scholarly journals Spectrophotometric determination of pefloxacin mesylate in pharmaceuticals

2007 ◽  
Vol 57 (2) ◽  
pp. 221-230 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Hullikal Prameela ◽  
Bankavadi Somashekar

Spectrophotometric determination of pefloxacin mesylate in pharmaceuticalsA 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 μg 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 theervalues 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'st-test andF-test. Accuracy evaluated by means of the spike recovery method, range from 97.0 to 106.0%, with precision better than 3%.

2006 ◽  
Vol 4 (4) ◽  
Author(s):  
Hosakere Revanasiddappa ◽  
Banadahalli Dayananda

AbstractHighly sensitive and simple spectrophotometric determination of selenium is described for the determination of selenium(IV) using a new reagent leuco malachite green. The method is based on the reaction of selenium(IV) with potassium iodide in an acidic condition to liberate iodine, the liberated iodine oxidizes leuco malachite green to malachite green dye. The green coloration was developed in an acetate buffer (pH 4.2–4.9) on heating in a water bath (∼ 40 °C). The formed dye exhibits an absorption maximum at 615 nm. The method obeys Beer’s law over a concentration range of 0.04–0.4 µg mL−1 selenium. The molar absorptivity and Sandell’s sensitivity of the color system were found to be 1.67 × 105 L mol−1 cm-1 and 0.5 ng cm−2, respectively. The optimum reaction conditions and other analytical parameters have been evaluated. The proposed procedure has been successfully applied to the determination of selenium in real samples of water, soil, plant material, human hair, and cosmetic samples. The results were compared to those obtained with the reference method. Statistical analysis of the results confirms the precision and accuracy of the proposed method. In addition, the developed method is cost-effective and involves easily accessible instrumentation technique which can be used by ordinary research laboratories.


2019 ◽  
Vol 12 (8) ◽  
pp. 3993-3997 ◽  
Author(s):  
Saad A. Al-Tamrah ◽  
Mohammad A. Abdalla ◽  
Abdullah A. Al-Otibi

2007 ◽  
Vol 4 (2) ◽  
pp. 173-179 ◽  
Author(s):  
K. Basavaiah ◽  
U. R. Anil Kumar

A simple spectrophotometric method is proposed for the determination of zidovudine(ZDV) in bulk drug and in pharmaceutical preparations. The method is based on the oxidation of ZDV by a known excess of oxidant N-bromosuccinimide (NBS), in buffer medium of pH 1.5, followed by the estimation of unreacted amount of oxidant with metol and sulphanilic acid. The reacted oxidant corresponds to the amount ZDV. The purple-red reaction product absorbs maximally at 530 nm and Beer’s law is obeyed over a range 5 to 75 μg mL-1. The apparent molar absorptivity is calculated to be 5.1×103L mol-1cm-1, and the corresponding Sandell sensitivity value is 0.052 μg cm-2. The limit of detection and quantification are found to be 0.90 and 2.72, respectively. Intra-day and inter-day precision and accuracy of the developed methods were evaluated as per the current ICH guidelines. The method was successfully applied to the assay of ZDV in tablet/capsule preparations and the results were statistically compared with those of the reference method by applying the Student’s t-test and F-test. No interference was observed from the common tablet/capsule excipients. The accuracy of the method was further ascertained by performing recovery studies via standard-addition method.


2018 ◽  
Vol 33 (2) ◽  
pp. 21
Author(s):  
Kanakapura Basavaiah ◽  
Okram Zenita Devi

