Print ISSN: 1812-125X

Online ISSN: 2664-2530

Main Subjects : Analytical Chemistry


Indirect Spectrophotometric Determination of Famotidine and Ciprofloxacin Hydrochloride in Pharmaceuticals Using N-Bromosuccinimde and Janus Green B Dye.

Muthanna B Abdullah; Elham S Salih

JOURNAL OF EDUCATION AND SCIENCE, In Press
DOI: 10.33899/edusj.2022.132289.1204

An indirect simple and sensitive spectrophotometric method has been developed for the determination of famotidine (FAM) and ciprofloxacin hydrochloride (CIP) in pure and pharmaceutical dosages. The method is based on the oxidation of FAM and CIP with known excess of N-Bromosuccinimde in acidic medium and subsequent occupation of unreacted oxidant in decolorization of Janus green B dye and measure the absorbance of residual dye at 618 nm. Calibration curves of residual Janus green B dye in the presence of FAM or CIP were rectilinear over the ranges 1.0-10.0 and 1.0-7.5 µg/ml with molar absorptivity 3.61×104 and 5.14×104 l.mol-1.cm-1 respectively. The accuracy (average recovery) was ranged between 99.68 and 100.23% and precision (RSD%) is less than 3.80%. The developed method was successfully applied for the determination of the studied drugs in their pharmaceutical preparations. The results obtained are in agreement with certified values of pharmaceutical preparations and also with standard addition procedure and standard method applied in state company for drugs industry and medical appliance,SDI.

Spectrophotometric estimation of para-aminophenol via oxidative coupling reaction with 4-chlororesorcinol –Application to paracetamol

Hiba Abdul -alsalam Alhafid; Nabeel Sabeeh Otman

JOURNAL OF EDUCATION AND SCIENCE, 2021, Volume 30, Issue 5, Pages 136-146
DOI: 10.33899/edusj.2021.131045.1186

A simple sensitive spectrophotometric method has been suggested for the estimation of pure p-aminophenol(p-AMPL), and p-AMPL results from the hydrolysis of paracetamol(PARL). The suggested method is based on oxidative coupling reaction of p-AMPL with 4-chlororesorcinol (4-CLRL) and potassium periodate to produce a stable, and water-soluble coloured product with maximum absorption at wavelength 556 nm. Beer's law is followed over the range of concentration from 2 to 20 µg p-AMPL. ml-1. The molar absorptivity value is equal to 1.0277×104 l.mol-1cm-1. All factors responsible for the completed reaction and highest intensity of the product have been studied, and the optimal of each factor has been selected. The suggested method was applied in an indirect method for the
determination of paracetamol in tablets and injection after acidic hydrolysis to p-AMPL. The common excipients added did not interfere in the estimation of paracetamol.
The suggested method was applied in an indirect method for the
determination of paracetamol in tablets and injection after acidic hydrolysis to p-AMPL. The common excipients added did not interfere in the estimation of paracetamol.

Spectrophotometric Determination of Amoxicillin Trihydrate by Coupling with Diazotized 2,4-dinitroaniline

Hisham Amin Taher Al-Herki; subhi Mohsin jarullah

JOURNAL OF EDUCATION AND SCIENCE, 2021, Volume 30, Issue 4, Pages 177-192
DOI: 10.33899/edusj.2021.130393.1165

Abstact:
A simple , accurate and sensitive spectrophotometric method has been developed for the determination of amoxicillin trihydrate (AMOX) as pure and in pharmaceutical preparations (capsule) . This method based on the coupling reaction of drug with diazotized 2,4- dinitroaniline reagent in an alkaline medium at 20 ºC to produce an intense red, water-soluble dye that is stable and has a maximum absorption at 555 nm . Beer's law was obeyed over the concentration range 3-16 µg/ml with molar absorptivity of 1.1 x104 l.mol-1.cm-1. The limit of detection(LOD) is 0.1448 µg/ml while the limit of quantitation(LOQ) is 0.4825 µg/ml. The method shows high accuracy (average recovery 100.43%) and precision(relative standard division (RSD) is less than 1.4%).The stoichiometry of the resulting azo dye has been also worked out and it is found to be 1:1 AMOX:Diazotized 2,4-Dinitroaniline.Standard addition method refers to the suggested method is free from interferences from common excipients. The developed method was successfully applied for the determination of studied drug in capsules comparable with the certified content value. .

