Use of Acidic Hydrolysis and Diazo Coupling Reaction for Spectrophotometric Determination of Furosemide in Urine and Pharmaceutical Formulation.

Author(s):  
Hawraa Ali ◽  
Sumayha Muhammed

     Simple and rapid spectrophotometric determination of furosemide (FUR) has been investigated .The method is based on acid hydrolysis of FUR to free primary aromatic amine and diazotization followed by coupling with 3, 5 di methyl phenol (3, 5-DMPH) at basic medium. The absorbance was measured at 434 nm, the method was optimized for best condition, and beers’ law is obeyed over the range of 0.4-50 µg.mL-1 with molar absorptivity and sandal’s sensitivity 1.3899 x104 L moL-1 .cm-1 and 0.0238x104 µg.cm-2 respectively. Analysis of solution containing nineteen different concentrations of FUR gave a correlation coefficient of (0.9999) and limit of detection, limit of quantitation were 0.127, 0.464µg.mL-1 respectively. The reaction stoichiometry was evaluated by Job’s and mole ratio method was found to be 1:1(diazotized FUR: 3, 5-DMPH) .The method was applied in synthetic urine and pharmaceutical formulation. The recovery of FUR in spiked urine was satisfactory resulting in the values of (99±3.32) %, the results of the suggested method was compared with available official literature method.

Author(s):  
RUAA MUAYAD MAHMOOD ◽  
HAMSA MUNAM YASSEN ◽  
SAMAR , NAJWA ISSAC ABDULLA AHMED DARWEESH ◽  
NAJWA ISSAC ABDULLA

Simple, rapid and sensitive extractive spectrophotometric method is presented for the determination of glibenclamide (Glb) based on the formation of ion-pair complex between the Glb and anionic dye, methyl orange (MO) at pH 4. The yellow colored complex formed was quantitatively extracted into dichloromethane and measured at 426 nm. The colored product obeyed Beer’s law in the concentration range of (0.5-40) μg.ml-1. The value of molar absorptivity obtained from Beer’s data was found to be 31122 L.mol-1.cm-1, Sandell’s sensitivity value was calculated to be 0.0159 μg.cm-2, while the limits of detection (LOD) and quantification (LOQ) were found to be 0.1086 and 0.3292 μg.ml-1, respectively. The stoichiometry of the complex created between the Glb and MO was 1:1 as determined via Job’s method of continuous variation and mole ratio method. The method was successfully applied for the analysis of pharmaceutical formulation.


2007 ◽  
Vol 4 (4) ◽  
pp. 496-501 ◽  
Author(s):  
M. Vamsi Krishna ◽  
D. Gowri Sankar

Simple, rapid and sensitive spectrophotometric procedures were developed for the analysis of Alfuzosin hydrochloride (AFZ) in pure form as well as in pharmaceutical formulations. The methods are based on the reaction of AFZ with nitrite in acid medium to form diazonium ion, which is coupled with ethoxyethylenemaleic ester (Method A) or ethylcyanoacetate (Method B) or acetyl acetone (method C) in basic medium to form azo dyes, showing absorption maxima at 440, 465 and 490 nm respectively. Beer’s law is obeyed in the concentration of 4-20 μg/mL of AFZ for methods A, B and 3-15 μg/mL of AFZ for method C. The molar absorptivity and sandell’s sensitivity of AFZ- ethoxyethylenemaleic ester, AFZ- ethylcyanoacetate and AFZ-acetyl acetone are1.90 × 104, 0.022; 1.93 × 104, 0.021 and 2.67 × 104L mole-1cm-1, 0.015 μg cm-2respectively. The optimum reaction conditions and other analytical parameters were evaluated. The methods were successfully applied to the determination of AFZ in pharmaceutical formulations.


