scholarly journals Uv Spectrophotometric Methods for Determination of Sofosbuvir in Pure Form and Pharmaceutical Dosage Forms in Presence of Its Alkaline Degradate

2020 ◽  
pp. 12-25
Author(s):  
Zeinab Adel Nasr ◽  
Noha S. Said ◽  
Sawsan A. Abdel-Razeq
Keyword(s):  
Good Accuracy ◽  
Dosage Forms ◽  
Difference Spectra ◽  
Pharmaceutical Dosage Forms ◽  
Spectrophotometric Methods ◽  
Good Linearity ◽  
Ratio Difference ◽  
Accuracy And Precision ◽  
Tablet Dosage

Aims: Two spectrophotometric methods were developed and validated for the determination of sofosbuvir in presence of its alkaline degradate. Study Design: Ratio difference and ratio derivative methods were assisted for determination of sofosbuvir in presence of its alkaline degradate, laboratory-prepared mixtures and in tablet dosage forms. Place and Duration of Study: Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy (Girls), Al - Azhar University, between December 2019 and January 2020. Methodology: Two analytical methods were achieved and validated for the quantitative determination of Sofosbuvir in presence of its alkaline degradate. The first method was ratio difference (RD) method, where the UV absorption spectra of different concentrations of sofosbuvir were divided by the spectrum of a certain concentration (15 µg mL-1) as a devisor of its alkaline degradate to get the ratio difference spectra. Afterwards, the peak amplitudes difference between 253.7 and 243.5 nm were measured. The second method was the ratio derivative (1DR) method, where the first derivative of the ratio spectra (1DR) was obtained and its amplitude was measured at 247 and 268 nm. Good linearity was obtained over the concentration range of 3-15 µg mL-1 for the proposed methods. The proposed procedures were adopted for the selective determination of intact Sofosbuvir in presence of up to 80% of its degradation product. Sofosbuvir was exposed to different conditions as alkaline, acidic and oxidative degradation. Results: The proposed methods were developed and validated with good linearity range of 3-15 µg mL-1 for both methods, and also with good accuracy and precision. And the obtained results were statistically compared to those obtained by the reported method. Conclusion: Sofosbuvir was successfully determined by the proposed ratio difference and ratio derivative methods in bulk powder, laboratory prepared mixtures and tablet dosage form with good accuracy and precision. The methods were validated according to ICH guidelines. The results obtained were compared with those of the reported method and were found to be in good agreement.

scholarly journals Validated Stability – Indicating Methods for Determination of Sofosbuvir by UPLC and HPTLC in Pure Form and Tablet Dosage Forms

2019 ◽  
pp. 1-13
Author(s):  
Sawsan A. Abdel-Razeq ◽  
Zeinab Adel Nasr ◽  
Noha S. Said
Keyword(s):  
Liquid Chromatography ◽  
Thin Layer ◽  
High Performance ◽  
Good Accuracy ◽  
Degradation Products ◽  
Dosage Forms ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Tablet Dosage

Aims: Two simple and sensitive stability- indicating methods were developed and validated for the quantitative determination of sofosbuvir in presence of its degradation products. Study Design: Ultra high performance liquid chromatography (UPLC), High performance thin layer chromatography (HPTLC) are developed for determination of sofosbuvir in presence of its degradation products, laboratory-prepared mixtures and in tablet dosage forms. Place and Duration of Study: Analytical Chemistry Department, Faculty of Pharmacy (Girls), Al-Azhar University, between August 2018 and March 2019. Methodology: Two simple and sensitive stability- indicating methods were developed and validated for the quantitative determination of Sofosbuvir in presence of its degradation products. The first method was an Ultra Performance Liquid Chromatography (UPLC) method, in which efficient separation was carried out on phenomenex kinetex 2.6 μm C18 100 A column using a mobile phase consisting of filtered and degassed mixture of 0.1% ortho-phosphoric acid in water and methanol with the ratio of (40:60% v/v) adjusted to pH 3.5, at a flow rate of 1 mL min-1 and UV detection at 260 nm at ambient temperature. The second method is a high performance- thin layer chromatographic one (HPTLC) in which chromatographic separation was performed on silica gel 60 F254 plates, with methanol – chloroform – ammonia (2.5: 6: 1.5 % v/v/v) as a developing system followed by densitometric determination at 261 nm. Sofosbuvir was subjected to stress conditions including alkaline, acidic and oxidative degradation. Results: Beer’s law was obeyed over the range of 1-20 μg mL–1 for UPLC and 2-12 μg / spot for HPTC with good accuracy and precision using the two procedures, respectively. Results obtained was statistically analysed and found to be in accordance with those given by the reported method. Conclusion: The proposed methods were successfully applied for the determination of sofosbuvir in bulk powder, laboratory prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The methods were validated according to ICH guidelines. The results obtained were compared with those of the reported method and were found to be in good agreement.