Two sensitive spectrophotometric methods are described for the determination of simvastatin (SMT) in bulk drug and in tablets. The methods are based on the oxidation of SMT by a measured excess of cerium (IV) in acid medium followed by determination of unreacted oxidant by two different reaction schemes. In one procedure (method A), the residual cerium (IV) is reacted with a fixed concentration of ferroin and the increase in absorbance is measured at 510 nm. The second approach (method B) involves thereduction of the unreacted cerium (IV) with a fixed quantity of iron (II), and the resulting iron (III) is complexed with thiocyanate and the absorbance measured at 470 nm. In both methods, the amount of cerium (IV) reacted corresponds to SMT concentration. The experimental conditions for both methods were optimized. In method A, the absorbance is found to increase linearly with SMT concentration (r = 0.9995) whereas in method B, the same decreased (r = -0.9943). The systems obey Beer’s law for 0.6-7.5 and 0.5-5.0 μg mL-1 for method A and method B, respectively. The calculated molar absorptivity values are 2.7 X 104 and 1.06 X 105 Lmol-1 cm-1, respectively; and the corresponding sandel sensitivity values are 0.0153 and 0.0039μg cm-2, respectively. The limit of detection (LOD) and quantification (LOQ) are reported for both methods. Intra-day and inter-day precision, and accuracy of the methods were established as per the current ICH guidelines. The methods were successfully applied to the determination of SMT in tablets and the results were statistically compared with those of the reference method by applying the Student’s t-test and F-test. No interference was observed from the common excipients added to tablets. The accuracy and validity of the methods were further ascertained by performing recovery experiments via standard addition procedure.


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.


2021 ◽  
Vol 9 (2) ◽  
pp. 64-71
Author(s):  
Mykola Blazheyevskiy ◽  
◽  
Valeriy Moroz ◽  
Olena Mozgova ◽  
◽  
...  

The oxidative derivatization method using potassium hydrogenperoxomonosulfate for the indirect spectrophotometric determination of Fluphenazine hydrochloride is presented. Potassium hydrogenperoxomonosulfate is introduced as a derivatizing agent for Fluphenazine hydrochloride, yielding the sulfoxide. This reaction product was successfully used for the spectrophotometric determination of the Fluphenazine hydrochloride. The UV spectroscopic detection of the sulfoxide proved to be a more robust and sensitive method. The elaborated method allowed the determination of Fluphenazine hydrochloride in the concentration range of 0.2-30 µg mL-1. The molar absorptivity at 349 nm is 5.6×103 (dm3cm-1mol-1). The limit of quantification, LOQ (10S) is 0.24 µg/mL. A new spectrophotometric technique was developed and the possibility of quantitative determination of Fluphenazine hydrochloride in tablets 5.0 mg was demonstrated. The present method is precise, accurate and excipients did not interfere. RSD for Fluphenazine Hydrochloride 5.0 mg tablets was 1.37 %.


2021 ◽  
Author(s):  
Wen-Yi Wang ◽  
Jia-Chi Chiou ◽  
Wan-Xue Chen ◽  
Jia-Li Yu ◽  
Chi-wai Kan

Abstract It is a challenge to determine the quantity of cationic finishing agents on the surface of cellulosic fabrics. Herein, we report a direct and feasible method by Kubelka-Munk equation to quantify the cationic poly (hexamethylene biguanide) hydrochloride (PHMB) adsorbed onto cotton fabrics based on the principle of formation of a stable blue dye between PHMB and bromophenol blue sodium (BPB). The adsorption of PHMB onto cotton fabrics was first investigated and the maximum adsorption of PHMB was found to be around 8 mg per gram of cotton fabric. After being dyed with BPB, colour strength shows a positive correlation with PHMB at low concentrations (< 2400 mg/L). A linear relationship with a high correlation (C(PHMB) = (K/S—0.7411)/3.4517, R2 = 0.9983) was thus established between colour strength and PHMB concentration. However, this equation should fulfill four requirements for quantifying PHMB: (1) the distribution of PHMB on the surface of cellulosic fabric should be in the form of a monolayer with the content less than 5.3 mg/g; (2) an excess of BPB dyebath should be applied; (3) the dyeing should come to equilibrium; and (4) the fabrics should be evenly dyed. Moreover, MTT assay results indicate that excess PHMB coated on cotton fabrics can cause cytotoxicity and the quantity of PHMB should not exceed 4.62 mg per gram of cotton fabrics for the purpose of biosafety. The sample can be considered non-cytotoxic if the K/S value is lower than 13.2 after dyeing with BPB.


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