Padmarajaiah Nagaraja

A sensitive and selective spectrophotometric estimation of catechol derivatives in pharmaceutical preparations.

A sensitive and simple spectrophotometric method for the estimation of catechol and its derivatives like dopamine hydrochloride (DPH), levodopa (LDP), methyldopa (MDP) and adrenaline hydrochloride (ADH) in both pure form and in pharmaceutical formulation, is described. The method is based on the interaction of diazotised sulphanilamide (DSA) with catechol derivatives in the presence of molybdate ions in acidic medium. Absorbance of the resulting red coloured product is measured at 490 nm for pyrocatechol (PCL) and at 500 nm for other catechol derivatives. The colour reaction is stable for 24-30 h. Under optimal conditions, Beers Law range for pyrocatechol was found to be between 0.04 and 2.4 (R.S.D.=0.78%), for DPH was 0.02-2.8 (R.S.D.=0.98%) for LDP was 0.1-2.8 (R.S.D.=1.21%) for MDP was 0.5-7 (R.S.D.=1.41%) and for ADH was 0.5-7 (R.S.D.=1.58%). The method is highly reproducible and specific for these selected catechol derivatives. The common excipients used as additives do not interfere in the proposed method. Analytical data for the determination of the pure compound is presented together with the application of the proposed method to the analysis of some pharmaceutical formulations. The results compare favourably with those of official and reported methods.

A new sensitive and selective spectrophotometric method for the determination of catechol derivatives and its pharmaceutical preparations

A sensitive and simple spectrophotometric method for the estimation of certain catechol derivatives like pyrocatechol (PCL), dopamine hydrochloride (DPH), levodopa (LDP), methyl dopa (MDP) and adrenaline (ADH) in either pure form or in its pharmaceutical formulation is described. The method is based on the interaction of diazotised p-nitro aniline (DPNA) with catechol derivatives in presence of molybdate ions in acidic medium. Absorbance of the resulting red complex is measured at 500-510 nm, respectively, and is stable for 2-10 h. The method is highly reproducible and specific for these selected catechol derivatives. The common excipients used as additives in pharmaceuticals and phenol, hydroquinone, resorcinol, pyrogallol and phloroglucinol do not interfere in the proposed method. Analytical data for determination of the pure compound is presented together with the application of the proposed method to the analysis of some pharmaceutical formulations. The results compare favourably with those of official and reported methods.

Spectrophotometric methods for the determination of certain catecholamine derivatives in pharmaceutical preparations

Two simple, rapid and sensitive spectrophotometric methods for the determination of catecholamine derivatives (pyrocatechol, dopamine, levodopa and methyldopa) are developed. The first method involves the oxidation of o-dihydroxybenzene derivatives by N-bromosuccinimide followed by oxidative coupling with isoniazid leading to the formation of a red-coloured products of maximum absorbance (lambda(max)=480-490 nm). The second method is based on the formation of green to blue complex (lambda(max)=635-660 nm) between o- dihydroxybenzene derivatives and sodium nitroprusside in the presence of hydroxylamine hydrochloride. All measurements of the two procedures are carried out in an alkaline medium at room temperature. The two methods are successfully applied for the determination of dopamine hydrochloride, levodopa and methyldopa in injections and tablets of pharmaceutical preparation. The common excipients used as additives in pharmaceuticals do not interfere in the proposed methods. The reliability of these methods are established by parallel determination with the reported and official methods.

Spectrophotometric determination of isoniazid with sodium 1,2-naphthoquinone-4-sulphonate and cetyltrimethyl ammonium bromide

A rapid, sensitive and simple spectrophotometric method is developed for the determination of isoniazid (INH) with sodium 1,2-naphthoquinone-4-sulphonate and cetyltrimethyl ammonium bromide (CTA) in alkaline medium. Beers law is obeyed in the range of INH concentrations of 2-5.6 mug ml(-1) at the maximum absorption of 500 nm. Sensitivity is enhanced by the addition of CTA. The method is successfully employed for the determination of INH in various pharmaceutical preparations and common excipients used as additives in pharmaceuticals do not interfere in the proposed method.

Spectrophotometric determination of folic acid in pharmaceutical preparations by coupling reactions with iminodibenzyl or 3-aminophenol or sodium molybdate-pyrocatechol

Novel coupling reagents are used for the simple and sensitive spectrophotometric determination of folic acid either in pure form or in its pharmaceutical preparations. The methods are based on the probable diazotization of the p-aminobenzoylglutamic acid obtained after reductive clevage of folic acid, followed by either coupling with iminodibenzyl to give a violet product with lambda(max) of 580nm or coupling with 3-aminophenol to produce an orange yellow-colored product with lambda(max) of 460nm. Sodium molybdate and pyrocatechol are used in the third method and the pale red-colored product formed has a lambda(max) of 490nm. The methods are highly reproducible and have been applied to the determination of folic acid in tablets and the results compare favorably with the official method. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed methods.