scholarly journals Optimization of Two Flow-Injection Spectrophotometric Methods for the Determination of Indapamide in Pharmaceutical Dosage Forms

2005 ◽  
Vol 88 (4) ◽  
pp. 1148-1154 ◽  
Author(s):  
Juan C Rodríguez ◽  
Julia Barciela ◽  
Sagrario García ◽  
Carlos Herrero ◽  
Rosa M Peña
Keyword(s):  
Flow Injection ◽  
Screening Method ◽  
Pharmaceutical Preparations ◽  
Dosage Forms ◽  
Response Surfaces ◽  
Subsequent Formation ◽  
Pharmaceutical Dosage Forms ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision

Abstract Multivariate experimental design has been used to optimize 2 flow-injection spectrophotometric methods for the determination of indapamide in pharmaceutical dosage forms, both pure and commercial tablets. The methods are based on the oxidation of this drug with iron (III) in acidic medium and the subsequent formation of an intensive orange-red complex between the liberated iron (II) and 2,2′-bipyridyl or 1,10-phenanthroline reagents. Plackett-Burman designs were applied as a screening method to evaluate the most significant factors with few experiments. Central composite 23+ star designs were performed to evaluate the response surfaces. The methods have been fully validated and were applied successfully to the determination of indapamide in pure and pharmaceutical forms with good accuracy and precision. Therefore, the 2 proposed procedures are simple, inexpensive, and rapid flow methods for the routine determination of indapamide in pharmaceutical preparations.

scholarly journals DEVELOPMENT AND VALIDATION OF NEW SPECTROPHOTOMETRIC METHODS FOR ESTIMATION OF ANTIPSYCHOTIC DRUG ASENAPINE MALEATE IN PURE AND DOSAGE FORMS

2020 ◽  
pp. 62-69
Author(s):  
RAGAA EL-SHEIKH ◽  
AHLAM E. ABD ELLATEIF ◽  
ESRAA AKMAL ◽  
AYMAN A. GOUDA
Keyword(s):  
Limit Of Detection ◽  
Dosage Forms ◽  
Ion Pair ◽  
Stoichiometric Ratio ◽  
Bromocresol Purple ◽  
Pharmaceutical Dosage Forms ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Significant Difference

Objective: Three sensitive, simple, precise, reproducible, and validated spectrophotometric methods have been developed for the determination of anti-psychotic drug (asenapine maleate) in pure and pharmaceutical dosage forms. Methods: The methods are based on the formation of yellow-colored ion-pair complex between asenapine maleate and three acid dyes, namely, bromocresol purple (BCP), bromophenol blue (BPB) and bromothymol blue (BTB) with absorption maxima at 410, 414 and 416 nm, respectively. Several parameters such as pH, buffer type and volume, reagent volume, the sequence of addition and effect of extracting solvent were optimized. Results: Under the optimum experimental conditions, beer’s law is obeyed over the concentration ranges of 1.0–20, 1.0–14, and 1.0-16 μg/ml for BCP, BPB and BTB, respectively, with good correlation coefficients (0.9994-0.9998). The apparent molar absorptivity and Sandell’s sensitivity values are reported for all methods. The limit of detection (LOD) and the limit of quantification (LOQ) values are found to be 0.27, 0.30, and 0.25 μg/ml and 0.90, 1.0, and 0.83 μg/ml for BCP, BPB and BTB, respectively. The stoichiometric ratio of the formed ion-pair complexes was found to be 1:1 (drug: reagent) for all methods, as deduced by Job's method of continuous variation. Conclusion: The proposed methods were successfully applied for the determination of asenapine maleate in pharmaceutical formulations with good accuracy and precision. Statistical comparison of the results was performed using Student's t-test and variance ratio F-test at the 95% confidence level and there was no significant difference between the reported and proposed methods regarding accuracy and precision. Further, the validity of the proposed methods was confirmed by recovery studies via standard addition technique in accordance with ICH guidelines.

