Simeprevir oxidative degradation product: Molecular modeling,in silicotoxicity and resolution by synchronous spectrofluorimetry

Luminescence ◽  
2017 ◽  
Vol 33 (2) ◽  
pp. 382-390 ◽  
Author(s):  
Khalid A. M. Attia ◽  
Nasr M. El-Abasawi ◽  
Ahmed El-Olemy ◽  
Ahmed Serag
Keyword(s):  
Molecular Modeling ◽  
Degradation Product ◽  
Oxidative Degradation ◽  
Synchronous Spectrofluorimetry

Stability-Indicating Chromatographic Methods for the Investigation of Ritodrine Hydrochloride Stability and Characterization of the Oxidative Degradation Product

2019 ◽  
Vol 57 (8) ◽  
pp. 730-737
Author(s):  
Noha Salem Rashed ◽  
Ola Mostafa Abdallah ◽  
Ahmed El-Olemy ◽  
Asmaa Ibrahim Hosam Eldin
Keyword(s):  
Degradation Product ◽  
Mobile Phase ◽  
Oxidative Degradation ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Chromatographic Methods ◽  
Ritodrine Hydrochloride ◽  
Accuracy And Precision ◽  
Intact Drug

Abstract Two simple and sensitive chromatographic methods were developed and validated for quantitative determination of ritodrine hydrochloride in presence of its oxidative degradation product. The first method depends on densitomeric determination of thin-layer chromatograms of the intact drug in presence of its oxidative degradate. Excellent separation was achieved at 220 nm using a mobile phase of dichloromethane–methanol–glacial acetic acid (15 : 5 : 0.25, v/v/v). The second was an HPLC method, in which efficient separation was carried out on C18 column (150 × 4.6 × 5 μm) using a mobile phase consisting of water: acetonitrile (70,30, v/v) at a flow rate of 1 mL min−1 and UV detection at 220 nm. Beer’s law was obeyed in the range of 0.025–0.3 μg/spot and 5–40 μg mL−1 of the intact drug using the two methods, respectively. The proposed methods were validated according to International Conference on Harmonization guidelines and successfully applied for the determination of ritodrine hydrochloride in bulk powder, laboratory prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The results obtained were compared with those of the reported method and were found to be in good agreement.

scholarly journals Column Liquid Chromatography-Ultraviolet and Column Liquid Chromatography/Mass Spectrometry Evaluation of Stress Degradation Behavior of Escitalopram Oxalate

2009 ◽  
Vol 92 (1) ◽  
pp. 138-147 ◽  
Author(s):  
Sunil R Dhaneshwar ◽  
Mahadeo V Mahadik ◽  
Mahesh J Kulkarni
Keyword(s):  
Mass Spectrometry ◽  
Column Liquid Chromatography ◽  
Liquid Chromatography ◽  
Degradation Product ◽  
Degradation Products ◽  
Oxidative Degradation ◽  
Stress Conditions ◽  
Assay Method ◽  
Infrared Spectrometry ◽  
Degradation Behavior

Abstract The objective of this work was to study the degradation behavior of escitalopram oxalate under different International Conference on Harmonization (ICH)-recommended stress conditions by column liquid chromatography (LC)-UV and LC/mass spectrometry (LC/MS) and to establish a validated stability-indicating LC assay method. Escitalopram oxalate was subjected to stress conditions of hydrolysis, oxidation, photolysis, and thermal decomposition. Extensive degradation was found to occur in alkaline medium. Mild degradation was observed in acidic and oxidative conditions. Escitalopram oxalate was stable to neutral, photolytic, and thermal stress. Successful separation of the drug from degradation products formed under stress conditions was achieved on a PerfectSil-100 ODS-3 column [C18 (5 m, 25 cm 4.6 mm id)] using methanol0.01 M acetate buffer pH 3.8 adjusted with acetic acid (45 + 55) as the mobile phase. The flow rate was 1 mL/min, and the detection wavelength was 239 nm. The method was validated according to ICH guidelines. Major degradation products formed in hydrolysis and oxidative conditions were isolated, and structural elucidation of degradation products was done by LC/MS and infrared spectrometry studies. The major hydrolysis degradation product was confirmed as 1-(3-dimethylaminopropyl)-1-(4-fluoro- phenyl)-1,3dihydroisobenzofuran-5-carboxylic acid, and the major oxidative degradation product was confirmed as 1-{[3-dimethylamino(oxide)- propyl]-1-(4-fluro-phenyl)}-1,3-dihydro-isobenzofuran- 5-carbonitrile.

