scholarly journals Colorimetric Assay of Cimetidine in the Presence of Its Oxidative Degradates

2009 ◽  
Vol 92 (2) ◽  
pp. 382-386 ◽  
Author(s):  
Alaa S Amin ◽  
Hassan A Dessouki ◽  
Sayed A Shama ◽  
Eslam A Gouda
Keyword(s):  
Rhodamine 6G ◽  
Degradation Products ◽  
Colorimetric Assay ◽  
Oxidative Degradation ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Stoichiometric Ratio ◽  
Relative Standard ◽  
Chromotrope 2R

Abstract Three simple, accurate, and sensitive colorimetric methods for the determination of cimetidine (Cim) in pure form, in dosage forms, and in the presence of its oxidative degradates were developed. These methods are indirect, involve the addition of excess oxidant N-bromosuccinimide (NBS) for method A; cerric sulfate Ce(SO4)2 for methods B and C of known concentration in acid medium to Cim, and the determination of the unreacted oxidant by measurement of the decrease in absorbance of amaranth dye for method A, chromotrope 2R for method B, and rhodamine 6G, for method C at a suitable maximum wavelength, max: 520, 528, and 525 nm, for the 3 methods, respectively. Regression analysis of the Beer plots showed good correlation in the concentration ranges of 0.24.4 g/mL for method A, and 0.23.4 g/mL for methods B and C. The apparent molar absorptivity, Sandell sensitivity, and detection and quantitation limits were evaluated. The stoichiometric ratio between the drug (Cim) and the oxidant (NBS or Ce 4) was estimated. The validity of the proposed methods was tested by analyzing pure and dosage forms containing Cim with relative standard deviation 1.18. The proposed methods could successfully determine the studied drug with varying excess of its oxidative degradation products, with recovery between 99.2 and 101.8, 100.2 and 102.8, and 99.8 and 102.0 for methods AC, respectively.

scholarly journals Development and Validation of Stability Indicating Spectroscopic Method for Content Analysis of Ceftriaxone Sodium in Pharmaceuticals

2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Revathi Ethiraj ◽  
Ethiraj Thiruvengadam ◽  
Venkattapuram Saravanan Sampath ◽  
Abdul Vahid ◽  
Jithin Raj
Keyword(s):  
Spectroscopic Method ◽  
Oxidative Degradation ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Stability Indicating ◽  
Ceftriaxone Sodium ◽  
Relative Standard ◽  
Validation Parameters ◽  
Development And Validation

A simple, selective, and stability indicating spectroscopic method has been selected and validated for the assay of ceftriaxone sodium in the powder for injection dosage forms. Proposed method is based on the measurement of absorbance of ceftriaxone sodium in aqueous medium at 241 nm. The method obeys Beer’s law in the range of 5–50 μg/mL with correlation coefficient of 0.9983. Apparent molar absorptivity and Sandell’s sensitivity were found to be 2.046×103 L mol−1 cm−1 and 0.02732 μg/cm2/0.001 absorbance units. This study indicated that ceftriaxone sodium was degraded in acid medium and also underwent oxidative degradation. Percent relative standard deviation associated with all the validation parameters was less than 2, showing compliance with acceptance criteria of Q2 (R1), International Conference on Harmonization (2005) guidelines. Then the proposed method was successfully applied to the determination of ceftriaxone sodium in sterile preparation and results were comparable with reported methods.

ICH/FDA Guidelines-Compliant Validated Stability-Indicating HPLC-UV Method for the Determination of Axitinib in Bulk and Dosage Forms

2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Degradation Products ◽  
Internal Standard ◽  
Dosage Forms ◽  
Uv Detector ◽  
Stability Indicating ◽  
Therapeutic Benefits ◽  
Relative Standard

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.

scholarly journals Development and validation of spectrophotometric method for phenylephrine hydrochloride estimation in nasal drops formulations

2008 ◽  
Vol 27 (2) ◽  
pp. 149 ◽  
Author(s):  
Ivana Savić ◽  
Goran Nikolić ◽  
Vladimir Banković
Keyword(s):  
Standard Deviation ◽  
Sodium Hydroxide ◽  
Relative Standard Deviation ◽  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Development And Validation