scholarly journals A NOVEL SPECTROPHOTOMETRIC DETERMINATION OF METHYLDOPA THROUGH TERNARY COMPLEXATION PROCEDURE USING FE(III), MN(II), AND CO(II) WITH 2-AMINOPYRIDINE

2019 ◽  
pp. 366-371 ◽  
Author(s):  
MUSTAFA JAMAL KHALEEL BICHAN ◽  
FADAM MUTEB ABDOON
Keyword(s):  
Low Cost ◽  
Dosage Forms ◽  
Optimum Conditions ◽  
Pharmaceutical Dosage Forms ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Ternary Complexation ◽  
Colored Complexes

Objective: The present study is aimed to find a three simple, low cost, accurate, rapid, and sensitive spectrophotometric methods based on the formation of ternary complexes to assay methyldopa (MTD) in both pure and pharmaceutical dosage forms. Methods: The suggested complexation procedure is based on the formation of ternary complex among MTD, 2-aminopyridine (2-Amp), and different metal cations such as [Fe(III), Mn(II), and Co(II)] to form three complexes of Fe(III)-MTD-2-Amp (A), Mn(II)-MTD-2-Amp (B), and Co(II)-MTD-2-Amp (C) in an aqueous medium. Results: The obtained colored complexes are spectrophotometrically measured for the previously mentioned complexes at 572, 473, and 465 nm, respectively. Under optimum conditions, the complexes exhibited apparent, molar absorptivities of 1810.62, 2954.18, and 2596.8 l/mol/cm, Sandell’s sensitivity of 0.132, 0.08, and 0.092 μg/cm2, and Beer–Lambert’s law is obeyed over the ranges 4–40, 4–32, and 4–40 μg/ml for the three developed methods, respectively. Conclusion: The developed spectrophotometric methods showed excellent results in regard to accuracy and precision with recovery of 99.48±1.62%, 100.24±1.76%, and 100.72±1.65% of the complexes A, B, and C, respectively. The obtained results are compared statistically with a reported method with respect to t- and F-tests and the calculated results displayed no significant difference.

scholarly journals Spectrophotometric determination of tadalafil in pure and dosage forms

2011 ◽  
Vol 17 (2) ◽  
pp. 125-132 ◽  
Author(s):  
Kaf Al ◽  
Ayman Gouda
Keyword(s):  
Ion Pairs ◽  
Dosage Forms ◽  
Ion Pair ◽  
Bromocresol Purple ◽  
Buffer Solution ◽  
Spectrophotometric Methods ◽  
Basic Nitrogen ◽  
Accuracy And Precision ◽  
Tablet Dosage

Two simple, rapid, and extractive spectrophotometric methods were developed for the determination of tadalafil (TDF) in both pure and tablet dosage form. These methods are based on the formation of ion-pair complexes between the basic nitrogen of the drug with bromocresol purple (BCP) and methyl orange (MO) in acidic buffer solution. The formed complexes were extracted with chloroform and measured at 410 and 425 nm using BCP and MO, respectively. Beer?s law was obeyed in the range 2.0-20 ?g mL?1 with correlation coefficient (n = 6) ? 0.9996. The molar absorpitivity, Sandell sensitivity, detection and quantification limits were also calculated. The composition of the ion pairs was found 1:1 by Job?s method. The proposed methods have been applied successfully for the analysis of TDF in pure and in its dosage forms. These developed methods were validated for accuracy and precision.

