scholarly journals Synthesis of a new organic probe 4-(4 acetamidophenylazo) pyrogallol for spectrophotometric determination of Bi(III) and Al(III) in pharmaceutical samples

2021 ◽  
Vol 40 (1) ◽  
pp. 108-126
Author(s):  
Jumana W. Ammar ◽  
Zainab A. Khan ◽  
Marwa N. Ghazi ◽  
Naser A. Naser
Keyword(s):  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Scanning Calorimetry ◽  
Spectrophotometric Methods ◽  
Modern Development ◽  
Relative Standard ◽  
Visible Spectra ◽  
Ft Ir ◽  
Linear Solvation Energy

Abstract A modern development discusses the synthesis and validity of simple, sensitive, and versatile spectrophotometric methods for Bi(III) and Al(III) determination in pharmaceutical formulations have been conducted. In the present paper, 4-(4 acetamidophenylazo) pyrogallol has been synthesized as a new organic compound, 4-APAP, by coupling pyrogallol in a regulated pH medium with diazotized p-aminoacetanilide. 4-APAP was identified by methods of FT-IR, 1H-NMR, 13C-NMR, and thermal analysis (thermogravimetry and differential scanning calorimetry). Solvatochromic activity was also studied in solvents with different polarities. The Kamlet and Taft linear solvation energy relationship was used to correlate shifts in UV-Visible spectra of 4-APAP with Kamlet-Taft parameters (α, β, and π*). The optimum assay conditions showed linearity from 0.3–13 to 0.5–11 μg·mL−1 for Bi(III) and Al(III), respectively. Molar absorptivity values were 3.365 × 104 and 0.356 × 104 L·mol−1·cm−1 for Bi(III) and Al(III), with similar Sandell's sensitivity measures of 0.006 and 0.008 μg·cm−2. Detection limits and quantification limits were 0.013 and 0.043 μg·mL−1 for Bi(III), respectively, and 0.018 and 0.059 μg·mL−1 for Al(III) with the relative standard deviation for determination of both metal ions using 4-APAP probe being <2.0%. The validity, accuracy, and efficiency of the approaches were demonstrated by the determination of Bi(III) and Al(III) in different formulations.

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.

Validated Spectrophotometric Determination of Rizatriptan Benzoate in Pharmaceutical Formulations using Alizarin Derivatives

2019 ◽  
Vol 10 (01) ◽  
Author(s):  
El Sheikh R ◽  
Hassan W. S. ◽  
Gouda A. A. ◽  
Al OwairdhiA. ◽  
Al Hassani K K H
Keyword(s):  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Optimum Conditions ◽  
Reaction Conditions ◽  
Alizarin Red ◽  
Rizatriptan Benzoate ◽  
Spectrophotometric Methods ◽  
Relative Standard

Two simple, sensitive, accurate, precise and economical spectrophotometric methods have been developed and validated for the determination of rizatriptan benzoate (RZT) in pure form and pharmaceutical formulations. These methods were based on the formation of charge transfer complex between RZT as n-electron donor and alizarin red S (ARS) or quinalizarin (Quinz) as π-acceptor in methanol to form highly colored chromogens which showed an absorption maximum at 532 and 574 nm using ARS and Quinz, respectively. The optimization of the reaction conditions such as the type of solvent, reagent concentration and reaction time were investigated. Under the optimum conditions, Beer’s law is obeyed in the concentration ranges 1.0-16 and 2.0-20 g mL-1 using ARS and Quinz, respectively with good correlation coefficient (r2 ≥ 0.9996) and with a relative standard deviation (RSD% ≤ 1.16). The molar absorptivity, Sandell sensitivity, detection and quantification limits were also calculated. The methods were successfully applied to the determination of RZT in its pharmaceutical formulations and the validity assesses by applying the standard addition technique. Results obtained by the proposed methods for the pure RZT and commercial tablets agreed well with those obtained by the reported method.

scholarly journals Spectrophotometric Determination of Pipazethate Hydrochloride in Pure Form and in Pharmaceutical Formulations

2007 ◽  
Vol 90 (3) ◽  
pp. 686-692 ◽  
Author(s):  
Ragaa El-Shiekh ◽  
Alaa S Amin ◽  
Faten Zahran ◽  
Ayman A Gouda
Keyword(s):  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Pure Form ◽  
Acetate Buffer Solution ◽  
Buffer Solution ◽  
Accurate Analysis ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Optimum Ph

