scholarly journals Simple and Selective Spectrophotometric Determination of Ofloxacin in Pharmaceutical Formulations Using Two Sulphonphthalein Acid Dyes

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Kudige N. Prashanth ◽  
Kanakapura Basavaiah ◽  
Madihalli S. Raghu

Two new simple and sensitive extraction-free spectrophotometric methods have been established for the determination of ofloxacin (OFX). The methods are based on ion-pair complex formation reaction between OFX and acidic sulphonphthalein dyes, bromocresol purple (method A), and bromocresol green (method B) in dichloromethane. The experimental variables such as reaction medium, reaction time, and reagent concentration have been carefully optimized to achieve the highest sensitivity. Both dyes react spontaneously with OFX to give yellow-colored complexes. Beer’s law is obeyed over the concentration ranges of 1.0–16 µg ml−1 OFX with correlation coefficient of 0.999 in both methods. The molar absorptivity values are calculated to be and l mol−1 cm−1, for method A and method B, respectively, with corresponding Sandell's sensitivity values of 0.015 and 0.019 µg cm−2. The limits of detection (LOD) and quantification (LOQ) are also reported. A Job’s plot of the absorbance versus the molar ratio of OFX to each of dyes under consideration indicated (1 : 1) ratio and the conditional stability constant () of the complexes have been calculated. The proposed methods were applied successfully to the determination of OFX in tablets with good accuracy and precision and without interference from common additives. The results obtained by the proposed methods were compared favorably with those of the reference method.

2014 ◽  
Vol 2014 ◽  
pp. 1-16 ◽  
Author(s):  
Ayman A. Gouda ◽  
Alaa S. Amin ◽  
Ragaa El-Sheikh ◽  
Amira G. Yousef

Simple, rapid, and extractive spectrophotometric methods were developed for the determination of some fluoroquinolones antibiotics: gemifloxacin mesylate (GMF), moxifloxacin hydrochloride (MXF), and enrofloxacin (ENF) in pure forms and pharmaceutical formulations. These methods are based on the formation of ion-pair complexes between the basic drugs and acid dyes, namely, bromocresol green (BCG), bromocresol purple (BCP), bromophenol blue (BPB), bromothymol blue (BTB), and methyl orange (MO) in acidic buffer solutions. The formed complexes were extracted with chloroform and measured at 420, 408, 416, 415, and 422 nm for BCG, BCP, BPB, BTB, and MO, respectively, for GMF; at 410, 415, 416, and 420 nm for BCP, BTB, BPB, and MO, respectively, for MXF; and at 419 and 414 nm for BCG and BTB, respectively, in case of ENF. The analytical parameters and their effects are investigated. Beer’s law was obeyed in the ranges 1.0–30, 1.0–20, and 2.0–24 μg mL−1for GMF, MXF, and ENF, respectively. The proposed methods have been applied successfully for the analysis of the studied drugs in pure forms and pharmaceutical formulations. Statistical comparison of the results with the reference methods showed excellent agreement and indicated no significant difference in accuracy and precision.


2012 ◽  
Vol 18 (2) ◽  
pp. 339-347 ◽  
Author(s):  
Sameer Abdulrahman ◽  
Kanakapura Basavaiah

Two simple, sensitive and extraction-free spectrophotometric methods are described for the determination of dothiepin hydrochloride (DOTH) both in pure form and in pharmaceutical tablets. The methods are based on ion-pair complex formation between dothiepin base (DOT) and two acidic dyes, namely, bromophenol blue (BPB) or bromocresol green (BCG) with absorption maximum at 425 nm for BPB method or 430 nm for BCG method. Beer?s law is obeyed over the concentration ranges of 1.0-15.0 and 1.0-17.5 ?g mL-1 DOT for BPB and BCG methods, respectively. The molar absorptivity values and Sandell?s sensitivity values are reported for both methods. The limits of detection (LOD) and quantification (LOQ) were calculated to be 0.18 and 0.53 ?g mL-1 for BPB method, and 0.17 and 0.50 ?g mL-1 for BCG method, respectively. The stoichiometry of the complex in either case was found to be 1: 1 and the conditional stability constant (KF) of the complexes has also been calculated. The proposed methods were applied successfully to the determination of DOTH in pure form and in its tablet form with good accuracy and precision. Statistical comparison of the results was performed using Student's t-test and variance ratio F-test at 95% confidence level and there was no significant difference between the official and proposed methods with regard to accuracy and precision. Further, the validity of the proposed methods was confirmed by recovery studies via standard addition technique.