2019 ◽  
Vol 53 (4) ◽  
Author(s):  
Padmarajaiah Nagaraja ◽  
Naef Ghllab Saeed Al-Tayar ◽  
Anantharaman Shivakumar ◽  
Ashwinee Kumar Shresta ◽  
Avinash K. Gowda

A very simple, sensitive and fairly selective direct spectrophotometric method is presented for the rapid determination of thallium(III) at trace level. The method is based on the oxidation of 2-hydrazono-3-methyl-2,3-dihydrobenzo[d]thiazole hydrochloride (MBTH) by thallium(III) in phosphoric acid medium to form a diazoniumcation, which couples immediately with 10,11-dihydro-5Hdibenzo[b,f]azepine (IDB) at room temperature giving a blue colored species having a maximum absorption at 660 nm. The reaction conditions and other important analytical parameters were optimized.The calibration curve was found to be linear over the range of 0.1-4 μg/mL with molar absorptivity of 4.5 × 104 L mol- cm-1 and Sandell’s sensitivity of 0.00454 μg cm-2. The relative standard deviation and limit of detection have been found to be 0.58% and 0.0147 μg/mL respectively. Almost all common anions and cations are found notto interfering in matrix level of the analytical process. The method has been successfully applied for the determination of thallium(III) in synthetic standard mixtures, water and human urine samples. The performance of proposed method was evaluated in terms of student’s t-test and variance ratio F-test, to find out the significance of proposed method over the reported methods.    


2008 ◽  
Vol 59 (1) ◽  
pp. 3-7
Author(s):  
Aurora Reiss ◽  
Mihaela Mureseanu ◽  
Nicolae Muresan

5-Hydroxy-6-mercapto-benzo [a] phenazine (HMBP) is proposed as a sensitive and selective analytical reagent for the extractive spectrophotometric determination of copper (II). Copper reacts with HMBP to give a dark red complex which is soluble in chloroform. The composition of the CuII � HMBP complex is established as 1:2 by Job�s continuous variation method and molar ratio method. The instability constant of the complex calculated by Job�s relation for nonisomolar series is 4.65 . 10-9, at room temperature. The CuII-HMBP complex in chlorophorm shows a maximum absorbance at 495 nm, with molar absorptivity and Sandell�s sensitivity values of 7.39 . 103dm3 mol-1 cm-1 and 0.012 mg cm-2, respectively. Beer�s law is obeyed in the concentration range 0.67 - 26.90 mg mL-1 and the detection limit is 0.59 mg mL-1. A repetition of the method is checked by finding the relative standard deviation (RSD) at 1.00 mg mL-1 CuII of 0.6%. The method is successfully employed for the determination of copper (II) in environmental samples. The reliability of the method is assured by analysing the standard alloys and by inter-comparison of experimental values, using an atomic absorption spectrometer.


2019 ◽  
Vol 10 (2) ◽  
pp. 1392-1396 ◽  
Author(s):  
Khalaf F Alsamarrai ◽  
Menaa Abdulsalam Al-Abbasi ◽  
Eman Thiab Alsamarrai

A new, sensitive, simple and cheap spectrophotometric method for the determination of Neomycin Sulphate (NEO) in pharmaceutical forms has been developed. The method is based on the reaction between NEO and NIN in basic medium. The maximum absorbance was at 574 nm. The conditions affecting the reaction were optimized. Under the optimal conditions, the calibration curve was linear over the range of 0.0002-0.0011 mol/L. The limit of detection and limit of quantification were 5.423×10-6 mol/L, and 1.643×10-5 mol/L, RSD% of seven replicate was 0.8217- 0.8321% and Rec% was between 99.2168-100.8857%. The proposed method was successfully applied to the determination of NEO tablets form.


2016 ◽  
Vol 24 (2) ◽  
pp. 88-101
Author(s):  
Mohauman Mohammad Al-Rufaie

Abstract A sensitive, simple and rapid spectrophotometric procedure for the assay of trace quantities of sulfadiazine (SDZ) drug as bulk and in diluted solution is characterized. The procedure depends on the diazotization reaction which is produced by coupling SDZ with (4-amino-2-hydroxy acetophenon) (AHA) to produce an intense colored complex spectrophotometrically determined at 410 nm. Beer’s law was applied in the range of concentration 0.5 - 15 ppm; the molar absorptivity and Sandell’s sensitivity were 2.8484 × 104 L mol-1 cm-1 and 0.008 μg cm-2 respectively. The method limit of detection (LOD) was 0.443 μg mL-1 and LOQ (the method limit of quantitation) was 0.249 μg mL-1. The procedure is not based on solvent extraction and the additives and excipients do not significantly influence the developed procedure.


