scholarly journals 2-Hydroxy-4-Methoxybenzophenone Oxime as an Analytical Reagent for Copper(II)

2005 ◽  
Vol 2 (2) ◽  
pp. 161-164 ◽  
Author(s):  
Miss Krishna Purohit ◽  
K. K. Desai

2-Hydroxy-4-methoxybenzophenoneoxime (HMBO) was developed as a new analytical reagent for the gravimetric determination of Cu(II). In pH 2.5-9.0 the reagent gives brown coloured precipitate with Cu(II). Spectrophotometric methods revealed that the stoichiometry of the complex is 1:2 (metal: ligand). Beer's law is obeyed up to 31.75 ppm of Cu(II). Molar absorptivity and Sandell's sensitivity at 400 nm were found to be 7.0×102L mol-1cm-1and 0.090 μg/cm2respectively. The stability constant of Cu(II)-HMBO complex is found to be 6.13×109. Gibb’s free energy change for complex formation reaction was found to be -13.93 Kcal/mol. The reagent can be used for the analysis of brass.

2007 ◽  
Vol 4 (1) ◽  
pp. 97-102 ◽  
Author(s):  
S. K. Shingadia ◽  
K. K. Desai

2-Hydroxy-5-methylbenzophenone oxime (HMBO) was developed as a new analytical reagent for the gravimetric determination of divalent copper ion. In pH rang of 3.0 to 6.0, the reagent gives a buff colored precipitate with Cu(II). Job’s method and mole ratio method revealed that the stoichiometry of the complex is 1:2 (metal: ligand). Beer’s law is obeyed up to 61.25 ppm of Cu(II). Molar absorptivity and Sandell’s sensitivity at 400 nm were found to be 6.32 × 102L mol-1cm-1and 0.359 μg/cm2respectively. The stability constant of Cu(II)-HMBO complex is found to be 2.43 × 109. Gibb’s free energy change for complex formation reaction was found to be -12.88 Kcal/mol. The reagent can be used for the analysis of brass and alloy.


2009 ◽  
Vol 6 (2) ◽  
pp. 303-307 ◽  
Author(s):  
Ambily P. Nair ◽  
J. Christine

2-Hydroxy-4-n-propoxy-5-bromoacetophenone oxime (HnPBAO) was developed as a new analytical reagent for the gravimetric determination of pentavalent vanadium ion. In the pH range 4.0-6.0, the reagent gave a brown coloured precipitate with V(V). Job’s method and Mole ratio method revealed that the stoichiometry of the complex is 1:1 (metal: ligand). Beer’s law is obeyed up to 20.38 ppm of V(V). Molar absorptivity and Sandells sensitivity at 450 nm were found to be 10.22 × 102L/mol/cm and 0.049 µg/cm2respectively. The stability constant of V(V)-HnPBAO complex is found to be 1.195 × 106. Gibb’s free energy change for complex formation reaction was found to be –8.34 kcal/mol. The reagent can be used for the analysis of vanadium in ferro-vanadium alloys.


2021 ◽  
Vol 88 (6) ◽  
pp. 982-992
Author(s):  
N. Rajendraprasad

Three simple, economic, selective and accurate and precise spectrophotometric methods are developed for determination of enrofloxacin (EFX) in pharmaceuticals. Method A is based on the measurement of absorbance of EFX in 0.1M HOAc at 315 nm. The ketoxime formation reaction has been employed in method B, in which the absorbance measurement of EFX oxime product at 275 nm is described. The third method (Method C) is indirect one and is based on the oxidation of EFX by cerium(IV), reaction of unreacted cerium(IV) with p-toludine (p-TD) and measurement of coloured solution at 540 nm. The Beer’s law is obeyed in the concentration ranges of 1.2–24, 1–8, and 1–20 μg/mL EFX in methods A, B, and C, respectively, with the corresponding molar extinction coefficients of 1.52×104, 3.86×104, and 6.6×103 L/mol/cm. The regression coefficients of calibration lines are 0.9996, 0.9913, and –0.9965, in methods A, B, and C, respectively. The limits of detection (LOD) and quantification (LOQ) have also been reported for each method. The methods have been validated to check accuracy, precision, robustness and ruggedness. The application of the methods proposed to determine EFX in tablets has been described and the results have been compared with a standard method. The results of validation and application have been found to be with excellent agreement. The standard addition procedure has been adopted in recovery experiments to further ascertain the accuracy of the methods and the results of the experiments are well satisfied. The stability indicating ability of Method A has been studied by subjecting EFX to acid and alkaline hydrolysis, oxidative, thermal and UV degradation followed by measurement of absorbance of resultant EFX solutions at 315 nm. The results of degradation study indicated unsusceptible nature of EFX to any of the stress conditions.