Simple, accurate and reproducible UV-spectrophotometric method was developed and validated for the estimation of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. Phenylephrine hydrochloride was estimated at 291 nm in 1 mol⋅dm-3 sodium hydroxide (pH 13.5). Beer’s law was obeyed in the concentration range of 10–100 μg⋅cm−3 (r2 = 0.9990) in the sodium hydroxide medium. The apparent molar absorptivity was found to be 1.63×103 dm3⋅mol−1⋅cm−1. The method was tested and validated for various parameters according to the ICH (International Conference on Harmonization) guidelines. The detection and quantitation limits were found to be 0.892 and 2.969 μg⋅cm−3, respectively. The proposed method was successfully applied for the determination of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation < 1 %), while being simple, cheap and less time consuming, and hence can be suitably applied for the estimation of phenylephrine hydrochloride in different dosage forms.

scholarly journals Utility of Charge Transfer and Ion-Pair Complexation for Spectrophotometric Determination of Eletriptan Hydrobromide in Pure and Dosage Forms

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Ayman A. Gouda ◽  
Ragaa El Sheikh ◽  
Rham M. El-Azzazy
Keyword(s):  
Charge Transfer ◽  
Correlation Coefficients ◽  
Standard Addition ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Ion Pair ◽  
Charge Transfer Complexes ◽  
Alizarin Red ◽  
Relative Standard

Three simple, sensitive, and accurate spectrophotometric methods have been developed for the determination of eletriptan hydrobromide (ELT) in pure and dosage forms. The first two methods are based on charge transfer complex formation between ELT and chromogenic reagents quinalizarin (Quinz) and alizarin red S (ARS) producing charge transfer complexes which showed an absorption maximum at 569 and 533 nm for Quinz and ARS, respectively. The third method is based on the formation of ion-pair complex between ELT with molybdenum(V)-thiocyanate inorganic complex in hydrochloric acid medium followed by extraction of the colored ion-pair with dichloromethane and measured at 470 nm. Different variables affecting the reactions were studied and optimized. Beer's law is obeyed in the concentration ranges 2.0–18, 1.0–8.0, and 2.0–32 μg mL−1for Quinz, ARS, and Mo(V)-thiocyanate, respectively. The molar absorptivity, Sandell sensitivity, detection, and quantification limits are also calculated. The correlation coefficients were ≥0.9994 with a relative standard deviation (R.S.D%.) of ≤0.925. The proposed methods were successfully applied for simultaneous determination of ELT in tablets with good accuracy and precision and without interferences from common additives, and the validity is assessed by applying the standard addition technique, which is compared with those obtained using the reported method.

scholarly journals Spectrophotometric Estimation of Cefuroxime and Ceftazidime in Bulk and in Dosage Forms

2001 ◽  
Vol 69 (2) ◽  
pp. 143-150 ◽  
Author(s):  
A. Amin ◽  
H. Khalli ◽  
H. Saleh
Keyword(s):  
Molar Absorptivity ◽  
Dosage Forms ◽  
Acetate Buffer Solution ◽  
Sodium Fluorescein ◽  
Buffer Solution ◽  
Experimental Conditions ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Optimum Concentration Range

Three simple, accurate and sensitive spectrophotometric methods (A, B and C) for the determination of cefuroxime and ceftazidime in bulk samples and in dosage forms are described. They are based on the reaction with nitrous acid forming a nitroso derivatives which can be measured at λmax 350 and 355 nm for cefuroxime (I) and ceftazidime (II), respectively (method A) or by oxidation of drug I or II with an excess of freshly prepared hypobromite and the residual hypobromite was treated with sodium fluorescein at the optimum experimental conditions and measured at λmax at 517 nm (method B). Method C is based on the formation of tris (0-phenanthroline) iron(II) complex (ferroin) upon the oxidation of the studied drug I or II with an iron (III)-o-phenanthroline mixture in acetate buffer solution of pH 3.6 and measuring at λmax 509 nm. Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 0.2 – 6.0, 0.2 – 3.2 and 0.1 – 5.6 μg ml−1 for methods A, B and C, respectively. The apparent molar absorptivity, Sandell sensitivity, detection and quantitation limits were calculated. For more accurate results, Ringbom optimum concentration range was 0.2 – 5.6 μg ml−1. The validity of the proposed methods was tested by analysing dosage forms containing the studied drugs I and II. The relative standard deviations were ≤ 1.25% with recoveries 98.6 – 101.4% .