Abstract Three simple, sensitive, and reproducible spectrophotometric methods (AC) for the determination of pipazethate hydrochloride (PiCl) in pure form and in pharmaceutical formulations are described. The first and second methods, A and B, are based on the oxidation of the drug by Fe3+ in the presence of o-phenanthroline (o-phen) or bipyridyl (bipy). The formation of tris-complex upon reactions with Fe3+-o-phen and/or Fe3+-bipy mixture in an acetate buffer solution of the optimum pH values was demonstrated at 510 and 522 nm, respectively, with o-phen and bipy. The third method, C, is based on the reduction of Fe(III) by PiCl in acid medium and subsequent interaction of Fe(II) with ferricyanide to form Prussian blue, which exhibits an absorption maximum at 750 nm. The concentration ranges are from 0.5 to 8, 2 to 16, and 3 to 15 g/mL for Methods AC, respectively. For more accurate analysis, Ringbom optimum concentration ranges were calculated. The molar absorptivity, Sandell sensitivity, and detection and quantitation limits were calculated. The developed methods were successfully applied to the determination of PiCl in bulk and pharmaceutical formulations without any interference from common excipients. The relative standard deviations were 0.83% with recoveries of 98.9101.15%.

scholarly journals Spectrophotometric Determination of Gemifloxacin Mesylate in Pharmaceutical Formulations Through Ion-Pair Complex Formation

2008 ◽  
Vol 5 (3) ◽  
pp. 515-520 ◽  
Author(s):  
Marothu Vamsi Krishna ◽  
Dannana Gowri Sankar
Keyword(s):  
Methylene Blue ◽  
Acidic Medium ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Basic Medium ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Safranin O

Four simple and sensitive ion-pairing spectrophotometric methods have been described for the assay of gemifloxacin mesylate (GFX) either in pure form or in pharmaceutical formulations. The developed methods involve formation of colored chloroform extractable ion-pair complexes of the drug with safranin O (SFN O) and methylene blue (MB) in basic medium; Napthol blue 12BR (NB 12BR) and azocaramine G (AG) in acidic medium. The extracted complexes showed absorbance maxima at 525, 650, 620 and 540 nm for SFN O, MB, NB 12BR and AG, respectively.Beer's law is obeyed in the concentration ranges 3-15, 4-20, 2-10 and 2-10 μg/mL with molar absorptivity of 2.81 × 104, 2.20 x 104, 4.02 × 104and 4.15 × 104L mole−1cm−1and relative standard deviation of 0.077, 0.104, 0.080 and 0.103% for SFN O, MB, NB 12BR and AG, respectively. These methods have been successfully applied for the assay of drug in pharmaceutical formulations. No interference was observed from common pharmaceutical adjuvants. Results of analysis were validated statistically and through recovery studies.

scholarly journals SPECTROPHOTOMETRIC METHODS FOR DETERMINATION OF SOFOSBUVIR AND DACLATASVIR IN PURE AND DOSAGE FORMS

2021 ◽  
pp. 112-119
Author(s):  
MONIR Z. SAAD ◽  
ATEF AMER ◽  
KHALED ELGENDY ◽  
BASEM ELGENDY
Keyword(s):  
Indigo Carmine ◽  
Reference Method ◽  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Experimental Conditions ◽  
Fixed Amount ◽  
Alizarin Red ◽  
Spectrophotometric Methods

Objective: Two simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sofosbuvir (SOF) and daclatasvir (DAC) in pure forms and pharmaceutical formulations. Methods: The proposed methods are based on the oxidation of SOF and DAC by a known excess of cerium(IV) ammonium nitrate in sulphuric acid medium followed by determination of unreacted cerium(IV) by adding a fixed amount of indigo carmine (IC) and alizarin red S (ARS) dyes followed by measuring the absorbance at 610 and 360 nm, respectively. The experimental conditions affecting the reaction were studied and optimized. Results: The beer’s law was obeyed in the concentration ranges of 0.2-3.0, 0.2-4.0 for SOF and 0.5-4.5 and 0.5-5.0 μg/ml for DAC using IC and ARS methods, respectively with a correlation coefficient ≥ 0.9991. The calculated molar absorptivity values are 2.354 × 104, 1.933 × 104 for SOF and 1.786 × 104 and 2.015 × 104 L/mol. cm for DAC using IC and ARS methods, respectively u. The limits of detection and quantification are also reported. Intra-day and inter-day precision and accuracy of the methods have been evaluated. Conclusion: The methods were successfully applied to the assay of SOF and DAC in tablets and the results were statistically compared with those of the reference method by applying Student’s t-test and F-test. No interference was observed from the common tablet excipients. The accuracy and reliability of the methods were further ascertained by performing recovery studies using the standard addition method.