2009 ◽  
Vol 15 (2) ◽  
pp. 69-76 ◽  
Author(s):  
S.M. Al-Ghannam ◽  
A.M. Al-Olyan

A sensitive spectrophotometric method was developed for the determination of some 1,4-dihydropyridine compounds namely, nicardipine and isradipine either in pure form or in pharmaceutical preparations. The method is based on the reduction of nicardipine and isradipine with zinc powder and calcium chloride followed by further reduction with sodium pentacyanoaminoferrate (II) to give violet and red products having the absorbance maximum at 546 and 539 nm with nicardipine and isradipine, respectively. Beer's law was obeyed over the concentration range 8.0-180 ?g/ml with the detection limit of 1.67 ?g/ml for nicardipine and 8.0-110 ?g/ml with the detection limit of 1.748 ?g/ml for isradipine. The analytical parameters and their effects on the reported methods were investigated. The molar absorptivity, quantization limit, standard deviation of intercept (Sa), standard deviation of slope (Sb) and standard deviation of the residuals (Sy/x) were calculated. The composition of the result compounds were found 1:1 for nicardipine and 1:2 for isradipine by Job's method and the conditional stability constant (Kf) and the free energy changes (?G) were calculated for compounds formed. The proposed method was applied successfully for the determination of nicardipine and isradipine in their dosage forms. The results obtained were in good agreement with those obtained using the reference or official methods. A proposal of the reaction pathway was presented.


2018 ◽  
Vol 15 (2) ◽  
pp. 6186-6198
Author(s):  
Abdul Aziz Ramadan ◽  
Souad Zeino

A simple, direct and accurate spectrophotometric method has been developed for the determination of Glimepiride (GLM) in pure and pharmaceutical formulations by complex formation with bromocresol purple (BCP). The method involves the formation of a yellow ion-pair complex between BCP with glimepiride at pH<3,8; after reacting GLM with Na2CO3 to give C24H33N4H+O5NaS which is extracted by chloroform. The formed complex [GLM]:[ BCP] was measured at lmax 418 nm against the reagent blank prepared in the same manner. Variables were studied in order to optimize the reaction conditions. Molar absorptivity (e) for complex was  20600  L.mol-1.cm-1. Beer’s law was obeyed in the concentration range of  1.226 – 46.608   mg.mL-1 in present of 5.0x10-4 mol/l of BCP with good correlation coefficient (R2= 0.9997). The relative standard deviation did not exceed 3.6%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.15 and 0.46 mg.mL-1, respectively. The proposed method was validated for specificity, linearity, precision and accuracy, repeatability, sensitivity (LOD and LOQ)  and robustness. The developed method is applicable for the determination of GLM in  pure and different dosage forms with average assay of 98.8 to 102.0% and the results are in good agreement with those obtained by the  RP-HPLC reference method.  