Spectrophotometric Determination of Salbutamol Sulphate and Mefenamic Acid Using Azur-A Dye in Presence of Oxidizing Agent N-bromosuccinimide

subhi Mohsin jarullah; Asmaa Hamza Abbas Al-Hashemi

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 4, Pages 222-244
DOI: 10.33899/edusj.2020.127113.1072

A simple, accurate and sensitive indirect spectrophotometric method has been developed for the determination of salbutamol sulphate and mefenamic acid in pure forms and in pharmaceutical preparations (capsule, syrup, tablet). This method based on the bromination of the drug with N-bromosuccinimide in acidic medium and the unreacted oxidizing agent react with constant amount of Azur-A dye solution due to bleach their colour and measured the absorbance of the residual colour dye at 606.5 nm.The molar absorptivity for salbutamol sulphate and mefenamic acid are 2.3 × 104 L.mol-1.cm-1 and 8.1× 103 L.mol-1.cm-1 respectively. Beer's Law was obeyed over the concentration range of 1.6 -12.8 µg/ml for salbutamol sulphate and1.6 -13.6 µg/ml for mefenamic acid. The limit of detection (LOD) were 0.0367µg/ml and limit of quantitation (LOQ) were 0.1226 µg/ml for both drugs. In addition, the recovery levels of the drugs were in the range 100.56% and 100.74%. The method was created to be simple, cost-effective and rapid because it does not involve any solvent extraction. The developed method was successfully applied for the determination of the studied drugs.

Spectrophotometric Determination of Thiamine hydrochloride Via Oxidative Coupling Reaction Using 4-Aminoantipyrine

Reem Abed Ahmed Al-Luhaiby; Mohammed Alenizzi

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 4, Pages 62-75
DOI: 10.33899/edusj.2020.126895.1062

A sensitive spectrophotometric method has been developed for the determination of thiamine hydrochloride by oxidative coupling reaction of thiamine with the reagent 4-aminoantipyrine (4-AAP) in the presence of copper sulphate as oxidizing agent in alkaine medium forming a reddish brown colour. The product show maximum absorption at 335 nm. The molar absorptivitiy is 26410.59 l/mol.cm for concentrations obeyed Beer’s law in the range 0.2-18 μg.ml-1. The recovery was 100.93 % with relative standard deviation < 2.0 % for thiamine hydrochloride.Thiamine and reagent 4-AAP product was formed in the ratio of 1:1. The stability constant of the product was 3.39×106 l.mol-1 for thiamine hydrochloride indicating the good stability of this product. The optimum conditions for full colour development are described and the proposed method was applied successfully for determination of thiamine in the pharmaceutical preparation (Neurorubine). The common excipients used as additives in pharmaceutical do not interfere in the proposed method.

Spectrophotometric Determination of Aminophenol Isomers Via Oxidative Coupling Reaction with 4-Aminoantipyrine

Reem Abed Ahmed Al-Luhaiby; Mohammed Alenizzi

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 3, Pages 68-84
DOI: 10.33899/edusj.2020.126543.1041

A spectrophotometric method has been developed for the determination of aminophenol isomers (o-aminophenol, m-aminophenol and p-aminophenol). The method is based on oxidative coupling reaction of these compounds with 4-aminoantipyrine (4-AAP) in the presence of cupper sulphate as oxidizing agent in alkaine medium forming a reddish brown colour. The products show maximum absorption at 440 nm, 480 nm and 445 nm for o-aminophenol, m-aminophenol and p-aminophenol respectively. The molar absorptivities are 8.632×103 ,9.33×103 and 9.1449×103 l.mol-1.cm-1 for concentrations obeyed Beer’s law in the range 1-20, 1-24 and 1-7 μg.ml-1 for the above compounds respectively. The average recovery was ranged between 98.38% and 101.01% with relative standard deviation < 1.6 for all the studied compounds. The 4-AAP products were formed in the ratio of 1:2 aminophenol isomers : 4-AAP. The stability constant of the products was 7.4 ×108, 3.27×108 and 9.94×107 l2.mol-2 for o-aminophenol, m-aminophenol and p-aminophenol products respectively indicating the good stability of these products.

Indirect Spectrophotometric Determination of Cefalexin monohydrate, Ceftriaxone Sodium and Cefotaxim Sodium in Pharmaceuticals Using N-Bromosuccinimde and Evans Blue Dye

mohamed thamer aghwan; Elham Sadullah Al-Talibi

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 3, Pages 11-31
DOI: 10.33899/edusj.2019.125959.1009

An indirect sensitive and selective spectrophotometric method has been developed for the determination of cephalexin monohydrate (CEM) ceftriaxone sodium (CFX) and cefotaxim sodium (CEF) in bulk and pharmaceutical formulation. The method is based on the oxidation of (CEM), (CFX) and (CEF) in hydrochloric acid medium with known excess on N-Bromosuccinimde and subsequent determination of unreacted oxidant by decolorization of Evans blue dye (EB) and measure the absorbance of residual dye at 608 nm. Calibration curves of evans blue dye in the presence of drugs were rectilinear over the ranges 1.0-9.0 , 1.0-8.0 and 1.0-9.0 µg/ml with molar absorptivity 2.75×104 , 9.28×104 and 7.81×104 l.mol-1.cm-1 and average recoveries 98.97, 102.08 and 100.08% for CEM, CFX and CEF respectively with RSD of less than 3.29%. The method was free from interference of many excipients and additives commonly found in pharmaceutical formulations. The developed method was successfully applied for determination of the studied drugs in their pharmaceutical formulation resulted in a good agreement with certified value and standard addition procedure.