2015 ◽  
Vol 69 (4) ◽  
Author(s):  
Teodora S. Stefanova ◽  
Kiril K. Simitchiev ◽  
Kiril B. Gavazov

AbstractLiquid-liquid extraction (LLE) and cloud point extraction (CPE) of vanadium(V) ternary complexes with 4-(2-pyridylazo)resorcinol (PAR) and 2,3,5-triphenyl-2H-tetrazolum chloride (TTC) were investigated. The optimal conditions for vanadium extraction and spectrophotometric determination were identified. The composition (V : PAR : TTC) of the extracted species was 1 : 2 : 3 (optimal conditions; LLE), 2 : 2 : 2 (low reagents concentrations; LLE), 1 : 1 : 1 (short heating time; CPE), and 1 : 1 : 1 + 1 : 1 : 0 (optimal extraction conditions; CPE). LLE, performed in the presence of 1,2-diaminocyclohexane-N,N,N’,N’-tetraacetic acid and NH4F as masking agents, afforded the sensitive, selective, precise, and inexpensive spectrophotometric determination of vanadium. The absorption maximum, molar absorptivity, limit of detection, and linear working range were 559 nm, 1.95 × 105 dm3 mol−1 cm−1, 0.7 ng cm−3, and 2.2-510 ng cm−3, respectively. The procedure thus developed was applied to the analysis of drinking waters and steels. The relative standard deviations for V(V) determination were below 9.4 % (4-6 × 10−7 mass %; water samples) and 2.12 % (1-3 mass %; steel samples).


2004 ◽  
Vol 1 (5) ◽  
pp. 267-271 ◽  
Author(s):  
G. Krishnamurthy Naidu ◽  
K. Suvardhan ◽  
M. V. Jyothi ◽  
B. S. Sastry ◽  
P. Chiranjeevi

A rapid, selective and sensitive spectrophotometric method for the determination of mosarpide in either pure form or in its formulations in pharmaceutical preparations is described. The method is based on the diazotization coupling reaction of mosapride with 1-naphthol in acidic medium to give red azo dye product with theλmaxof 500 nm and is stable for more than 12 hours at optimum condition, Beer's law is obeyed at concentration of 0.2 to 12 μg mL-1at the wavelength of maximum absorbance. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed method. The developed method is highly reproducible and applied to wide variety of pharmaceutical formulation and the results were compared favourably with the reported method.


2016 ◽  
Vol 11 (2) ◽  
pp. 3540-3551
Author(s):  
Taghreed A. Mohammed ◽  
Mona A. Mohamed

A selective and new spectrophotometric method is described for determination of three antiepileptic drugs; namely lamotrigine (LAM), gabapentin (GAB), and oxcarbazepine (OXC) in drug substances and in drug products using vanillin reagent as the chromogenic agent. The method is based on a coupling reaction between the cited drugs and vanillin reagent in acidic condition. Under optimized conditions, the yellow colored products were measured at 405, 396, and 400 nm respectively. Beer’s law was obeyed at (0.4 – 10), (0.1-10), and (0.5-11) μg/mL, and  the calculated molar absorptivity values are 2.52 x 104, 1.74 x 104, and 2.54 x 104 L/mol/cm for LAM, GAB, and OXC respectively. Sandell sensitivity, the limit of detection (LOD) and limit of quantification (LOQ) were calculated. No interference was observed from common additives found in drug products. The presented method was validated according to ICH guidelines. Statistical comparison of the results was performed using Student's t-test and F-ratio at 95% confidence level, and there was no significant difference between the reference and proposed method with regard to accuracy and precision. The method offers the advantages of rapidity, simplicity and sensitivity and low cost and can be easily applied to resource poor settings without the need for expensive instrumentation and reagents.


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