Author(s):  
MONIR Z. SAAD ◽  
ATEF AMER ◽  
KHALED ELGENDY ◽  
BASEM ELGENDY

Objective: Two simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sofosbuvir (SOF) and daclatasvir (DAC) in pure forms and pharmaceutical formulations. Methods: The proposed methods are based on the oxidation of SOF and DAC by a known excess of cerium(IV) ammonium nitrate in sulphuric acid medium followed by determination of unreacted cerium(IV) by adding a fixed amount of indigo carmine (IC) and alizarin red S (ARS) dyes followed by measuring the absorbance at 610 and 360 nm, respectively. The experimental conditions affecting the reaction were studied and optimized. Results: The beer’s law was obeyed in the concentration ranges of 0.2-3.0, 0.2-4.0 for SOF and 0.5-4.5 and 0.5-5.0 μg/ml for DAC using IC and ARS methods, respectively with a correlation coefficient ≥ 0.9991. The calculated molar absorptivity values are 2.354 × 104, 1.933 × 104 for SOF and 1.786 × 104 and 2.015 × 104 L/mol. cm for DAC using IC and ARS methods, respectively u. The limits of detection and quantification are also reported. Intra-day and inter-day precision and accuracy of the methods have been evaluated. Conclusion: The methods were successfully applied to the assay of SOF and DAC in tablets and the results were statistically compared with those of the reference method by applying Student’s t-test and F-test. No interference was observed from the common tablet excipients. The accuracy and reliability of the methods were further ascertained by performing recovery studies using the standard addition method.


2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
K. Susmitha ◽  
M. Thirumalachary ◽  
T. Charan Singh ◽  
G. Venkateshwarlu

Tenofovir disoproxil fumarate is a nucleotide reverse transcriptase inhibitor that has activity against the hepatitis B and HIV viruses. Three simple and sensitive extractive spectrophotometric methods have been described for the assay of tenofovir disoproxil fumarate either in pure form or in pharmaceutical formulations. The developed methods involve formation of colored chloroform extractable ion-pair complexes of the drugs with triphenylmethane dyes, namely, bromothymol blue (BTB), bromophenol blue (BPB), and bromocresol purple (BCP) in acidic medium. The extracted complexes showed absorbance maxima between 410 and 415 nm. Beer’s law is obeyed in the concentration ranges 1.5–25, 1.0–25, and 1.25–25 μg mL−1 with BTB, BPB, and BCP, respectively. The effectc of concentration of dye, pH, and interference of excipients have been studied and optimized. The limits of detection and quantification have been determined. All three methods are validated as per the guidelines of ICH. The methods have been applied to the determination of drug in commercial tablets and results of analysis were validated statistically through recovery studies.


2011 ◽  
Vol 6 ◽  
pp. ACI.S8090 ◽  
Author(s):  
Lobna M. Abdellaziz ◽  
Mervat M. Hosny

Three simple spectrophotometric and atomic absorption spectrometric methods are developed and validated for the determination of moxifloxacin HCl in pure form and in pharmaceutical formulations. Method (A) is a kinetic method based on the oxidation of moxifloxacin HCl by Fe3+ ion in the presence of 1,10 o-phenanthroline (o-phen). Method (B) describes spectrophotometric procedures for determination of moxifloxacin HCl based on its ability to reduce Fe (III) to Fe (II), which was rapidly converted to the corresponding stable coloured complex after reacting with 2,2’ bipyridyl (bipy). The formation of the tris-complex formed in both methods (A) and (B) were carefully studied and their absorbance were measured at 510 and 520 nm respectively. Method (C) is based on the formation of ion- pair associated between the drug and bismuth (III) tetraiodide in acidic medium to form orange—red ion- pair associates. This associate can be quantitatively determined by three different procedures. The formed precipitate is either filtered off, dissolved in acetone and quantified spectrophotometrically at 462 nm (Procedure 1), or decomposed by hydrochloric acid, and the bismuth content is determined by direct atomic absorption spectrometric (Procedure 2). Also the residual unreacted metal complex in the filtrate is determined through its metal content using indirect atomic absorption spectrometric technique (Procedure 3). All the proposed methods were validated according to the International Conference on Harmonization (ICH) guidelines, the three proposed methods permit the determination of moxifloxacin HCl in the range of (0.8-6, 0.8-4) for methods A and B, (16-96, 16-96 and 16-72) for procedures 1-3 in method C. The limits of detection and quantitation were calculated, the precision of the methods were satisfactory; the values of relative standard deviations did not exceed 2%. The proposed methods were successfully applied to determine the drug in its pharmaceutical formulations without interference from the common excipients. The results obtained by the proposed methods were comparable with those obtained by the reference method.


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