Spectrophotometric determination of enrofloxacin and pefloxacin through ion-pair complex formation

Mostafa, Samia M.; El-Sadek, Mohamed; Alla, Esmail Awad

doi:10.1016/s0731-7085(01)00591-x

Cited by 54 publications

(27 citation statements)

References 6 publications

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“…From Table I, it is clear that the proposed spectrophotometric method is highly selective compared to most existing methods (7,(15)(16)(17)(18)(19)(20)(21)(22)(23)(24)(25). The most striking feature of the method is its extraordinary Brought to you by | MIT Libraries Authenticated Download Date | 5/11/18 1:39 AM sensitivity, which is comparable to that of the spectrofluorometric method.…”

Section: Application To Dosage Formsmentioning

confidence: 99%

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Spectrophotometric determination of pefloxacin mesylate in pharmaceuticals

Basavaiah

Prameela²,

Somashekar³

2007

Acta Pharmaceutica

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Pefloxacin mesylate dihydrate (PFM) is a fluorinated quinolone structurally related to nalidixic acid. Chemically, PFM, is 1-ethyl-6-fluoro-1,4-dihydro-7-(4-methyl-1-peperazinyl)-4-oxo-3-quinolinecarboxylic acid, methane sulfonate dihydrate (Fig. 1). It is an antibacterial drug, which is highly effective against both Gram-negative and Gram-positive pathogens that are resistant to other antibacterials (1). The therapeutic importance of PFM has necessitated the development of analytical methods for its determination in dosage forms in compliance with good manufacturing standards. The drug is official in British and European Pharmacopoeias which describe a potentiometric non-aqueous titration procedure for its assay (2, 3). The drug has been determined in pharmaceutical formulations by a variety of analytical techniques such as UV-spectrophotometry (4, 5), A spectrophotometric method is described for assay of pefloxacin mesylate (PFM) in bulk drug and in tablets. The method is based on back extraction of the bromophenol blue dye at pH 5.2 from the dye-drug ion pair followed by measurement of the dye absorbance at 590 nm. The working conditions of the method were investigated and optimized. Beer's law plot showed a good correlation in the concentration range of 0.15-1.25 mg mL -1 . Sensitivity indices such as molar absorptivity, limits of detection and quantification are reported. Intra-day and inter-day precision, and accuracy of the methods were established according to the ICH guidelines, and the e r values were in the range of -1.7 to 1.8% with RSD values ranging from 1.0 to 1.1%. The method was successfully applied to the assay of PFM in tablet preparations with recoveries varying from 97.5 to 101.9%, with standard deviation in the range of 0.6 to 1.9. The results were statistically compared with those of the reference method by applying Student's t-test and F-test. Accuracy evaluated by means of the spike recovery method, range from 97.0 to 106.0%, with precision better than 3%.

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Section: Application To Dosage Formsmentioning

confidence: 99%

“…A few visible spectrophotometric methods based on acid-base (15), redox (7,(16)(17)(18), oxidative coupling (19), complex formation (20)(21)(22)(23)(24) reactions have been earlier reported for the determination of PFM in dosage forms. The reported methods have their respective advantages and disadvantages as indicated in Table 1.…”

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confidence: 99%

Spectrophotometric determination of pefloxacin mesylate in pharmaceuticals

Basavaiah

Prameela²,

Somashekar³

2007

Acta Pharmaceutica

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“…The effect of volume of aqueous phase was studied by using different volumes of aqueous phase (including drug, AZS, and HCl) such as 15,20,25,30, and 35 mL and extracting with 10 mL of dichloromethane. The use of 25 mL of aqueous phase was found to be sufficient to achieve maximum absorbance of measured species and minimum absorbance of reagent blank and hence an aqueous phase of 25 mL was fixed throughout.…”

Section: Effect Of the Volume Of Aqueous Phasementioning

confidence: 99%

“…Extractive spectrophotometric procedures have received considerable attention for quantitative determination of many organic compounds of pharmaceutical interest [26][27][28][29][30] employing many dyes including alizarin red S (AZS) [31][32][33]. This study was directed to develop two accurate, selective, precise, and inexpensive procedures for the determination of FFH in pharmaceuticals based on ion-pair complex formation using AZS as a reagent.…”