Spectrophotometric determination of metronidazole and tinidazole in pharmaceutical preparations.

Sensitive and simple spectrophotometric methods for the determination of metronidazole (MNZ) and tinidazole (TNZ) in either pure form or in its pharmaceutical formulations are described. The first method is based on the interaction of 3-methylbenzothiazolin-2-one hydrazone (MBTH) with MNZ/TNZ (reduced drug) in presence of copper sulphate and pyridine in acidic medium. The resulting yellowish orange products have lambda(max) of 500 and 490 nm, respectively, for MNZ and TNZ and are stable for about 4 h. The second method describes the reaction between reduced diazotised drugs with N-(1-naphthyl)ethylenediamine dihydrochloride (NEDA) in neutral medium to yield pink products which have lambda(max) of 520 and 505 nm, respectively, for MNZ and TNZ, respectively. The products are stable for more than 24 h. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed method. Both the methods are highly reproducible and have been applied to a wide variety of pharmaceutical preparations and the results compare favourably with those of official methods.

Extractive spectrophotometric methods for the assay of sildenafil citrate (Viagra) in pure form and in pharmaceutical formulations

Two simple and sensitive extractive spectrophotometric methods for the determination of sildenafil citrate (SC) are proposed. The methods are based on the formation of ion-association complexes of sildenafil citrate with bromocresol green (BCG, method A) and with chromoxane cyanine R (CCR, method B) in aqueous acidic buffer. The complex species, extractable to chloroform phase, were quantitatively measured at 415 and 460 nm for methods A and B, respectively. Beers law was obeyed in the SC concentration range 1.25-25 mug ml(-1) with a limit of detection 0.16 mug ml(-1) and 1.5-60 mug ml(-1) with a limit of detection 0.18 mug ml(-1), respectively, for methods A and B. The methods have been successfully applied to the analysis of bulk drug and its tablets. No interference was observed from common pharmaceutical adjuvants.

Stability indicating RP-LC determination of sildenafil citrate (Viagra) in pure form and in pharmaceutical samples

A simple, precise, sensitive and stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method has been developed for the quantitation of sildenafil citrate (SC) in pure form and its pharmaceutical formulations. Method employs water and acetonitrile (48:52 v/v) as mobile phase with flow rate of 1 ml min(-1), LiChrospher C18-5 microm (25 x 0.46 cm) column and UV detection set at 245 nm. The internal standard method using piroxicam (PX) as the internal standard is used. The linear dynamic range of SC was found to be 0.05-7.5 microg ml(-1). The proposed method is successfully employed for the determination of SC in the tablets. The excipients present in the formulations do not interfere with the assay procedure. Analytical parameters were calculated and full statistical evaluation is included.

Spectrophotometric method for the determination of paracetamol and phenacetin

A rapid, sensitive and simple spectrophotometric method is proposed for the determination of hydrolysis products of paracetamol (PRL) and phenacetin (PHN) with sodium 1,2-naphthoquinone-4-sulphonate and cetyltrimethyl ammonium bromide (CTA) in alkaline medium. The absorbances are measured at 570 and 500 nm and the molar absorptivities found to be 1.118 x 10(4) and 4.54 x 10(3) l mol-1 cm-1 for PRL and PHN, respectively. The coloured species conforms to Beers law over the range 1-20 micrograms ml-1 for PRL and 2-24 micrograms ml-1 of PHN. The sensitivity is enhanced by the addition of CTA. The method is successfully employed for determination of PRL or PHN in various pharmaceutical preparations and laboratory made tablets and results have been statistically compared with those obtained by the official method.

3-Aminophenol as a novel coupling agent for the spectrophotometric determination of sulfonamide derivatives.

A rapid, simple and sensitive spectrophotometric method for the determination of some sulfa drugs is described. The method is based on the formation of orange yellow colored azo product by the diazotization of sulfonamides, viz., dapsone (DAP), sulfathiazole (SFT), sulfadiazine (SFD), sulfacetamide (SFA), sulfamethoxazole (SFMx), sulfamerazine (SFMr), sulfaguanidine (SFG) and sulfadimidine (SFDd) followed by a coupling reaction with 3-aminophenol in aqueous medium. Absorbance of the resulting orange yellow product is measured at 460 nm and is stable for 6 days at 27 degrees C. Beers law is obeyed in the concentration range of 0.05-8.0 microg/ml at the wavelength of maximum absorption. The method is successfully employed for the determination of sulfonamides in various pharmaceutical preparations and common excipients used as additives in pharmaceuticals do not interfere in the proposed method. Plausible reaction mechanism is proposed for the formation of the azo product.