Spectrophotometric Assay of Piperazine hexahydrate in Pharmaceutical Formulation with 3,5- Dinitrosalysilic Acid Reagent

Usra Ibrahim Al-Neaimy; USRA Ibrahim Al-Neaimy

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 3, Pages 46-57
DOI: 10.33899/edusj.2020.126231.1023

A simple spectrophotometric method for the determination of piperazine hexa- hydrate was developed. The method was based on the proton transfer reaction with 3,5- dinitrosalicylic acid (DNS) in basic solution to form yellow product showing a maximum absorbance at 410 nm with molar absorptivity of 8350 l/mol.cm . The method is obeyed Beer’s law over the concentration range 0.5-20 µg/ml. The average recovery % of the method is 99.12% and RSD % of the method is less than 2%.
The method was applied for the determination of piperazine hexahydrate in pharmaceutical formulation as elixir and the results were in good agreement with the standard addition method .- - - - - - - - - - - - - - - - - - - - - - - - - - - - - -- - - - - - - - - - - - - - -

Indirect Spectrophotometric Determination of Paracetamol Via Decolorization of Eriochrom Black-T With N-Bromosuccinimide

Theiaa Al-Sabha; Zahraa Jameel Al-Gubouri

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 3, Pages 246-256
DOI: 10.33899/edusj.2020.126846.1060

A simple, precise and sensitive indirect spectrophotometric method is described for the assay of Paracetamol in its pure form and pharmaceutical formulations in the aqueous medium. The method is based on the oxidation of the Paracetamol with an excess of N-Bromosuccinimide (NBS) in alkaline medium and the residual oxidizing agent bleaches the purple-colored Eriochrom black-T (EBT) to colorless species which is measured at 516 nm at room temperature. Calibration graph is linear over 0.5-9 µg mL-1 and molar absorptivity is 3.7×104 L.mol-1.cm-1. The detection and quantification limits were 0.068 and 0.229 µgmL-1 respectively. The accuracy (Average recovery %) is 98.57, and Precision (RSD) is ≤ 1.5. No interference effect has been observed from the excipients that exist in drug formulations. The method has been applied successfully in the determination of the Paracetamol in its commercial formulations (injection, syrup, and tablet), and compared favorably with other spectrophotometric methods used different reagents. The reaction mechanism for the oxidation of Paracetamol and EBT was postulated.

Using of Acetylacetone-formaldehyde Reagent in Spectrophotometric Determination of Aniline in Various Water Samples

Nabeel Othman; Safa Abdul aleem Al- Zakaria; Muna Subhe Abdulla

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 2, Pages 241-249
DOI: 10.33899/edusj.2020.126192.1022

A simple and accurate spectrophotometric method for the estimation of aniline in various water samples was done. The method was based on the condensation reaction of acetyl acetone-formaldehyde(AC-FA) reagent with aniline. to produce a yellow colored product, with maximum absorption at 417 nm, which has good stability at room temperature and it is very soluble in water (the medium of reaction). Beer's law is applied in the concentration range of 2.5 to 50 µg. ml-1 of aniline with a molar absorptivity 3.864×103 l.mol-1.cm-1 and Sandell's sensitivity index 0.0241 µg.cm-2 , a relative error of – 0.51 to +4.15 % and a relative standard deviation of ±0.78 to ±1.28% depending on the concentration level. The study also included the effect of organic compounds on the recovery of aniline in water samples. Aniline is the simple type of primary aromatic amines as it enters into many industrial fields and is considered as an important material. Aniline regarded as major pollutant of water, thus, its estimation was studied in different samples of water such as river, tap and Zamzam well waters.