Development and Validation of Stability Indicating High-Performance Liquid Chromatographic Method for Determination of Cyproheptadine Hydrochloride, its Impurity And Degradation Product

2020 ◽  
Author(s):  
Maha M Abdelrahman ◽  
Eglal A Abdelaleem ◽  
Nouruddin W Ali ◽  
Raghda A Emam
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Oxidative Degradation ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Good Resolution ◽  
Intermediate Precision ◽  
Rp Hplc

Abstract This work presents a sensitive, accurate and selective RP-HPLC method for simultaneous determination of cyproheptadine HCl (CPH), its impurity B (dibenzosuberone) and CPH oxidative degradation product (10,11-dihydroxy-dibenzosuberone) in bulk powder and in pharmaceutical formulation. The RP-HPLC method depends on isocratic elution using C8 column and mobile phase consisting of 0.05 M KH2PO4 buffer:methanol (35:65, v/v, pH = 4.5) at a flow rate of 2 mL/min, and the eluant was monitored at 245 nm. Good resolution was obtained with tR values of 3.05, 7.54 and 6.17 min for CPH, impurity and oxidative degradate, respectively. The proposed method has been validated as per ICH guidelines using pure forms of CPH, its impurity and degradation product in pharmaceutical formulation with an accuracy of 100.48, 100.16 and 100.11, respectively. Additional spiking experiments yielded an accuracy of 100 ± 1.6%. Repeatability and intermediate precision results indicated acceptable low <2% RSD values. Moreover, the developed method’s statistical results were favorably compared to the previously reported method results regarding both accuracy and precision. The developed method can be applied for analysis of the three components in quality control laboratories.

Comparative Study Between Zero-Order Spectra-Processing and Ratio Spectra-Manipulating Methods Applied for the Determination of Isoxsuprine Hydrochloride in the Presence of Its Oxidative Degradation Product

2017 ◽  
Vol 100 (6) ◽  
pp. 1739-1746 ◽  
Author(s):  
Khalid A M Attia ◽  
Nasr M A El-Abassawi ◽  
Ragab A M Said ◽  
Ahmed El-Olemy ◽  
Sherif Ramzy
Keyword(s):  
Degradation Product ◽  
Oxidative Degradation ◽  
Area Under The Curve ◽  
Standard Addition ◽  
Zero Order ◽  
Spectrophotometric Methods ◽  
The Third ◽  
Ratio Difference ◽  
Spectra Processing

Abstract Four accurate, precise, and validated stability-indicating spectrophotometric methods handling either zero-order spectra or ratio spectra have been developed and compared for the analysis of isoxsuprine hydrochloride (ISX) in the presence of its oxidative degradation product. The first two methods processed zero-order spectra, namely graphical absorbance ratio or Q-Analysis and area under the curve, whereas the third and fourth methods manipulated ratio spectra, namely the ratio difference spectrophotometric method and derivative ratio. The proposed methods showed good linearity in the range of 2–23 µg/mL. The methods were tested for specificity using laboratory-prepared mixtures containing the drug and its degradation product. The proposed methods were applied for the determination of ISX in Vascular tablets and the obtained results were acceptable, with small percentage RSD values. The validity of the proposed procedures was further assessed by applying the standard addition technique, which showed no interference from excipients. The obtained results were statistically compared with those obtained by the reported method, showing no significant differences when t- and F-tests were applied.

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