scholarly journals A sensitive spectrophotometric determination of tadalafil in pharmaceutical preparations and industrial wastewater samples

2013 ◽  
Vol 10 (3) ◽  
pp. 1005-1013 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Standard Deviation ◽  
Industrial Wastewater ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Average Recovery ◽  
Relative Standard ◽  
Wastewater Samples ◽  
Sensitive Spectrophotometric Method

A simple, accurate, precise, rapid, economical and a high sensitive spectrophotometric method has been developed for the determination of tadalafil in pharmaceutical preparations and industrial wastewater samples, which shows a maximum absorbance at 204 nm in 1:1 ethanol-water. Beer's law was obeyed in the range of 1-7?g/ mL ,with molar absorptivity and Sandell ? s sensitivity of 0.783x105l/mol.cm and 4.97 ng/cm2respectively, relative standard deviation of the method was less than 1.7%, and accuracy (average recovery %) was 100 ± 0. 13. The limits of detection and quantitation are 0.18 and 0.54 µg .ml-1, respectively. The method was successfully applied to the determination of tadalafil in some pharmaceutical formulations (tablets) and industrial wastewater samples. The proposed method was validated by sensitivity and precision which proves suitability for the routine analysis of tadalafil in true samples.

scholarly journals Spectrophotometric Methods for the Assay of Pyrilamine Maleate Using Chromogenic Reagents

2010 ◽  
Vol 7 (4) ◽  
pp. 1507-1513 ◽  
Author(s):  
V. Annapurna ◽  
G. Jyothi ◽  
V. Nagalakshmi ◽  
B. B. V. Sailaja
Keyword(s):  
Charge Transfer ◽  
Oxidative Coupling ◽  
Coupling Reaction ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Method Of Least Squares ◽  
Spectrophotometric Methods ◽  
Oxidative Coupling Reaction ◽  
Charge Transfer Complexation

Simple, accurate and reproducible UV spectrophotometric methods were established for the assay of pyrilamine maleate (PYRA) based on the formation of oxidative coupling and precipitation, charge transfer complexation products. Method A includes the oxidative coupling reaction of PYRA with 3-methyl-2-benzathiazolinone hydrazone (MBTH) in presence of Ce(IV). The formation of oxidative coupling product with 4-amino phenazone (4-AP) in presence of K3Fe(CN)6is incorporated in method B. Precipitation/charge transfer complex formation of the PYRA with tannic acid (TA)/Metol-Cr(VI) in method C were proposed. The optical characteristics such as Beers law limits, molar absorptivity and Sandell’s sensitivity for the methods (A-C) are given. Regression analysis using the method of least squares was made to evaluate the slope (b), intercept (a) and correlation coefficient (r) and standard error of estimation (Se) for each system. Determination of pyrilamine in bulk form and in pharmaceutical formulations were also incorporated.

scholarly journals Sensitive Spectrophotometric Methods for the Determination of Ascorbic Acid

2008 ◽  
Vol 5 (1) ◽  
pp. 10-15 ◽  
Author(s):  
H. D. Revanasiddappa ◽  
M. A. Veena
Keyword(s):  
Ascorbic Acid ◽  
Acid Medium ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Spectrophotometric Methods ◽  
Maximum Absorbance ◽  
Hydrochloric Acid Medium ◽  
Subsequent Determination ◽  
Sulphuric Acid Medium

