scholarly journals Development and Validation of an Extractive Spectrophotometric Method for Miconazole Nitrate Assay in Pharmaceutical Formulations

2018 ◽  
Vol 2018 ◽  
pp. 1-5
Author(s):  
Tadele Eticha ◽  
Getu Kahsay ◽  
Teklebrhan Hailu ◽  
Tesfamichael Gebretsadikan ◽  
Fitsum Asefa ◽  
...  
Keyword(s):  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Bromocresol Green ◽  
Ich Guidelines ◽  
Miconazole Nitrate ◽  
Method Of Continuous Variation ◽  
Development And Validation ◽  
Job's Method ◽  
Full Factorial

A simple extractive spectrophotometric technique has been developed and validated for the determination of miconazole nitrate in pure and pharmaceutical formulations. The method is based on the formation of a chloroform-soluble ion-pair complex between the drug and bromocresol green (BCG) dye in an acidic medium. The complex showed absorption maxima at 422 nm, and the system obeys Beer’s law in the concentration range of 1–30 µg/mL with molar absorptivity of 2.285 × 104 L/mol/cm. The composition of the complex was studied by Job’s method of continuous variation, and the results revealed that the mole ratio of drug : BCG is 1 : 1. Full factorial design was used to optimize the effect of variable factors, and the method was validated based on the ICH guidelines. The method was applied for the determination of miconazole nitrate in real samples.

Extractive Spectrophotometric Method for the Determination of Glibenclamide by Ion-Pair Complex in Pure Form and Pharmaceutical Formulation

2019 ◽  
Vol 9 (o3) ◽  
Author(s):  
RUAA MUAYAD MAHMOOD ◽  
HAMSA MUNAM YASSEN ◽  
SAMAR , NAJWA ISSAC ABDULLA AHMED DARWEESH ◽  
NAJWA ISSAC ABDULLA
Keyword(s):  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Pharmaceutical Formulation ◽  
Ratio Method ◽  
Colored Complex ◽  
Colored Product ◽  
Method Of Continuous Variation ◽  
Job's Method

Simple, rapid and sensitive extractive spectrophotometric method is presented for the determination of glibenclamide (Glb) based on the formation of ion-pair complex between the Glb and anionic dye, methyl orange (MO) at pH 4. The yellow colored complex formed was quantitatively extracted into dichloromethane and measured at 426 nm. The colored product obeyed Beer’s law in the concentration range of (0.5-40) μg.ml-1. The value of molar absorptivity obtained from Beer’s data was found to be 31122 L.mol-1.cm-1, Sandell’s sensitivity value was calculated to be 0.0159 μg.cm-2, while the limits of detection (LOD) and quantification (LOQ) were found to be 0.1086 and 0.3292 μg.ml-1, respectively. The stoichiometry of the complex created between the Glb and MO was 1:1 as determined via Job’s method of continuous variation and mole ratio method. The method was successfully applied for the analysis of pharmaceutical formulation.

QBD BASED RP-HPLC METHOD FOR SCREENING AND ANALYSIS OF TELAPRAVIR AND 7 OTHER ANTIRETROVIRAL AGENTS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (02) ◽  
pp. 20-33
Author(s):  
N. S Kumar ◽  
◽  
R Kumaraswamy ◽  
S. Shantikumar ◽  
D. Paul
Keyword(s):  
Quality By Design ◽  
Pharmaceutical Formulations ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Full Factorial

The present study describes the separation and simultaneous estimation of eight anti-retroviral drugs, namely, Telaprevir (TPV), Emtricitabine (ECB), Fosamprenavir (FANV), Tenofavir (TNF), Ritonavir (RNV), Raltegravir (RGV) and Oseltamivir (OSMV) and Zidovudine (ZDV) as an active pharmaceutical ingredient, by RP-HPLC method by applying the principles of Quality by Design (QbD). An application of DoE (Design of Experiments) full factorial design was used for initial screening and optimization. The final optimized method consists of separation being carried out on a Fortis C18 column (150 mm × 4.6 mm, 5μ particle size) using acetonitrile and 10 mm ammonium formate buffer (pH 3 adjusted with formic acid) using a gradient program. The quantitative evaluation was performed with a diode array detector at 251 nm and 230 nm with a flow rate of 1 mL min–1. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the International Conference on Harmonization (ICH) guidelines. The method is selective, precise, robust and accurate and can be used for routine analysis of pharmaceutical formulations in quality control and counterfeit screening.

