SPECTROPHOTOMETRIC METHOD FOR THE DETERMINATION OF CEFEPIME, CEFAZOLIN SODIUM AND CEFALOTHIN SODIUM IN PURE AND PHARMACEUTICAL DOSAGE FORMS BY USING NINHYDRIN

Objectives: cefazolin sodium and cefalothin sodium are the broad spectrum of antibiotics, are mainly used to control gram positive and gram negative bacterial infections. Cefepime is used to treat moderate-severe nosocomical pneumonia, infections caused by multi resistant microorganisms.(eg. pseudomonos aeruginosa) and empirical treatment of febrile neutropenia. The objective of our method is to develop an effective, simple and sensitive spectrophotometric method for the assay of the above mentioned drugs in both tablet and in pharmaceutical dosage forms.Methods: The method is based on the reaction of cephalosporin's with ninhydrin reagent in the presence of sodium molybdate by maintaining the pH (5.5) using citrate buffer. The reaction is carried out at a temperature of 100 0C for 10 min for CEPM, 15 min for both CFZS and CFLS. The resulting Ruhemann's purple product having the absorption maximum at 570 nm is measured against the reagent blank.Results: Beer's law is obeyed in the concentration range of (1-10 µg/ml) for cefepime, (2-20 µg/ml) for cefazolin sodium and (6-40 µg/ml) for cefalothin sodium respectively. The correlation coefficient's (r2), molar absorptivity (€), Sandell's sensitivity (s), Limit of detection (LOD) and quantification limits (LOQ) for the studied drugs were calculated. Recovery studies shows that this method is accurate and can be successfully employed for the determination of the studied cephalosporin's.Conclusion: Recovery studies, optical parameters and statistical comparisons justify that the present proposed method can be applied to routine drug formulation in pure and dosage forms and can be recommended for routine analysis and also for quality control of these drugs.Â

Upotreba N,N-dietil-p-fenilenediamin sulfata za spektrofotometrijsko određivanje lijekova iz skupine fenola i amina

Spectrophotometric methods are proposed for the determination of drugs containing a phenol group salbutamol sulphate (SLB), ritodrine hydrochloride (RTD), isoxsuprine hydrochloride (IXP) and drugs containing an aromatic amine group dapsone hydrochloride (DAP), sulfamethoxazole (SFM) and sulfadiazine (SFD) in pharmaceutical dosage forms. The methods are based on coupling of N,N-diethyl-p-phenylenediamine sulphate with the drugs in the presence of KIO4 to give a green colored product (λmax at 670 nm) and a red colored product (λmax at 550 nm), respectively. Linear relationships with good correlation coefficients (0.99860.9996) were found between absorbance and the corresponding concentration of drugs in the range 17, 222, 117, 1.512, 225, and 221 μg mL1 for SLB, RTD, IXP, DAP, SFM and SFD, respectively. Variable parameters such as temperature, reaction time and concentration of the reactants were analyzed and optimized. The RSD of intra-day and inter-day studies was in the range of 0.21.0 and 0.41.0 %, respectively. No interference was observed from common pharmaceutical adjuvants. The reliability and performance of the proposed methods was validated statistically; percentage recovery ranged from 99.5 ± 0.1 to 99.9 ± 0.3 %. Limits of detection were 0.14, 0.21, 0.51, 0.44, 0.33 and 0.37 µg mL1 for SLB, RTD, IXP, DAP, SFM, and SFD, respectively.U radu je predložena spektrofotometrijska metoda za određivanje lijekova s fenolnom skupinom salbutamol sulfat (SLB), ritodrin hidroklorid (RTD), izoksuprin hidroklorid (IXP) i lijekova s aromatskom amino skupinom dapson hidroklorid (DAP), sulfametoksazol (SFM) i sulfadiazin (SFD) u farmaceutskim dozirnim pripravcima. Metode se temelje na reakciji ljekovitih tvari s N,N-dietil-p-fenilendiamin sulfatom u prisutnosti KIO4, pri čemu nastaje zeleni (λmax pri 670 nm), odnosno crveni produkt (λmax pri 550 nm). Apsorbancije linerano ovise o koncentrancijama lijekova uz visok koeficijent korelacije (0,99860,9996) u koncentracijskom području 17, 222, 117, 1,512, 225 i 221 μg mL1 za SLB, RTD, IXP, DAP, SFM i SFD. Analizirani su i optimirani promjenjivi parametri kao što su temperatura, reakcijsko vrijeme i koncentracija reaktanata. Repetibilnost i intermedijarna preciznost iznosile su 0,21,0, odnosno 0,41,0 %. Nije primjećena nikakva interferencija s uobičajenim farmaceutskim pomoćnim sredstvima. Pouzdanost i izvedbene značajke predložene metode validirane su statistički. Povrat analitičke metode bio je od 99,5 ± 0,1 do 99,9 ± 0,3 %. Granice detekcije bile su 0,14, 0,21, 0,51, 0,44, 0,33 i 0,37 µg mL1 za SLB, RTD, IXP, DAP, SFM, odnosno SFD

