A new, simple, rapid and sensitive batch chemiluminescence (CL) method for determination of six fluoroquinolones (ciprofloxacin, gatifloxacin, levofloxacin, lomefloxacin HCl, ofloxacin and sparfloxacin) is proposd. The method is based on the CL generated during the oxidation of luminol by N-bromosuccinimide (NBS) in alkaline medium. The determination of the studied drugs is based on their inhibiting effect on the emission intensity of NBS-luminol chemiluminescent reaction. The effect of analytical variables on this CL system is discussed. The study was validated according to ICH guidelines. Under the optimum experimental conditions, the linear range is 50 to 400 ng/ml for ciprofloxacin, 50 to 600 ng/ml for gatifloxacin, lomefloxacin HCl and sparfloxacin and 25 to 400 ng/ml for levofloxacin and ofloxacin and the detection and quantitation limits for the studied drugs were not more than 4.88 and 14.80 ng/ml, respectively. The proposed method has been applied to detect the studied drugs in their pure forms and in different pharmaceutical formulations. The possible mechanism of the CL reaction was discussed.

A new, simple, rapid and sensitive batch chemiluminescence (CL) method for determination of six fluoroquinolones (ciprofloxacin, gatifloxacin, levofloxacin, lomefloxacin HCl, ofloxacin and sparfloxacin) is proposd. The method is based on the CL generated during the oxidation of luminol by N-bromosuccinimide (NBS) in alkaline medium. The determination of the studied drugs is based on their inhibiting effect on the emission intensity of NBS-luminol chemiluminescent reaction. The effect of analytical variables on this CL system is discussed. The study was validated according to ICH guidelines. Under the optimum experimental conditions, the linear range is 50 to 400 ng/ml for ciprofloxacin, 50 to 600 ng/ml for gatifloxacin, lomefloxacin HCl and sparfloxacin and 25 to 400 ng/ml for levofloxacin and ofloxacin and the detection and quantitation limits for the studied drugs were not more than 4.88 and 14.80 ng/ml, respectively. The proposed method has been applied to detect the studied drugs in their pure forms and in different pharmaceutical formulations. The possible mechanism of the CL reaction was discussed.

A new, simple, rapid and sensitive batch chemiluminescence (CL) method for determination of six fluoroquinolones (ciprofloxacin, gatifloxacin, levofloxacin, lomefloxacin HCl, ofloxacin and sparfloxacin) is proposd. The method is based on the CL generated during the oxidation of luminol by N-bromosuccinimide (NBS) in alkaline medium. The determination of the studied drugs is based on their inhibiting effect on the emission intensity of NBS-luminol chemiluminescent reaction. The effect of analytical variables on this CL system is discussed. The study was validated according to ICH guidelines. Under the optimum experimental conditions, the linear range is 50 to 400 ng/ml for ciprofloxacin, 50 to 600 ng/ml for gatifloxacin, lomefloxacin HCl and sparfloxacin and 25 to 400 ng/ml for levofloxacin and ofloxacin and the detection and quantitation limits for the studied drugs were not more than 4.88 and 14.80 ng/ml, respectively. The proposed method has been applied to detect the studied drugs in their pure forms and in different pharmaceutical formulations. The possible mechanism of the CL reaction was discussed.

This study describes, for the first, the development and validation of a novel high-throughput micorwell spectrophotometric assay for determination of the quinolone antibiotic rosoxacin (ROS) in its bulk and capsules. The assay involved the reaction between ROS and sodium nitroprusside (SNP) forming a red-colored product exhibiting maximum absorption peak (λmax) at 455 nm. The reaction was carried out in 96-microwell plate and the absorbance of the colored-product was measured by microwell plate absorbance reader at 455 nm. The variables affecting the reaction were carefully investigated using the microwell format and the optimum conditions under were established. Under the optimized conditions, a linear relationship with good correlation coefficient (0.9992) was found between the absorbance of the ROS-SNP chromogen and ROS concentration in the range of 15-150 μg/mL. The limits of detection and quantification were 3.5 and 11.6 μg/mL, respectively. The assay showed high precision as the values of relative standard deviations (RSD) did not exceed 2%. The proposed assay was successfully applied to the determination of ROS in its capsules; the label claim percentages were 102.81±1.43%. The results were compared favorably with those of a reference pre-validated method. The proposed assay is practical and valuable in terms of its routine application in determination of ROS in its bulk and capsules in pharmaceutical quality control laboratories.

This study describes, for the first, the development and validation of a novel high-throughput micorwell spectrophotometric assay for determination of the quinolone antibiotic rosoxacin (ROS) in its bulk and capsules. The assay involved the reaction between ROS and sodium nitroprusside (SNP) forming a red-colored product exhibiting maximum absorption peak (λmax) at 455 nm. The reaction was carried out in 96-microwell plate and the absorbance of the colored-product was measured by microwell plate absorbance reader at 455 nm. The variables affecting the reaction were carefully investigated using the microwell format and the optimum conditions under were established. Under the optimized conditions, a linear relationship with good correlation coefficient (0.9992) was found between the absorbance of the ROS-SNP chromogen and ROS concentration in the range of 15-150 μg/mL. The limits of detection and quantification were 3.5 and 11.6 μg/mL, respectively. The assay showed high precision as the values of relative standard deviations (RSD) did not exceed 2%. The proposed assay was successfully applied to the determination of ROS in its capsules; the label claim percentages were 102.81±1.43%. The results were compared favorably with those of a reference pre-validated method. The proposed assay is practical and valuable in terms of its routine application in determination of ROS in its bulk and capsules in pharmaceutical quality control laboratories.

