentrations in the range of 0.1–8 μg/mL final solution, with a correlation coefficient of 0.9993. Eight replicate determinations of nickel at 2 μg/mL in the final solution gave an absorbance of 0.1222, with a relative standard deviation (RSD) of ±1.2%. The interference of a large number of anions and cations was studied, and the proposed method was used for the determination of nickel in various standard reference samples. The accuracy of the proposed method was evaluated by analyzing standard reference samples, and the results were satisfactory (recoveries of &gt;96%; RSD of &lt;3.5%).

scholarly journals An Indirect Atomic Absorption Spectrometric Determination of Trifluoperazine Hydrochloride in Pharmaceutical Formulations Based on Chelate Formation with Palladium(II)

2010 ◽  
Vol 7 (s1) ◽  
pp. S433-S441
Author(s):  
Ameen W. Qasim ◽  
Zuhair A. A. Khammas
Keyword(s):  
Atomic Absorption ◽  
Direct Determination ◽  
Pharmaceutical Formulations ◽  
Mean Value ◽  
Pharmaceutical Dosage Form ◽  
Accuracy And Precision ◽  
Standard Additions ◽  
Optimized Conditions ◽  
Atomic Absorption Spectrometric

A new application of an indirect atomic absorption spectrometric (AAS) method was offered for the assay of low concentration of trifluoperazine hydrochloride (TFPH) in pure and pharmaceutical dosage form with good accuracy and precision. The method is depended on the formation of metal complex between the drug (TFPH) and palladium(II) to form orange-yellowish product extractable in organic solvent prior to its aspiration into an air-acetylene flame and indirectly determined by AAS. Using AA responses, all experimental parameters such as, pH, concentration of palladium, reaction time, extraction time and phase ratio which affect the complexation and extraction of TFPH-Pd(II), have been investigated. Under optimized conditions, linearity was observed in the range of 0.5-17 μg mL-1with detection limit (S/N) of 0.038 μg mL-1, precision in range of 1.18-1.92%, accuracy as the %Erelof 2.4% and recoveries ranged from 101.7 to 104% with mean value of 102.4±0.135. The proposed method was applied for the determination of TFPH in the drug stelazine by both direct calibration and standard additions procedures and found to be 4.88 and 4.87 mg per unite, respectively compared with the stated value of 5 mg per unite. This method is also compared statistically with direct determination by using UV-Vis spectrophotometric technique which is preformed in our laboratory and found to be insignificant at 95% confidence level. All statistical calculations were implemented via the chemsoftware Minitab version 11.

scholarly journals Validated Analytical Spectrofluorimetric Method for Quantitation of Diphenhydramine HCl in Commercial Dosage Forms

2018 ◽  
Vol 1 (4) ◽  
pp. 12-26
Author(s):  
Syed Najmul Hejaz Azmi ◽  
Aisha Al-Mahroqi ◽  
Khoula Al-Mamari ◽  
Shaima Al-Shukaili
Keyword(s):  
Dynamic Range ◽  
Fluorescence Emission ◽  
Reference Method ◽  
Pharmaceutical Formulations ◽  
Ion Pair ◽  
Ratio Method ◽  
Eosin Y ◽  
Stoichiometric Ratio ◽  
Buffer Solution

Diphenhydramine HClis a weakly fluorescent drug having tertiary amine group forming ion pair complex with eosin Y in dichloromethane at pH 5 in disodium hydrogen phosphate-citric acid buffer solution. The complex formation was the basis for the development of new analytical method for determination of active diphenhydramine in pharmaceutical formulations. The stoichiometric ratio between diphenhydramine and eosin Y was studied by mole ratio method and found to be 2:1. The ion-pair complex showed maximum fluorescence emission intensity at 554 nm with excitation at 259 nm. The linear dynamic range was obtained in the concentration range of 2-22 µg mL-1 with a linear equation of FI = 0.361 + 13.675 C. The apparent Gibb’s free energy (ΔGº) was calculated and found to be -80.783 KJ mol-1, confirmed the feasibility of the reaction. The proposed method was successfully applied to the determination of diphenhydramine HCl in pharmaceutical formulations and in good agreement with 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.

Atomic Absorption Spectrometric Determination of Arsenite in Water Samples by Graphite Furnace After Extraction with Ammonium sec-Butyldithiophosphate

1984 ◽  
Vol 67 (2) ◽  
pp. 277-280
Author(s):  
Dipankar Chakraborti ◽  
Kurt J Irgolic ◽  
F Adams
Keyword(s):  
Atomic Absorption ◽  
River Water ◽  
Water Samples ◽  
Graphite Furnace ◽  
Dimethylarsinic Acid ◽  
Relative Standard ◽  
Methylarsonic Acid ◽  
Atomic Absorption Spectrometric ◽  
Hexane Solution

Abstract Arsenite—but not arsenate, methylarsonic acid, or dimethylarsinic acid—is extracted from water samples by 5 mL of a 0.01M hexane solution of rec-dibutylthiophosphate. A 10 μL aliquot of the extract is injected into an atomic absorption spectrometer with a graphic furnace for the determination of arsenic. The calibration curve is linear to 1500 Dg As. Quantities of arsenic as low as 100 ng As (0.2 ppb As when contained in 500 mL) can be confidently determined. The method was tested with natural river water and synthetic river water. The relative standard deviations associated with the recoveries of arsenite from natural water and synthetic river water spiked with arsenite range from 4.8 to 8.0%. Ten to 15 arsenite determinations can be completed in 1h.

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