Section: Introductionmentioning

confidence: 99%

Use of Alizarin Red S as an Ion-Pair Reagent for the Spectrophotometric Assay of Fexofenadine in Pharmaceuticals and in Spiked Human Urine

et al. 2012

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The present study describes two simple, rapid, selective, and cost-effective spectrophotometric methods for the determination of an antiallergic drug, fexofenadine hydrochloride (FFH), in bulk drug, tablets, and in spiked human urine. The first method (method A) is based on the formation of yellow-colored ion-pair complex between FFH and alizarin red S (AZS) in acid medium which was extracted into dichloromethane, and the absorbance was measured at 440 nm. The second method (method B) is based on the breaking of the yellow FFH-AZS ion-pair complex in alkaline medium followed by the measurement of the violet-colored free dye at 590 nm. Under the optimized conditions, Beer's law is obeyed over the concentration ranges of 0.4-12.0 and 0.2-3.5 μg mL −1 FFH for method A and method B, respectively, and the corresponding molar absorptivity values are 3.80 × 10 4 and 1.61 × 10 5 L mol −1 cm −1 . The Sandell's sensitivity, detection, and quantification limits are also reported. The proposed methods were successfully applied to the determination of FFH in pure drug and commercial tablets. The accuracy and reliability of the proposed methods were further established by recovery studies via standard addition technique.

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“…Most of these methods use high-performance liquid chromatography (HPLC) with a variety of detectors (5)(6)(7)(8)(9)(10)(11)(12)(13)(14)(15)(16). Other methods have also been developed for the determination of ENRO, including: solid-phase spectrofluorimetry (SPF) (17); fluorescence (FL) (4,(18)(19)(20); solidphase extraction and UV-diode array detection (SPE-UV-DAD) (21); high-performance thin layer chromatography (HPTLC) (22); corona discharge ion mobility spectrometry (CD-IMS) (23); atomic absorption spectroscopy (AAS) (24); capillary electrophoresis (CE) (25,26); voltametry (27,28); and spectrophotometry (29,30). Also a DNA-based surface plasmon resonance biosensor for ENRO was developed by Cao et al, whose detection limit in milk samples was estimated to be 3.0 μg/mL (31).…”

Section: Introductionmentioning

confidence: 99%

Flow‐injection chemiluminescence determination of enrofloxacin using the Ru(phen)₃²⁺–Ce(IV) system and central composite design for the optimization of chemical variables

Rezaei

Mokhtari

2008

Luminescence

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The main purpose of this study was to develop an inexpensive, simple, rapid and sensitive chemiluminescence (CL) method for the determination of enrofloxacin (ENRO) using a flow-injection system. This method is based on rapid reduction of Ru(phen)(3)(3+), which is produced in the reaction between Ru(phen)(3)(2+) and acidic Ce(IV) by ENRO, producing strong CL. A central composite design (CCD) was used for optimization of the chemical variables. Regression analysis of the data from the CCD demonstrated that a second-order polynomial model is an adequate description of the surface over the factor limits studied. Optimization using CCD gave approximately four-fold better results than the single-factor-at-a-time method. Under optimal experimental conditions, the CL response was proportional to the concentration of ENRO over a wide range (0.008-3.6 microg/mL) with a correlation coefficient of 0.9986 and a detection limit of 0.003 microg/mL (3sigma). The relative standard deviation for 11 repeated determinations of 0.14 microg/mL ENRO was 4.2%. This method was successfully applied to the analysis of commercial formulations, spiked plasma and spiked poultry tissue. Sample analyses showed good recovery percentages for drugs and spiked plasma (95.1-103.9%). Recovery percentages for spiked poultry tissue were in the range 77.6-87.3%. The minimum sampling rate was 100 samples/h.

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Spectrophotometric determination of enrofloxacin and pefloxacin through ion-pair complex formation

Cited by 54 publications

References 6 publications

Spectrophotometric determination of pefloxacin mesylate in pharmaceuticals

Spectrophotometric determination of pefloxacin mesylate in pharmaceuticals

Use of Alizarin Red S as an Ion-Pair Reagent for the Spectrophotometric Assay of Fexofenadine in Pharmaceuticals and in Spiked Human Urine

Flow‐injection chemiluminescence determination of enrofloxacin using the Ru(phen)₃²⁺–Ce(IV) system and central composite design for the optimization of chemical variables

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Spectrophotometric determination of enrofloxacin and pefloxacin through ion-pair complex formation

Cited by 54 publications

References 6 publications

Spectrophotometric determination of pefloxacin mesylate in pharmaceuticals

Spectrophotometric determination of pefloxacin mesylate in pharmaceuticals

Use of Alizarin Red S as an Ion-Pair Reagent for the Spectrophotometric Assay of Fexofenadine in Pharmaceuticals and in Spiked Human Urine

Flow‐injection chemiluminescence determination of enrofloxacin using the Ru(phen)32+–Ce(IV) system and central composite design for the optimization of chemical variables

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Flow‐injection chemiluminescence determination of enrofloxacin using the Ru(phen)₃²⁺–Ce(IV) system and central composite design for the optimization of chemical variables