Spectrophotometric Determination of Diethylpropion Hydrochloride Bulk Drug and Tablets in the Presence of Its Degradation Products

1991 ◽  
Vol 74 (4) ◽  
pp. 600-603
Author(s):  
Gamal A Saleh
Keyword(s):  
Association Constant ◽  
Charge Transfer Complex ◽  
Degradation Products ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Thiamine Hydrochloride ◽  
Pyridoxine Hydrochloride ◽  
Bulk Drug ◽  
Sensitive Spectrophotometric Method

Abstract The charge transfer complex formation between diethylpropion and iodine was investigated and used as the basis for a simple and sensitive spectrophotometric method for diethylpropion and Its dosage forms. The solution exhibited blueshifted iodine bands at 295 and 365 nm. A Job's plot Indicated a 1:1 complexatlon ratio. At 295 nm, the absorbance was linear (r = 0.9995) over the 0.2-2.4 μg/mL concentration range. The method has been applied successfully to the analysis of commercially available diethylpropion hydrochloride tablets without interference from thiamine hydrochloride, pyridoxine hydrochloride, nicotinamide, and riboflavin. Interference from the degradation products 1-phenyl-1,2- propanedione and diethylamine was avoided. Molar absorptivity, association constant, and free energy change were investigated further.

scholarly journals Colorimetric Assay of Thiamine Hydrochloride in Pharmaceutical Preparations

2019 ◽  
Vol 16 (4) ◽  
pp. 0898
Author(s):  
Ahmad Et al.
Keyword(s):  
Colorimetric Assay ◽  
Pharmaceutical Preparations ◽  
Aldehyde Group ◽  
Molar Absorptivity ◽  
Thiamine Hydrochloride ◽  
Schiff’S Base ◽  
Colored Complex ◽  
Relative Standard ◽  
Primary Amino

            A simple, rapid, accurate and sensitive spectrophotometric method for the determination of thiaminehydrochloride has been developed. The method is based on the formation of the Schiff’s base between the primary amino group present in thiamine hydrochloride and aldehyde group present in the vanillin reagent to produce a yellow colored complex having maximum absorption at 390 nm. Beer’s law has obeaid over the concentration range of 2-28µg/mL, with molar absorptivity of 0.96x104L/mol.cm. The average recovery which is a measure of accuracy is 100±1.3% and the relative standard deviation (RSD) is less than1.5 .The present method is considered to be simple because it does not need heating, hydrolysis and solvent extraction steps. The ingredients often formulated with thiamine and have been shown not to interfere, and is suitable for the routine determination of thiamine hydrochloride. The proposed method has been successfully applied for the determination of thiamine hydrochloride in pure form and in pharmaceutical preparations.

scholarly journals Spectrophotometric Determination of sulphadiazine by oxidative coupling reaction with ortho-amino phenol as reagent

2019 ◽  
Vol 24 (4) ◽  
pp. 40
Author(s):  
Aisha A. Abd ◽  
Ali I. Khaleel ◽  
, Faiez M. Hamed
Keyword(s):  
Oxidative Coupling ◽  
Coupling Reaction ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Oxidative Coupling Reaction ◽  
Relative Standard ◽  
Amino Phenol ◽  
532 Nm

A simple, rapid and sensitive spectrophotometric method for determination of sulphadiazine (SDZ) in aqueous solution is described. The method iis based on the oxidation of SDZ by potasium Periodate, and coupling with ortho-amino phenol to give a violet colour of  maximum absorbaance at 532 nm. Beer's law is obeyed over the concentration range of 5-40 µg /ml of SDZ with a (R2=0.9980) and molar absorptivity 5581.6 L.mol-1.cm-1  and a relative error in the range of - 0.06 - 2.3  % and a relative standard deviation of not more than 0.31 %. The composition of the resulting product is also investigated and it is found to be1:1. The method is successfully applied for the determinatiion of SDZ in pure and pharmaceutical dosage forms, with recovery of noot less than 101.1%.   http://dx.doi.org/10.25130/tjps.24.2019.070

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

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