scholarly journals A Simple and Rapid RP-HPLC Method for the Estimation of Nevirapine in Bulk and Pharmaceutical Dosage Forms

2008 ◽  
Vol 5 (s2) ◽  
pp. 1081-1086
Author(s):  
Palaniappan Mohanraj ◽  
Deb Kumar Sarkar ◽  
Tirthankar Choudhury ◽  
Karunakaran Gauthaman
Keyword(s):  
Limit Of Detection ◽  
Dosage Forms ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Accuracy And Precision ◽  
Tablet Dosage

A reverse phase HPLC method is described for the determination of nevirapine in tablet dosage forms. Chromatography was carried on an ODS column using a mixture of methanol and water (89:11 v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 284 nm. The retention time of the drug was 3.22 min. The detector response was linear in the concentration of 25-200 mcg/mL. The limit of detection and limit of quantification was 0.004 and 0.0121 mcg/mL respectively. The percentage assay of nevirapine was 99.52%. The method was validated by determining its sensitivity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of nevirapine in bulk and tablet dosage forms.

scholarly journals Development and Validation of Spectrophotometric Methods for Determination of Fluoxetine, Sertraline, and Paroxetine in Pharmaceutical Dosage Forms

2005 ◽  
Vol 88 (1) ◽  
pp. 38-45 ◽  
Author(s):  
Ibrahim A Darwish
Keyword(s):  
Correlation Coefficients ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Factors Affecting ◽  
Spectrophotometric Methods ◽  
Linear Relationships ◽  
Relative Standard ◽  
Optimum Reaction ◽  
Standard Deviations

Abstract Three simple and sensitive spectrophotometric methods were developed and validated for determination of the hydrochloride salts of fluoxetine, sertraline, and paroxetine in their pharmaceutical dosage forms. These methods were based on the reaction of the N-alkylvinylamine formed from the interaction of the free secondary amino group in the investigated drugs and acetaldehyde with each of 3 haloquinones, i.e., chloranil, bromanil, and 2,3-dichloronaphthoquinone, to give colored vinylamino-substituted quinones. The colored products obtained with chloranil, bromanil, and 2,3-dichloronaphthoquinone exhibit absorption maxima at 665, 655, and 580 nm, respectively. The factors affecting the reactions were studied and optimized. Under the optimum reaction conditions, linear relationships with good correlation coefficients (0.9986–0.9999) were found between the absorbances and the concentrations of the investigated drugs in the range of 4–120 μg/mL. The limits of detection for the assays ranged from 1.19 to 2.98 μg/mL. The precision values of the methods were satisfactory; the relative standard deviations were 0.56–1.24%. The proposed methods were successfully applied to the determination of the 3 drugs in pure and pharmaceutical dosage forms with good accuracy; the recoveries ranged from 99.1 to 101.3% with standard deviations of 1.15–1.92%. The results compared favorably with those of reported methods.

scholarly journals Use of N, N-diethyl-p-phenylenediamine sulphate for the spectrophotometric determination of some phenolic and amine drugs

2010 ◽  
Vol 60 (2) ◽  
pp. 217-227 ◽  
Author(s):  
Padmarajaiah Nagaraja ◽  
Ashwinee Shrestha ◽  
Anantharaman Shivakumar ◽  
Avinash Gowda
Keyword(s):  
Spectrophotometric Determination ◽  
Correlation Coefficients ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Variable Parameters ◽  
Spectrophotometric Methods ◽  
Linear Relationships ◽  
Colored Product ◽  
And Performance