2018 ◽  
Vol 35 (1) ◽  
pp. 55
Author(s):  
N. Rajendraprasad ◽  
K. Basavaiah ◽  
K. B. Vinay

Two new, simple, rapid and reproducible spectrophotometric methods have been developed for the determination of lamotrigine (LMT) both in pure form and in its tablets. The first method (method A) is based on the formation of a colored ion-pair complex (1:1 drug/dye) of LMT with bromocresol green (BCG) at pH 5.02±0.01 and extraction of the complex into dichloromethane followed by the measurement of the yellow ion-pair complex at 410 nm. In the second (method B), the drug-dye ion-pair complex was dissolved in ethanolic potassium hydroxide and the resulting base form of the dye was measured at 620 nm. Beer’s law was obeyed in the concentration range of 1.5-15 μg mL-1 and 0.5-5.0 μg mL-1 for method A and method B, respectively, and the  = corresponding molar absorptivity values are 1.6932 x 104 and 3.748 x 104L mol-1cm-1. The Sandell sensitivity values are 0.0151 and 0.0068 μg cm-2 for method A and method B, respectively. The stoichiometry of the ion-pair complex formed between the dug and dye (1:1) was determined by Job’s continuous variations method and the stability constant of the complex was also calculated. The proposed methods were applied successfully for the determination of drug in commercial tablets.


Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 2039
Author(s):  
Gamal A. E. Mostafa ◽  
Ahmed Bakheit ◽  
Najla AlMasoud ◽  
Haitham AlRabiah

The reactions of ketotifen fumarate (KT) with 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) and 7,7,8,8-tetracyanoquinodimethane (TCNQ) as π acceptors to form charge transfer (CT) complexes were evaluated in this study. Experimental and theoretical approaches, including density function theory (DFT), were used to obtain the comprehensive, reliable, and accurate structure elucidation of the developed CT complexes. The CT complexes (KT-DDQ and KT-TCNQ) were monitored at 485 and 843 nm, respectively, and the calibration curve ranged from 10 to 100 ppm for KT-DDQ and 2.5 to 40 ppm for KT-TCNQ. The spectrophotometric methods were validated for the determination of KT, and the stability of the CT complexes was assessed by studying the corresponding spectroscopic physical parameters. The molar ratio of KT:DDQ and KT:TCNQ was estimated at 1:1 using Job’s method, which was compatible with the results obtained using the Benesi–Hildebrand equation. Using these complexes, the quantitative determination of KT in its dosage form was successful.


2018 ◽  
Vol 33 (2) ◽  
pp. 21
Author(s):  
Kanakapura Basavaiah ◽  
Okram Zenita Devi

Two sensitive spectrophotometric methods are described for the determination of simvastatin (SMT) in bulk drug and in tablets. The methods are based on the oxidation of SMT by a measured excess of cerium (IV) in acid medium followed by determination of unreacted oxidant by two different reaction schemes. In one procedure (method A), the residual cerium (IV) is reacted with a fixed concentration of ferroin and the increase in absorbance is measured at 510 nm. The second approach (method B) involves thereduction of the unreacted cerium (IV) with a fixed quantity of iron (II), and the resulting iron (III) is complexed with thiocyanate and the absorbance measured at 470 nm. In both methods, the amount of cerium (IV) reacted corresponds to SMT concentration. The experimental conditions for both methods were optimized. In method A, the absorbance is found to increase linearly with SMT concentration (r = 0.9995) whereas in method B, the same decreased (r = -0.9943). The systems obey Beer’s law for 0.6-7.5 and 0.5-5.0 μg mL-1 for method A and method B, respectively. The calculated molar absorptivity values are 2.7 X 104 and 1.06 X 105 Lmol-1 cm-1, respectively; and the corresponding sandel sensitivity values are 0.0153 and 0.0039μg cm-2, respectively. The limit of detection (LOD) and quantification (LOQ) are reported for both methods. Intra-day and inter-day precision, and accuracy of the methods were established as per the current ICH guidelines. The methods were successfully applied to the determination of SMT in tablets and the results were statistically compared with those of the reference method by applying the Student’s t-test and F-test. No interference was observed from the common excipients added to tablets. The accuracy and validity of the methods were further ascertained by performing recovery experiments via standard addition procedure.


Author(s):  
MONIR Z. SAAD ◽  
ATEF AMER ◽  
KHALED ELGENDY ◽  
BASEM ELGENDY

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.


2010 ◽  
Vol 7 (4) ◽  
pp. 1507-1513 ◽  
Author(s):  
V. Annapurna ◽  
G. Jyothi ◽  
V. Nagalakshmi ◽  
B. B. V. Sailaja

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.


2011 ◽  
Vol 8 (1) ◽  
pp. 217-225 ◽  
Author(s):  
S. Lakshmi Narayana ◽  
C. Ramachandraiah ◽  
A. Varada Reddy ◽  
Dongyeun Lee ◽  
Jaesool Shim

A simple, rapid, sensitive and inexpensive method has been developed for the determination of trace amounts of palladium(II) using 3,4-dihydroxybenzaldehydeisonicotinoylhydrazone (3,4-DHBINH). The metal ion gives a yellow colored complex with 3,4-DHBINH in acetate buffer of pH 3.0 with 1:1 (metal: ligand) composition. The complex shows maximum absorption at 380 nm. Beer’s law is obeyed in the range 0.5-20.0 ppm of Pd(II). The molar absorptivity, Sandell’s sensitivity and detection limit were found to be 0.53×104L mol-1cm-1, 0.02 μg cm-2and 0.0948 μg mL-1, respectively. The correlation coefficient and regression coefficient of the Pd(II)-3,4-DHBINH complex were 1.08 and 0.04 respectively. Major cations and anions did not show any interference. Anti-microbial activity of the Pd(II)-3,4-DHBINH has been studied. The developed method has been successfully applied to the analysis of Pd(II) in spiked samples. Comparing the results with those obtained using an atomic absorption spectrophotometer tested the validity of the method


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