One titrimetric and two spectrophotometric methods are presented for the assay of metaprolol tartrate (MPT) in bulk drug and in tablets. The methods employ N-bromosuccinimide (NBS) as the oxidimetric reagent and two dyes, methyl orange and indigo carmine as spectrophotometric reagents. In titrimetry, an acidified solution of MPT is treated with a known excess amount of NBS and after a definite time, the unreacted oxidant is determined by iodometric back titration. Spectrophotometry involves adding a measured excess of NBS to MPT in acid medium followed by determination of residual NBS by reacting with a fixed amount of either methyl orange and measuring the absorbance at 520 nm (Method A) or indigo carmine and measuring the absorbance at 610 nm (Method B). In all the methods, the amount of NBS reacted corresponds to the amount of MPT. Reaction conditions have been optimized. Titrimetry allows the determination of 1 - 12 mg of MPT and the calculations are based on a 1: 4 (MPT: NBS) reaction stoichiometry. In spectrophotometry, the measured absorbance is found to increase linearly with the concentration of MPT serving as basis for quantitation. The systems obey Beer’s law for 0.5 - 4.0 μg mL-1 and 1.25 - 10.0 μg mL-1 for method A and method B, respectively. The apparent absorptivities are calculated to 1.07 × 105 be and 4.22 × 104 L mol cm-1 for method A and method B, respectively. The methods developed were applied to the assay of MPT in commercial tablet formulations, and the results were compared statistically with those of a reference method. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition method.

K. Basavaiah

B. C. Somashekar

Titrimetric and Spectrophotometric Determination of Metaprolol tartrate in Pharmaceuticals Using N-Bromosuccinimide

A rapid, highly sensitive high performance liquid chromatographic method has been developed for the determination of finasteride(FNS) in bulk drug and in tablets. FNS was eluted from a ODS C18 reversed phase column at laboratory temperature (30 ± 2°C) with a mobile phase consisting of methanol and water (80+20) at a flow rate of 1 mL min-1 with UV detection at 225 nm. The retention time was ∼ 6.1 min and each analysis took not more than 10 min. Quantitation was achieved by measurement of peak area without using any internal standard. Calibration graph was linear from 2.0 to 30 μg mL-1 with limits of detection (LOD) and quantification (LOQ) being 0.2 and 0.6 μg mL-1, respectively. The method was validated according to the current ICH guidelines. Within-day co efficients of variation (CV) ranged from 0.31 to 0.69% and between-day CV were in the range 1.2-3.2%. Recovery of FNS from the pharmaceutical dosage forms ranged from 97.89 – 102.9 with CV of 1.41-4.13%. The developed method was compared with the official method for FNS determination in its tablet forms.

Determination of Finasteride in Tablets by High Performance Liquid Chromatography

The activated carbon (AC) was used for removal of As(III) and As(V) ions from aqueous solutions. Sorption experiments were conducted using both batch and column systems. The effect of some important parameters on sorption of these by AC was studied. It was found that among the different factors affecting sorption capacity and efficiency in removal of arsenic from aqueous solutions, the effect of pH and the oxidation state were the most prominent. The optimum pH values for removal of As(III) and As(V) from aqueous solutions using AC was found 12 and 3 respectively. Impregnation of AC with sulphur contain organic dyes, it is possible to improve As(III) uptake considerably.

R. Ansari

M. Sadegh

Application of Activated Carbon for Removal of Arsenic Ions from Aqueous Solutions

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 × 102 L mol -1 cm-1 and 0.359 μg/cm2 respectively. 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.

S. K. Shingadia

K. K. Desai

2-Hydroxy-5-methylbenzophenone oxime(HMBO) as an Analytical Reagent for Gravimetric Determination of Cu(II)

There are two series of α, β-unsaturated ketones derived form Biphenyl and 9H-Fluorenyl, and ketones with various substituted benzaldehydes under solvent free conditions using silica-sulphuric acid as a reagent in an oven. The catalyst silica is reusable and the yields of chalcones are more than 90%. These chalcones are characterized by physical constants and spectral data.

G. Thirunarayanan

G. Vanangamudi

Synthesis of Some Aryl Chalcones Using Silica-Sulphuric Acid Reagent under Solvent Free Conditions

A simple, general and efficient method has been developed for the conversion of aldehydes to 1,1-diacetates using acetic anhydride, a catalytic amount of non commercial Keggin heteropolyacid (H6 PalMo11O40) (1% mol) in solvent free conditions at room temperature. Aromatic and aliphatic, simple and conjugated aldehydes were protected with excellent yields.

G. Romanelli

P. Dimitroff

P. Vázquez

J. C. Autino

Chemoselective Preparation of 1,1-Diacetates from Aldehydes, Mediated by a Keggin Heteropolyacid Under Solvent Free Conditions at Room Temperature

Three new simple, sensitive, rapid and economical spectrophotometric Methods (A, B and C) have been developed for the determination of Raloxifene Hydrochloride in pharmaceutical bulk and tablet dosage form. Method A is based on the formation of yellow colored chromogen with 0.1N Sodium hydroxide exhibiting maximum absorbance against the corresponding reagent blank. The method B is based on the reaction of Raloxifene with Ferric chloride and 1, 10-phenanthroline to form blood red colored chromogen. The method C is based on the formation of blood red colored chromogen with Ferric chloride and 2, 2' bipyridyl. The absorbencies of the chromogens were measured at their respective wavelength of maximum absorbance against the corresponding reagent blank. The proposed methods have been successfully applied to the analysis of the bulk drug and its tablet dosage form. The methods have been statistically evaluated and were found to be precise and accurate.

M. Mathrusri Annapurna

M. E. Bhanoji Rao

B. V. V. Ravi Kumar

Spectrophotometric Determination of Raloxifene Hydrochloride in Pharmaceutical Formulations

The millimeter-wave rotational spectra of the excited vibrational states v7=1 and v8=1 of the symmetric top molecule trifluoroacetonitrile, CF3CN, have been analyzed again. The ζ=±1 series have been assigned and the rotational parameters including B7 =2944.9748(14) MHz, q+t=1.4505(16) MHz for v7=1 and B8 =2950.4853(4) MHz, q+t= 3.6035(20) MHz for v8=1states were determined accurately.

Masoud Motamedi

Bahram Vahabzadeh Zargari

New Investigation of Millimeter-Wave Rotational Spectrum of CF3CN in the Excited Vibrational States v7=1 and v8=1

Hydroperoxide at &#945;-position to the aromatic ring is the primary oxidation product formed. In all cases monoalkylbenzenes lead to the formation of benzoic acid. Oxidation in the presence of transition metal salts not only accelerate but also selectively decompose the hydroperoxides. Alkyl naphthalenes mainly produce the corresponding naphthalene carboxylic acids. Hock-rearrangement by the influence of strong acids converts the hydroperoxides to hemiacetals. Peresters formed from the hydroperoxides undergo Criegee rearrangement easily. Alkali metals accelerate the oxidation while CO2 as co-oxidant enhances the selectivity. Microwave conditions give improved yields of the oxidation products.

T. S. S. Rao

Shubhra Awasthi

Oxidation of Alkylaromatics

Analytical Chemistry

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Journal of Chemistry publishes original research articles as well as review articles on all aspects of fundamental and applied chemistry, including biological, environmental, forensic, inorganic, organic, physical and theoretical.

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Journal of Chemistry publishes original research articles as well as review articles on all aspects of fundamental and applied chemistry, including biological, environmental, forensic, inorganic, organic, physical and theoretical.

Journal of Chemistry