A new, Simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sulfanilamide (SNA) drug in pure and in synthetic sample. This method based on the reaction of sulfanilamide (SNA) with 1,2-napthoquinone-4-sulphonic acid (NQS) to form N-alkylamono naphthoquinone by replacement of the sulphonate group of the naphthoquinone sulphonic acid by an amino group. The colored chromogen shows absorption maximum at 455 nm. The optimum conditions of condensation reaction forms were investigated by: (1) univariable method, by optimizing the effect of experimental variables; (different bases, reagent concentration, borax concentration and reaction time), (2) central composite design (CCD) including the effect of three experimental factors (reagent concentration, borax concentration, and reaction time). The linearity ranges of sulfanilamide are (5-30 µg.mL -1 ) at 455 nm with molar absorptivity (6.9568×10 4 - 7.0774×10 4 L.mol -1 .cm -1 ), Sandell's sensitivity index (2.4753 - 2.4330 μg.cm -2 ) and detection limit of (0.546 – 0.536 µg.mL -1 ) for each procedure respectively. The results showed there are no interferences of excipients on the determination of the drug. The proposed method has been successfully applied for the determination of sulfanilamide in pure and in synthetic sample. Keywords: Spectrophotometric determination, Sulfanilamide, Central composite design, 1, 2-napthoquinone-4-sulphonic acid (NQS).
A simple, sensitive, accurate and low cost effective spectrophotometric method has been developed for the determination of Tetracycline and Doxycycline in pure and pharmaceutical formulations. The method is based on the reaction of methyldopa with 4-aminoantipyren (4-AAP) in presence of potassium ferriecyanide (PFC) in an alkaline medium. Two optimization methods were applied to determine the optimum conditions of oxidizing coupling reaction variables; univariate and design of experiment (DOE) method. The conditions effecting the reaction; pH, buffer Volume, reagent concentration, oxidant concentration, type of buffer, order of addition, time of reaction and stability were optimized . Under univariate and design
... Show MoreA new, simple, rapid and sensitive spectrophotometric method for the determination of sulfamethoxazole in both pure form and pharmaceutical preparations has been reported.The adapted technique based on utilization 4-aminobenzene sulfonic acid as a new modern chromogenic through an oxidative coupling reaction with sulfamethoxazole and potassium iodate in basic media to form orange soluble dye product with absorption maxima at 490 nm. Subject to Beer's law in the range 2–32μg mL-1. The values of molarabsorption coefficient (ε) and correlation coefficient were found to be 9.118 × 103 and0.9999 respectively whereas the Sandels index was
... Show MoreCeftriaxone sodium were one of the widely antibacterial drugs used. Azo dye derivatization of diazonium salt that formed via the reaction between ceftriaxone with hydrochloric acid and sodium nitrite was developed for the on-research drug analysis then coupling with each one 2,5-dimethylphenol (2,5-DMP) and 4-tertbutylphenol (4-TBP) respectively in the alkaline media. The developed diazonium coupling methods include an optimization study. The results show a limit of detection and limit of quantification 0.482, 0.284 µg/mL, and 1.607, 0.945 µg/mL using 2,5-DMP and 4-TBP reagents respectively. Moreover, the recovery % obtained was 100.89%, and 103.37% at linear concentration range 3.0 – 50, and 10 – 30 µg/mL, with mo
... Show MoreA rapid and sensitive method for the determination of amoxicillin trihydrate (AMXT) based on the diazo-coupling reaction was studied. Sulphanilic acid diazotizes with nitrite ion in acidic medium to produce a water soluble, colorless diazonium ion, which subsequently coupled with AMXT to form a colored azo dye in the alkaline medium, having maximum absorption at 455 nm. The calibration graph showed that Beer's law is obeyed over the concentration range of 0.3 – 30.0 μg/mL of AMXT, with the detection limit of 0.15 μg/mL and molar absorptivity was 2.3 × 104 L/mol.cm. The accuracy and the precision were acceptable depending upon the values of error percentage and relative standard deviation. The influence of common interfer
... Show MoreA simple and sensitive spectrophotometric method is described for the determination of diclofenac sodium (DCL), in pure form and pharmaceutical formulations. The method is based on the oxidation of 2,4-dinitrophenylhydrazine (2,4-DNPH) and coupling of the oxidized product with DCL in alkaline medium to give intensively colored chromogen which exhibits maximum absorption (λmax) at 600 nm, and the concentration of DCL was determined spectrophotometrically. The optimum reaction conditions and other analytical parameters were evaluated. In addition to classical univariate optimization, modified simplex method (MSM) has been applied in optimization of the variables affecting the color producing reaction. Beer’s law is obeyed in the
... Show MoreA simple, accurate and sensitive spectrophotometric method for the determination of Procaine penicillin (PP) is described. The method is based on charge-transfer reaction of PP with metol (N-methyl-p-hydroxy aniline) in the presence of ferric sulphate to form a purple-water soluble complex ,which is stable and has a maximum absorption at 510 nm .A graph of absorbance versus concentration shows that Beer’s low is obeyed over the concentration range of 3-80 µg /ml of PP (i.e.,3-80 ppm) with a molar absorbativity of 4.945 ×103 L.mol-1.cm-1 ,Sandell sensitivity of 0.1190 µg cm-2 ,a relative error of (-1.57)-2.79 % and a standard deviation of less than 0.59 depending on the concentration of PP.The optimum conditions for full co
... Show MoreFor the determination of metoclopramide hydrochloride (MCPD) in pharmaceutical formulations, a rapid and straightforward spectrophotometric method has been proposed. The method involves diazotizing the main amino group of MCPD with sodium nitrite followed by coupling reaction with reagent 1,7-Dihydroxynaphthalene (1,7-DHN) to form a stable and colored compound in alkaline medium of sodium hydroxide which showed a maximum absorbance intensity at the wavelength 578 nm. The linearity of developed method has ranged from 1.0 - 15 µg.ml-1 while the molar absorptivity 2.9867x104 l.mol-1.cm-1, RSD% was less than 1.11%. While the LOD and LOQ were 0.059 µg.ml-1
... Show MoreThis paper concerned with development of a spectrophotometric method for the determination of paracetamol, based on the diazotisation and coupling reaction with anthranilic acid in basic medium, to form an intense yellow coloured, water-soluble and stable azo-dye which shows a maximum absorption at 421nm. Beer’s law is obeyed over the concentration range of 1.0-10 µg/ml; with molar absorptivity of 2.1772×104 L.mol -1.cm-1 and Sandell’s sensitivity index 6.9446 µg.cm-2. The method has been applied successfully for the determination of paracetamol in pharmaceutical formulation.
A simple, precise and accurate spectrophotometric method has been developed for simultaneous estimation of sulfanilamide and furosemide in their mixture by using first and second order derivative method in the ultraviolet region. The method depends on first and second derivative spectrophotometry, with zero-crossing and peak to base line and peak area measurements. The first derivative amplitudes at 214, 238 and 266 nm were selected for the assay of sulfanilamide and 240, 260, 284, 314 and 352 nm for furosemide. Peak area at 201222, 222-251 and 251-281 nm selected for estimation of sulfanilamide and at 229-249, 249270, 270-294, 294-333 and 333-382 nm for furosemide. The second derivative amplitudes at 220, 252 and 274 nm for sulfanilamid
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