Use ofN, N-diethyl-p-phenylenediamine sulphate for the spectrophotometric determination of some phenolic and amine drugsSpectrophotometric methods are proposed for the determination of drugs containing a phenol group [salbutamol sulphate (SLB), ritodrine hydrochloride (RTD), isoxsuprine hydrochloride (IXP)] and drugs containing an aromatic amine group [dapsone hydrochloride (DAP), sulfamethoxazole (SFM), and sulfadiazine (SFD)] in pharmaceutical dosage forms. The methods are based on coupling ofN, N-diethyl-p-phenylenediamine sulphate with the drugs in the presence of KIO4to give a green colored product (λmaxat 670 nm) and a red colored product (λmaxat 550 nm), respectively. Linear relationships with good correlation coefficients (0.9986-0.9996) were found between absorbance and the corresponding concentration of drugs in the range 1-7, 2-22, 1-17, 1.5-12, 2-25, and 2-21 μg mL-1for SLB, RTD, IXP, DAP, SFM and SFD, respectively. Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. The RSD of intra-day and inter-day studies was in the range of 0.2-1.0 and 0.4-1.0%, respectively. No interference was observed from common pharmaceutical adjuvants. The reliability and performance of the proposed methods was validated statistically; the percentage recovery ranged from 99.5 ± 0.1 to 99.9 ± 0.3%. Limits of detection were 0.14, 0.21, 0.51, 0.44, 0.33 and 0.37 μg mL-1for SLB, RTD, IXP, DAP, SFM, and SFD, respectively.

Fully Validated Simultaneous Determination of Bisoprolol Fumarate and Hydrochlorothiazide in Their Dosage Forms Using Different Voltammetric, Chromatographic, and Spectrophotometric Analytical Methods

2013 ◽  
Vol 96 (1) ◽  
pp. 42-51 ◽  
Author(s):  
Burcin Bozal ◽  
Mehmet Gumustas ◽  
Burcu Dogan -Topal ◽  
Bengi Uslu ◽  
Sibel A Ozkan
Keyword(s):  
Simultaneous Determination ◽  
Square Wave Voltammetry ◽  
Internal Standard ◽  
Differential Pulse ◽  
Dosage Forms ◽  
Spectrophotometric Methods ◽  
Rp Hplc ◽  
Wave Voltammetry ◽  
Tablet Dosage

Abstract Voltammetric, chromatographic, and spectrophotometric methods were developed for the simultaneous determination of bisoprolol fumarate (BIS) and hydrochlorothiazide (HCZ). Differential pulse and square wave voltammetry techniques were used to analyze BIS and HCZ simultaneously by measuring at about 1400 and 1100 mV, respectively. RP-HPLC was the second method for simultaneous analysis of the compounds. The mixture of BIS, HCZ, and moxifloxacin as an internal standard was separated on an RP Zorbax Eclipse XDB-C18 column (150 × 4.6 mm, id, 5 μm particle size) using acetonitrile–15 mM phosphate (25 + 75, v/v) mobile phase at a 1.0 mL/min flow rate. The third method was based on first derivative of the ratio-spectra method obtained from the measurements of the amplitudes at 246 and 257 nm for BIS and HCZ, respectively. All the proposed methods were effectively applied for the simultaneous determination of BIS and HCZ in tablet dosage forms without any time-consuming extraction, sample preparation, or derivatization procedures.

scholarly journals Direct Spectrophotometric Determination of Cefuroxime Axetil in Pure Form and Pharmaceutical Dosage Forms.

2018 ◽  
Vol 15 (2) ◽  
pp. 6282-6295
Author(s):  
Abdul Aziz Ramadan ◽  
Marwa Bakdash
Keyword(s):  
Reference Method ◽  
Cost Effective ◽  
Bromothymol Blue ◽  
Cefuroxime Axetil ◽  
Dosage Forms ◽  
Experimental Conditions ◽  
Pharmaceutical Dosage Forms ◽  
Tablet Dosage ◽  
Good Agreement

A simple, direct and cost-effective spectrophotometric method for determination of cefuroxime axetil (CRXA)  in pure and tablet dosage forms was applied. This method is based on formation of ion-pair complex ([CRXA]:[BTB]) between CRXA and bromothymol blue (BTB) in chloroform. Beer’s law in the optimum experimental conditions using [CRXA]:[BTB] complex is valid within a concentration range of 2.00-50.00 ?M (1.021–25.524 ?g.mL-1). The developed method is applied for the determination of CRXA in pure and its commercial tablets without any interference from excipients with average assay of 96.8 to 101.6% and the results are in good agreement with those obtained by the HPLC reference method. Associated drugs (sulbactam and linesolid) with cefuroxime axetil are considered to be interfere, while metronidazole can be considered as non-interfere.

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