Two simple and sensitive spectrophotometric methods (A and B) have been described for the determination of ascorbic acid. Method A is based on the oxidation of ascorbic acid (AA) by known excess of Se(IV) in hydrochloric acid medium and subsequent determination of unreacted Se(IV) by reacting it with iodide in the same acid medium to liberate iodine, which react with starch to form a stable blue coloured iodine-starch complex, which shows maximum absorbance at 590 nm. Method B is based on the oxidation of ascorbic acid (AA) by known excess of Cr(VI) in sulphuric acid medium and the determination of unreacted Cr(VI) with diphenyl carbazide (DPC) under the same acidic medium to produce a stable red-violet coloured species, which shows a maximum absorbance at 550 nm. The reacted oxidants (in methods A and B) correspond to the AA content. The apparent molar absorptivity values are found to be 1.627×104and 1.641×104L mol-1cm-1for methods A and B, respectively. The proposed methods are simple, sensitive and suitable for the routine analysis of AA in pharmaceutical formulations and in real samples.

scholarly journals Application of Cerium (IV) as an Oxidimetric Agent for the Determination of Ethionamide in Pharmaceutical Formulations

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagib A. S. Qarah ◽  
Sameer A. M. Abdulrahman
Keyword(s):  
Quality Control ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Sample Solution ◽  
Standing Time ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Back Titration ◽  
Bulk Drug

Two simple methods are described for the determination of ethionamide (ETM) in bulk drug and tablets using cerium (IV) sulphate as the oxidimetric agent. In both methods, the sample solution is treated with a measured excess of cerium (IV) solution in H2SO4 medium, and after a fixed standing time, the residual oxidant is determined either by back titration with standard iron (II) solution to a ferroin end point in titrimetry or by reacting with o-dianisidine followed by measurement of the absorbance of the orange-red coloured product at 470 nm in spectrophotometry. In titrimetry, the reaction proceeded with a stoichiometry of 1 : 2 (ETM : Ce (IV)) and the amount of cerium (IV) consumed by ETM was related to the latter’s amount, and the method was applicable over 1.0–8.0 mg of drug. In spectrophotometry, Beer’s law was obeyed over the concentration range of 0.5–5.0 μg/mL ETM with a molar absorptivity value of 2.66 × 104 L/(mol·cm). The limits of detection (LOD) and quantification (LOQ) calculated according to ICH guidelines were 0.013 and 0.043 μg/mL, respectively. The proposed titrimetric and spectrophotometric methods were found to yield reliable results when applied to bulk drug and tablets analysis, and hence they can be applied in quality control laboratories.

scholarly journals New Spectrophotometric Methods for Estimation of Perindopril Erbumine in Bulk and Pharmaceutical Formulations

2014 ◽  
Vol 6 (2) ◽  
pp. 319-327
Author(s):  
A. Unnisa ◽  
K. V. G. Raju ◽  
K. Balaji ◽  
A. N. Jyothi ◽  
T. S. Kumar
Keyword(s):  
Regression Analysis ◽  
Citric Acid ◽  
Pharmaceutical Formulations ◽  
Bulk Sample ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Spectrophotometric Methods ◽  
Perindopril Erbumine ◽  
Detection And Quantification

Three rapid, simple, inexpensive, precise, and accurate spectrophotometric procedures were developed for the determination of Perindopril erbumine (PPE) using cobalt-thiocyanate, citric acid and 2,3- dichloro-5,6-dicyano benzoquinone in bulk sample and in dosage forms. The procedures are based on the coordination complex of the drug (electron donor) and the chromogenic reagents used. The colored products are extracted into non aqueous solvents and measured spectrophotometrically at the optimum ?maxfor each complex. Regression analysis of Beer-Lambert plots showed good correlation in the concentration range of 30-70 µg mL?1, 4-20 µg mL?1 and 20-60 µg mL?1 for cobalt-thiocyanate, citric acid and 2,3- dichloro-5,6-dicyano benzoquinone, respectively. The apparent molar absorptivity, Sandell’s sensitivity, detection and quantification limits were calculated. The developed methods were successfully applied for the determination of PPE in bulk and pharmaceutical formulations without any interference from common excipients and hence can be used for their routine analysis. Keywords: Perindopril erbumine; Spectrophotometry; Cobalt-thiocyanate; Citricacid-acetic anhydride.  © 2014 JSR Publications. ISSN: 2070-0237 (Print); 2070-0245 (Online). All rights reserved.   doi: http://dx.doi.org/10.3329/jsr.v6i2.16106 J. Sci. Res. 6 (2), 319-327 (2014)

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