REDOX REACTION BASED SPECTROPHOTOMETRIC ASSAY OF SOME DRUGS IN PHARMACEUTICALS

Objectives: Pyridoxine hydrochloride (PRC) is used in the treatment of side roblastic anemia's and is also used in a variety of disorders including the treatment of depression. Dobutamine Hydrochloride (DOB) is used in the case of congestive heart failure to increase cardiac output and is also commonly used in the hospital setting as a pharmacologic stress testing agent to identify coronary artery disease. Linezolid (LZD) is a synthetic antibiotic used for the treatment of serious infections caused by gram-positive bacteria that are resistant to several other antibiotics. The main objective of our method is to develop a simple, accurate and sensitive spectrophotometric method for the assay of the above mentioned drugs in both tablet and pharmaceutical dosage forms.Methods: The method is based on the red ox reaction of drugs with Folin Ciocalteu (FC) reagent in sodium carbonate medium and the resulting blue colored chromogen is measured at 755 nm.Results: Beer's law is obeyed in the concentration range of 2.5–30 µg/ml (PRC), 1–10 µg/ml (DOB) and 2.5–70 µg/ml (LZD) respectively, with the corresponding molar absorptivity values of 7.145 X 103, 3.2080 X 104 and 6.299 X 103 l mol-1 cm-1. The method is validated for accuracy, precision, LOD, LOQ, robustness and ruggedness as per the current ICH guidelines.Conclusion: The validated method is successfully applied to quantify PRC, DOB and LZD in their commercial formulations with satisfactory results; hence the method is suitable for the determination of drugs in bulk and pharmaceuticals.Â

Osjetljiva spektrofotometrijska metoda za određivanje sulfonamida u farmaceutskim pripravcima

A new, simple and sensitive spectrophotometric method for the determination of some sulfonamide drugs has been developed. The method is based on the diazotisation of sulfacetamide, sulfadiazine, sulfaguanidine, sulfamerazine, sulfamethazine, sulfamethoxazole and coupling with 8-hydroxyquinoline in alkaline media to yield red coloured products, with absorption maximum at 500 nm. The Beer’s law is obeyed from 0.17.0 µg mL1. The limits of quantification and limits of detection were 0.110.18 and 0.030.5 µg mL1, respectively. Intraday precision (RSD 0.10.5%) and accuracy (recovery 97.3100.8) of the developed method were evaluated. No interference was observed from common adjuvants. The method has been successfully applied to the assay of sulpha drug in the pharmaceutical formulations.U radu je opisana nova, jednostavna i osjetljiva spektrofotometrijska metoda za određivanje sulfonamida. Metoda se temelji na prevođenju sulfacetamida, sulfadiazina, sulfagvanidina, sulfamerazina, sulfometazina i sulfametoksazola u diazoderivate koji kondenzacijom s 8-hidroksikinolinom u alkalnom mediju daju crveno obojene produkte s maksimumom apsorpcije pri 500 nm. Beerov zakon vrijedi u koncentracijskom rasponu 0,17,0 µg mL1. Granice kvantifikacije i granice detekcije su 0,11-0,18, odnosno 0,03-0,05 µg mL-1. Za predloženu metodu procijenjene su intermedirska preciznost (RSD 0.1-0,5%) i točnost (analitički povrat 97,3-100,8). Uobičanjene pomoćne tvari u tabletama ne interferiraju tijekom određivanja. Metoda je uspješno primijenjena za analizu sulfonamida u farmaceutskim pripravcima

Highly Sensetive Reaction for the Estimation of Carbaryl Using 4-4ˊ- Diaminodiphenyl Sulfone in Environmental Samples

A rapid, sensitive Spectrophotometric method for the determination of ultra trace amount of carbaryl (1- Napthyl-N- Methyl Carbamate) is proposed. The method is based on an alkali hydrolysis of carbaryl in the presence of methanolic KOH, followed by coupling with diazotized 4-41- diaminodiphenyl sulfone in an alkaline medium. The water soluble pink dye obtained shows an absorption maximum at 540 nm. The system obeys Beer’s law over the range of 0.06-2.0μg mL-1. The absorptivity of the coloured product is 7.014 × 104 l mol-1 cm-1 and the developed colour is stable for 48h. The detection limit of Carbaryl is 0.0102 μg mL-1. This method is a very good alternative tool and it can be used successfully for the determination of carbaryl residue in environmental water and grain samples

Rapid Spectrophotometric Determination of Trace Amounts of Nitrate-Nitrogen Using Dapsone and α-Naphthol

A simple, rapid and sensitive spectrophotometric method has been developed for the trace determination of nitrite using Dapsone and α-Naphthol. The proposed method is based on the diazotization of Dapsone followed by coupling with α-Naphthol in sodium hydroxide medium to give an intense pink coloured azo dye. The dye shows absorption maximum at 540 nm. The molar absorptivity and Sandell’s sensitivity being 5.749 × 104 l mol-1 cm-1 and 0.24 ng cm-3 respectively. Tolerance limit for interfering ions and complexing agents were reported. Other analytical parameters and applications of the method for analysis of tap water, lake water, and industrial effluents have been investigated