scholarly journals Application of Cerium (IV) as an Oxidimetric Agent for the Determination of Ethionamide in Pharmaceutical Formulations

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagib A. S. Qarah ◽  
Sameer A. M. Abdulrahman
Keyword(s):  
Quality Control ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Sample Solution ◽  
Standing Time ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Back Titration ◽  
Bulk Drug

Two simple methods are described for the determination of ethionamide (ETM) in bulk drug and tablets using cerium (IV) sulphate as the oxidimetric agent. In both methods, the sample solution is treated with a measured excess of cerium (IV) solution in H2SO4 medium, and after a fixed standing time, the residual oxidant is determined either by back titration with standard iron (II) solution to a ferroin end point in titrimetry or by reacting with o-dianisidine followed by measurement of the absorbance of the orange-red coloured product at 470 nm in spectrophotometry. In titrimetry, the reaction proceeded with a stoichiometry of 1 : 2 (ETM : Ce (IV)) and the amount of cerium (IV) consumed by ETM was related to the latter’s amount, and the method was applicable over 1.0–8.0 mg of drug. In spectrophotometry, Beer’s law was obeyed over the concentration range of 0.5–5.0 μg/mL ETM with a molar absorptivity value of 2.66 × 104 L/(mol·cm). The limits of detection (LOD) and quantification (LOQ) calculated according to ICH guidelines were 0.013 and 0.043 μg/mL, respectively. The proposed titrimetric and spectrophotometric methods were found to yield reliable results when applied to bulk drug and tablets analysis, and hence they can be applied in quality control laboratories.

scholarly journals Development and Validation of an HPLC Method for the Determination of the macrolide antibiotic Clarithromycin using Evaporative Light Scattering Detector in raw materials and Pharmaceutical Formulations

2017 ◽  
Vol 6 (4) ◽  
pp. 133-141 ◽  
Author(s):  
Zampia Tzouganaki ◽  
Michael Koupparis
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Gas Flow ◽  
Raw Materials ◽  
Pharmaceutical Formulations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Development And Validation

In this work, ELS-Detector has been used for the development of an HPLC method for the determination of clarithromycin in pharmaceutical formulations (tablets and pediatric suspension). Isocratic reversed phase HPLC approach has been developed using a C-18 column (Waters Spherisorb 5 μm ODS2, 4.6x250 mm) and a mobile phase consisting of acetonitrile / aqueous trifluoroacetic acid as pairing reagent. Experimental parameters (temperature of heated drift tube, flow rate of mobile phase, gas flow rate, mobile phase composition) were optimized. Clarithromycin’ s stability was thoroughly examined in different solvent systems. Using the optimized conditions the working range was 5-100 μg/mL (upper limit can be increased considerably), with a detection limit of 4.5 μg/mL (6x10-6 M). The method was validated as per ICH guidelines. The retention time was 4.7 min. The method was successfully applied for the content assay of clarithromycin formulations.

scholarly journals Stability indicating RP-HPLC method development and validation for the simultaneous estimation of ceftriaxone and tazobactum in sterile powder for injection

2019 ◽  
Vol 1 (2) ◽  
pp. 40-43
Author(s):  
T. Vimalakkannan ◽  
P. Shaik Parveen ◽  
Salomi ◽  
K. Ravindra Reddy
Keyword(s):  
Method Development ◽  
Pharmaceutical Formulations ◽  
Accurate Method ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation

A simple, rapid, precise and accurate method is developed for the quantitative simultaneous determination of ceftriaxone and tazobactum in bulk and pharmaceutical formulations. Separation of ceftriaxone and tazobactum was successfully achieved by using Inertsil C18 ODS column 250X4.6mm, 5µm in an isocratic mode using water and acetonitrile (80:20) at a flow rate of 1.0 ml/min and was monitored at 254 nm with a retention time of 3.049 minutes and 4.317 minutes for ceftriaxone and tazobactum respectively. The method was validated and the response was found to be linear in the drug concentration range of 20µg/ml to 80 µg/ml for ceftriaxone and 5 µg/ml to 35 µg/ml for tazobactum. The values of the correlation coefficient were found to be 0.999 for ceftriaxone and 0.999 for tazobactum respectively. The LOD and LOQ for ceftriaxone were found to be 0.021 and 0.064 respectively. The LOD and LOQ for tazobactum were found to be 0.030 and 0.091 respectively. The percentage recovery for ceftriaxone and tazobactum were found to be 98-102% respectively which indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample. The method was extensively validated according to ICH guidelines for Linearity, Accuracy, Precision, Specificity and Robustness.  Stability of the drugs was determined by using acid/base, thermal, oxidative stress testing.

scholarly journals Development and Validation of Simple UV Spectrophotometric Method for the Estimation of Dextromethorphan Hydrobromide in Bulk and Marketed Dosage Formulations

2016 ◽  
Vol 8 (03) ◽  
Author(s):  
Vineeta V. Khanvilkar ◽  
Rupali Kothekar
Keyword(s):  
Spectrophotometric Method ◽  
Pharmaceutical Formulations ◽  
Solid Dosage ◽  
Ich Guidelines ◽  
Chewable Tablets ◽  
Label Claim ◽  
Development And Validation ◽  
Dextromethorphan Hydrobromide ◽  
Good Agreement

A simple, rapid and economic UV spectrophotometric method has been developed and validated using a solvent 0.1N HCl to determine Dextromethorphan hydrobromide content in bulk and two different pharmaceutical solid dosage formulations, lozenges and chewable tablets. At the pre-determined λmax of 278 nm, it was proved linear in the range of 5.0-30.0 µg/ml and exhibited good correlation coefficient (R2=0.9993) and excellent mean recovery (101.37-100.76%) and (100.66-101.17%) for lozenges and chewable tablets respectively. This method was successfully applied to the determination of Dextromethorphan hydrobromide content in lozenges and chewable tablets and the results were in good agreement with the label claim. The method was validated as per ICH guidelines for linearity, precision, accuracy, specificity, LOD and LOQ. The obtained results proved that the method can be employed for the routine analysis of Dextromethorphan hydrobromide in bulks as well as in the pharmaceutical formulations.

scholarly journals Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF254for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

2015 ◽  
Vol 2015 ◽  
pp. 1-9 ◽  
Author(s):  
Małgorzata Dołowy ◽  
Alina Pyka
Keyword(s):  
Silica Gel ◽  
Mobile Phase ◽  
Research Study ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Simple Economic

This research study describes the applicability of silica gel 60 RPW18F254plates for the development and validation of new, simple, economic, accurate, and precise RPHPTLC-densitometric method suitable for the quantification of nicotinamide (asVitamin PP) in three marketed preparations. The mobile phase used was methanol-water in volume composition 3 : 7. Detection wavelength was 200 nm. The proposed method was validated according to ICH guidelines and also based on Ferenczi-Fodor and Konieczka reports. Results were found to be linear over a range of 1.00 to 2.00 μg/spot. Limit of detection (LOD) and limit of quantification (LOQ) were 0.15 μg/spot and 0.45 μg/spot, respectively. The percent content of nicotinamide in the investigated preparations was found to be 99.2% (Product 1), 99.3% (Product 2), and 99.4% (Product 3). Developed method is accurate and precise (CV<3%) and may be successfully applied for the quality control of pharmaceutical formulations containing nicotinamide in the presence of its derivatives, such as N,N-diethylnicotinamide, N-methylnicotinamide, and nicotinic acid.

scholarly journals DEVELOPMENT AND VALIDATION OF SPECTROPHOTOMETRIC METHOD FOR THE DETERMINATION OF DPP-4 INHIBITOR, SITAGLIPTIN, IN ITS PHARMACEUTICAL PREPARATIONS

2018 ◽  
Vol 35 (3) ◽  
pp. 45
Author(s):  
C. Bala Sekaran ◽  
A. Prameela Rani
Keyword(s):  
Spectrophotometric Method ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Amino Group ◽  
Reaction Conditions ◽  
Colored Product ◽  
Primary Amino ◽  
Development And Validation