This study describes, for the first, the development and validation of a novel high-throughput micorwell spectrophotometric assay for determination of the quinolone antibiotic rosoxacin (ROS) in its bulk and capsules. The assay involved the reaction between ROS and sodium nitroprusside (SNP) forming a red-colored product exhibiting maximum absorption peak (λmax) at 455 nm. The reaction was carried out in 96-microwell plate and the absorbance of the colored-product was measured by microwell plate absorbance reader at 455 nm. The variables affecting the reaction were carefully investigated using the microwell format and the optimum conditions under were established. Under the optimized conditions, a linear relationship with good correlation coefficient (0.9992) was found between the absorbance of the ROS-SNP chromogen and ROS concentration in the range of 15-150 μg/mL. The limits of detection and quantification were 3.5 and 11.6 μg/mL, respectively. The assay showed high precision as the values of relative standard deviations (RSD) did not exceed 2%. The proposed assay was successfully applied to the determination of ROS in its capsules; the label claim percentages were 102.81±1.43%. The results were compared favorably with those of a reference pre-validated method. The proposed assay is practical and valuable in terms of its routine application in determination of ROS in its bulk and capsules in pharmaceutical quality control laboratories.

The kinetics and mechanism of hexacholroiridate(IV) oxidation of carboxymethyl cellulose (CMC) in aqueous solutions at a constant ionic strength of 0.1 mol dm−3 has been investigated spectrophotometrically. The experimental results showed first-order dependence in [IrCl6]2− and fractional first-order kinetics with respect to CMC concentration. An inversefractional first-order in [H+] was observed. A kinetic evidence for the formation of 1:1 intermediate complex was revealed. The reaction kinetics seems to be of considerable complexity where one chloride ion from hexacholoiridate(IV) oxidant may act as a bridging ligand between the oxidant and the substrate into the formed intermediate complex. The ionic strength was found to have a negligible influence on the reaction rates. The kinetic parameters have been evaluated, and a tentative reaction mechanism consistent with the kinetic results is discussed.

The kinetics of oxidation of tellurium(IV) by [IrCl6]2 in aqueous perchlorate solutions at a constant ionic strength of 0.1 mol dm3 have been investigated spectrophotometrically. The results showed a firstorder dependence in [IrCl6]2, fractional-first-order kinetics with respect to tellurium(IV) concentration and second-order overall kinetics. The increase in the [H+] was found to be accompanied by a decrease in the rate constants, i.e., the oxidation reaction was acid-inhibited. Kinetic evidence for the formation of a 1 : 1 intermediate binuclear complex between the two reactants has been obtained. The ionization constant of tellurium(IV) has been evaluated and found to be 1.69  103 dm3 mol1 at 25 1C. The kinetic parameters have been calculated and a tentative reaction mechanism consistent with the kinetic data is suggested.

tThe kinetics and mechanism of oxidation of alginate polysaccharide (Alg) by alkaline hexacyanoferrate(III)in basic solutions at a constant ionic strength of 1.0 mol dm−3have been investigated spectrophotomet-rically. The experimental results showed complex kinetics, where the reaction time curves of the pseudofirst-order plots were found to be of sigmoidal S-shape nature. The initial parts of the plots were relativelyfast, followed by slow-linear portions after short time periods. The oxidation rates were increased withincreasing the alkali concentration indicating that the oxidation is base-catalyzed. A kinetic evidence forformation of 1:1 intermediate complexes was revealed. The activation parameters have been evaluatedand a tentative reaction mechanism consistent with the kinetic results is suggested and discussed.

A simple and selective micellar electrokinetic chromatographic (MEKC) method has been developed for the analysis of five pharmaceutical binary mixtures containing three non-steroidal anti-inflammatory drugs (NSAIDs). The investigated mixtures were Ibuprofen (IP)–Paracetamol (PC), Ibuprofen (IP)–Chlorzoxazone (CZ), Ibuprofen (IP)–Methocarbamol (MC), Ketoprofen (KP)– Chlorzoxazone (CZ) and Diclofenac sodium (DS)–Lidocaine hydrochloride (LC). The separation was run for all mixtures using borate buffer (20 mM, pH 9) containing 15% (v/v) methanol and 100 mM sodium dodecyl sulphate (SDS) at 15 kV and the components were detected at 214 nm. Different factors affecting the electrophoretic mobility of the seven investigated drugs were studied and optimized. The method was validated according to international conference of harmonization (ICH) guidelines and United States pharmacopoeia (USP). The method was applied to the analysis of five pharmaceutical binary mixtures in their dosage forms. The results were compared with other reported high performance liquid chromatographic methods and no significant differences were observed.