A Friendly Environment Approach for determination of paracetamol

Hanaa Mahmood

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 2, Pages 230-240
DOI: 10.33899/edusj.2019.125964.1011

Abstract
This paper involves a determination of paracetamol using less environment harmful reagent; the hydroxy analog of the pharmaceutical naproxen replaced a chemical reagent in which it is used as a coupling agent for the diazotized p-aminophenol (the hydrolysis product of paracetamol), the paper offers a determination of an analgesic paracetamol in the presence of high content of another analgesic.
Paracetamol azo-dye exhibits maximum absorption at 500 nm. Beer's law is obeyed over the concentration range from 10 to 650 µg/20ml, (i.e. 0.5-32.5 ppm) with a good sensitivity (molar absorptivity 1.2x104 l.mol-1.cm-1), good precision (RSD better than ±0.275%) and high accuracy (relative error less than + 0.77%), Sandell's sensitivity index is 0.0124µg.cm-2, the limit of detection (LOD) is 0.0030 µg/ml and the limit of quantitation (LOQ) is 0.0101 µg/ml. The method has been successfully applied for determination for paracetamol in dosage forms and its already applicable for the determination of paracetamol in presence of naproxen.

Indirect Spectrofluorometric Determination of Enoxaparin Sodium in Pharmaceutical Formulation (Injection) by Ion Association Complex Formation with Acriflavine Dye

mohamed thamer aghwan; Elham Sadullah Al-talibi

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 2, Pages 45-62
DOI: 10.33899/edusj.2019.125843.1001

A simple, sensitive and selective spectrofluorometric method has been developed for the determination of enoxaparin sodium in bulk and dosage forms (injection). The method was based on the quantitative quenching effect of enoxaparin on the native fluorescence of acriflavine due to the formation of nonfluorescent supramolecular ion issociation complex between the studied drug and acriflavine dye in aqueous solution. The decrease of acriflavine fluorescence was observed at 506 nm after excitation at 402 nm. The relationship between quenching fluorescence intensity and concentration of enoxaparin sodium was linear in the range 0.05-20 µg/ml and with correlation coefficient 0.9990 and with LOD and LOQ 0.011 and 0.035 µg/ml respectively. The average recovery was 100.51% and RSD is less than 3.23%. The stoichiometry of enoxaparin to acriflavine was calculated a 1:4. The method was applied successfully to the determination of enoxaparin form injection samples and the results were in a good agreement with certified value and standard addition procedure.

Spectrophotometric determination of Aspirin and Pyridoxine Hydrochloride using 9- Chloroacridin reagent in aqueous solution

Intisar Adil Shehab; Theiaa Al-Sabha

JOURNAL OF EDUCATION AND SCIENCE, 2020, Volume 29, Issue 1, Pages 60-74
DOI: 10.33899/edusj.2019.125898.1003

This research paper tackles a developed method for Aspirin and Pyridoxine drugs determination in their pure forms and pharmaceutical formulations. It is based on the formation of nucleophilic substitution reaction between given drugs and 9-Chloroacridine forming a reddish orange colours. The products show maximum absorption at 532 nm and 534 nm for Aspirin and Pyridoxine respectively. The method was adhering to the Beer's law over concentration range 0.2-18 and 0.4-24 µg/ml with molar absorptivity values 1.1×104 and 7×103 l. mol-1. cm-1 and average recovery 99.87% and 100.00 % for the given drugs respectively. No observed interferences appeared from the excipients commonly existed in pharmaceuticals. Successfully, application for both Aspirin and Pyridoxine was conducted in their pharmaceutical formulations. The continuous variations and the slope ratio of the products between Aspirin and pyridoxine hydrochloride were followed with 9-chloroacridine. The ratio of 1: 1 was obtained between the above two drugs and the reagent The stability constant of the products was 6.38 x 104 and 9.25 × 104 l / mol for both Aspirin and Pyridoxine Hydrochloride products respectively indicating the good stability of these products.

Spectrophotometric method for the determination of tolnaftate in pharmaceutical preparations

Nief Rahman Ahmed; Nawfal Sheet Mohamad

JOURNAL OF EDUCATION AND SCIENCE, 2018, Volume 27, Issue 1, Pages 35-42
DOI: 10.33899/edusj.1970.161563

Abstract
A simple, accurate, rapid and sensitive visible spectrophotometric method has been developed for the determination of tolnaftate in pure and pharmaceutical preparations. The method is based on the reaction of tolnaftate with potassium permanganate in alkaline medium to form a bluish green colored product with an absorption maximum at 610 nm. Beer’s law was obeyed in the range of 5-60 µg/25ml with a molar absorbitivity of 5.379×104 L.mol.-1.cm-1. The optimum conditions for all color development were described and the proposed method has been successfully applied for the determination of tolnaftate in pharmaceutical preparations. A statistical comparison of these results with those of official method using (t and F) values at 95% confidence level, The calculated t- and F- values did not exceed the theoretical values indicating that there was no significant differences between the precision of the proposed and official method. So that the proposed method can be used as a routine quality control for determination of tolnaftate in pure form and in pharmaceutical formulations.The common excipients and additives did not interfere in the proposed method.