Syed Najmul Hejaz Azmi

Quantitative analysis of cefixime via complexation with palladium(II) in pharmaceutical formulations by spectrophotometry

An optimized and validated spectrophotometric method has been developed for the determination of cefixime in pharmaceutical formulations. The method is based on the complexation reaction between cefixime and palladium ion in the presence of acidic buffer solution (pH 3) in ethanol-distilled water medium at room temperature. The complex absorbed maximally at 352 nm. Beer’s law is obeyed in the working concentration range of 2.5–35 μg/mL with apparent molar absorptivity of 1.015×104 L/mol cm and Sandell’s sensitivity of 0.001 μg/cm2/0.001 absorbance unit. The limits of detection and quantitation for the proposed method are 0.175 and 0.583 μg/mL, respectively. The effect of common excipients used as additives has been studied in the determination of cefixime. The proposed method has been successfully applied for the determination of cefixime in pharmaceutical formulations. The results obtained by the proposed method were statistically compared with the reference method using t and F values and found no significant difference between the two methods.

Utility of eosin Y as a complexing reagent for the determination of citalopram hydrobromide in commercial dosage forms by fluorescence spectrophotometry

An accurate, selective and sensitive spectrofluorimetric method was developed for the determination of citalopram hydrobromide in commercial dosage forms. The method was based on the formation of a fluorescent ion-pair complex between citalopram hydrobromide and eosin Y in the presence of a disodium hydrogen phosphate/citric acid buffer solution of pH 3.4 that was extractable in dichloromethane. The extracted complex showed fluorescence intensity at λem = 554 nm after excitation at 259 nm. The calibration curve was linear over at concentrations of 2.0-26.0 µg/mL. Under optimized experimental conditions, the proposed method was validated as per ICH guidelines. The effect of common excipients used as additives was tested and the tolerance limit calculated. The limit of detection for the proposed method was 0.121 μg/mL. The proposed method was successfully applied to the determination of citalopram hydrobromide in commercial dosage forms. The results were compared with the reference RP-HPLC method.

Optimized and validated spectrophotometric method for the determination of palladium(II) in synthetic mixture and automobile workshop area samples

Abstract An optimized and validated spectrophotometric method has been developed for the determination of Pd(II) in synthetic mixture and automobile workshop area samples. The method was based on the complex formation of Pd(II) with cefixime in methanol-distilled water medium in the presence of Na2HPO4-citric acid buffer solution of pH 2.6 at room temperature. The complex showed the maximum absorption wavelength at 352 nm. Beer’s law was obeyed in the working concentration range of 0.7502–16.5004 μg mL−1 with apparent molar absorptivity of 1.224 × 104 L mol−1 cm−1 and Sandell’s sensitivity of 0.002 μg/cm2/0.001 absorbance unit. Limits of detection (LOD) and quantitation (LOQ) for the proposed method were 0.07 and 0.21 μg mL−1, respectively. The effect of diverse ions such as Cu(II), Mg(II), Mn(II), Ca(II), Fe(II), Cr(III), Ni(II), Al(III), Fe(III), Cd(II) and Zn(II) has been studied in the presence of Pd(II) and the maximum tolerance limit of each metal was calculated. The proposed method was successfully applied for the determination of Pd(II) in synthetic mixture and automobile workshop area samples.