A simple, sensitive and reproducible spectrophotometric method was developed for the determination of sitagliptin phosphate in bulk and in pharmaceutical formulations. The proposed method is based on condensation of the primary amino group of sitagliptin phosphate with acetyl acetone and formaldehyde producing a yellow colored product, which is measured spectrophotometrically at 430nm. The color was stable for about 1 hour. Beer’s law is obeyed over a concentration range of 5-25 μg/ml. The apparent molar absorptivity and Sandell sensitivity values are 1.067 x 104 Lmol-1cm-1 and 0.0471 μgcm-2 respectively. All the variables were studied to optimize the reaction conditions. No interference was observed in the presence of common pharmaceutical excipients. The validity of the method was tested by analyzing sitagliptin phosphate in its pharmaceutical preparations. Good recoveries were obtained. The developed method was successfully employed for the determination of sitagliptin phosphate in various pharmaceutical preparations.

Extraction and spectrophotometric determination of molybdenum(VI) with N-phenylbenzohydroxamic acid and phenylfluorone

1987 ◽  
Vol 65 (5) ◽  
pp. 1124-1127 ◽  
Author(s):  
H. Dasaratha Gunawardhana ◽  
S. Amarasiri Fernando
Keyword(s):  
Hydrochloric Acid ◽  
Steel Sample ◽  
Chloroform Extract ◽  
Molar Absorptivity ◽  
Hydrochloric Acid Medium ◽  
Coloured Complex ◽  
Method Of Continuous Variation ◽  
Job's Method ◽  
Standard Steel

N-Phenylbenzohydroxamic acid reacts with molybdenum(VI) in 3.5–6.0 M hydrochloric acid to give a complex that is extractable into chloroform. The chloroform extract of the molybdenum complex, on second extraction from a dilute hydrochloric acid medium (0.2–0.3 M) in the presence of phenylfluorone and ethanol, forms an intensely coloured complex possessing an absorption maximum at 518 nm. Job's method of continuous variation reveals that the complex is Mo(VI)—2NPBHA—PF. The molar absorptivity under optimum conditions is 7.4 × 104 cm3 mol−1 cm−1. The system obeys Beer's law up to 0.6 ppm of molybdenum(VI). Considerable amounts of many cations and anions can be tolerated. The interference from vanadium(IV) and vanadium(V) can be eliminated by the addition of sodium metabisulphite, whereas the interference from titanium(IV) is mitigated by oxalate ions. The method has been successfully applied for the determination of molybdenum in a standard steel sample.

scholarly journals Sensitive Spectrophotometric Determination of Lamotrigine in Bulk Drug and Pharmaceutical Formulations using Bromocresol Green

2018 ◽  
Vol 35 (1) ◽  
pp. 55
Author(s):  
N. Rajendraprasad ◽  
K. Basavaiah ◽  
K. B. Vinay
Keyword(s):  
Potassium Hydroxide ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Bromocresol Green ◽  
Spectrophotometric Methods ◽  
Base Form ◽  
Bulk Drug ◽  
The Stability

Two new, simple, rapid and reproducible spectrophotometric methods have been developed for the determination of lamotrigine (LMT) both in pure form and in its tablets. The first method (method A) is based on the formation of a colored ion-pair complex (1:1 drug/dye) of LMT with bromocresol green (BCG) at pH 5.02±0.01 and extraction of the complex into dichloromethane followed by the measurement of the yellow ion-pair complex at 410 nm. In the second (method B), the drug-dye ion-pair complex was dissolved in ethanolic potassium hydroxide and the resulting base form of the dye was measured at 620 nm. Beer’s law was obeyed in the concentration range of 1.5-15 μg mL-1 and 0.5-5.0 μg mL-1 for method A and method B, respectively, and the  = corresponding molar absorptivity values are 1.6932 x 104 and 3.748 x 104L mol-1cm-1. The Sandell sensitivity values are 0.0151 and 0.0068 μg cm-2 for method A and method B, respectively. The stoichiometry of the ion-pair complex formed between the dug and dye (1:1) was determined by Job’s continuous variations method and the stability constant of the complex was also calculated. The proposed methods were applied successfully for the determination of drug in commercial tablets.

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