scholarly journals Validated spectral manipulations for determination of an anti-neoplastic drug and its related impurities including its hazardous degradation product

RSC Advances ◽  
2021 ◽  
Vol 11 (35) ◽  
pp. 21332-21342
Author(s):  
Ibrahim A. Naguib ◽  
Eglal A. Abdelaleem ◽  
Eman S. Hassan ◽  
Aml A. Emam
Keyword(s):  
Absorption Spectra ◽  
Degradation Product ◽  
Zero Order ◽  
Sterile Water ◽  
Related Impurities ◽  
Amino Imidazole

Zero order absorption spectra of 12 μg mL−1 of Dacarbazine (), 5-amino-imidazole-4 carboxamide (), and 2-azahypoxanthine (…) using sterile water as a blank.

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.

scholarly journals A New Platform for Profiling Degradation-Related Impurities Via Exploiting the Opportunities Offered by Ion-Selective Electrodes: Determination of Both Diatrizoate Sodium and Its Cytotoxic Degradation Product

2018 ◽  
Vol 101 (3) ◽  
pp. 723-731 ◽  
Author(s):  
Safaa M Riad ◽  
Mohamed K Abd El-Rahman ◽  
Esraa M Fawaz ◽  
Mostafa A Shehata
Keyword(s):  
Degradation Product ◽  
Degradation Products ◽  
Ion Selective Electrodes ◽  
Selective Determination ◽  
Pharmaceutical Ingredients ◽  
Related Impurities ◽  
Chromatographic Methods ◽  
Stability Indicating Method ◽  
Impurity Profiling

Abstract Although the ultimate goal of administering active pharmaceutical ingredients (APIs) is to save countless lives, the presence of impurities and/or degradation products in APIs or formulations may cause harmful physiological effects. Today, impurity profiling (i.e., the identity as well as the quantity of impurity in a pharmaceutical) is receiving critical attention from regulatory authorities. Despite the predominant use of spectroscopic and chromatographic methods over electrochemical methods for impurity profiling of APIs, this work investigates the opportunities offered by electroanalytical methods, particularly, ion-selective electrodes (ISEs), for profiling degradation-related impurities (DRIs) compared with conventional spectroscopic and chromatographic methods. For a meaningful comparison, diatrizoate sodium (DTA) was chosen as the anionic X-ray contrast agent based on its susceptibility to deacetylation into its cytotoxic and mutagenic degradation product, 3,5-diamino-2,4,6 triiodobenzoic acid (DTB). This cationic diamino compound can be also detected as an impurity in the final product because it is used as a synthetic precursor for the synthesis of DTA. In this study, four novel sensitive and selective sensors for the determination of both DTA and its cytotoxic degradation products are presented. Sensors I and II were developed for the determination of the anionic drug, DTA, and sensors III and IV were developed for the determination of the cationic cytotoxic impurity. The use of these novel sensors not only provides a stability-indicating method for the selective determination of DTA in the presence of its degradation product, but also permits DRI profiling. Moreover, a great advantage of these proposed ISE systems is their higher sensitivity for the quantification of DTB relative to other spectroscopic and chromatographic methods, so it can measure trace amounts of DTB impurities in DTA bulk powder and pharmaceutical formulation without a need for preliminary separation.

Determination of Impurities in Perampanel Bulk Drugs by High-Performance Liquid Chromatography and Gas Chromatography

2020 ◽  
Vol 16 ◽  
Author(s):  
Yun-Yan Xia ◽  
Qiao-Gen Zou ◽  
Yu-Fei Yang ◽  
Qian Sun ◽  
Cheng-Qun Han
Keyword(s):  
Gas Chromatography ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Quantitative Detection ◽  
Dihydrogen Phosphate ◽  
Phosphate Solution ◽  
Related Impurities ◽  
Bulk Drug

Background: High-performance liquid chromatography (HPLC) method has been used to detect related impurities of perampanel. However, the detection of impurities is incomplete, and the limits of quantification and detection are high. A sensitive, reliable method is in badly to be developed and applied for impurity detection of perampanel bulk drug. Objective: Methodologies utilising HPLC and gas chromatography (GC) were established and validated for quantitative determination of perampanel and its related impurities (a total of 10 impurities including 2 genotoxic impurities). Methods: The separation was achieved on a Dikma Diamonsil C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase of 0.01 mol/L potassium dihydrogen phosphate solution (A) and acetonitrile (B) in gradient elution mode. The compound 2-bromopropane was determined on an Agilent DB-624 column (0.32 mm × 30 m, 1.8 μm) by electron capture detector (μ-ECD) with split injection ratio of 1:5 and proper gradient temperature program. Result: Both HPLC and GC methods were established and validated to be sensitive, accurate and robust according to International Council for Harmonization (ICH) guidelines. The methods developed were linear in the selected concentration range (R 2≥0.9944). The average recovery of all impurities was between 92.6% and 103.3%. The possible production mechanism of impurities during the synthesis and degradation processes of perampanel bulk drug was also discussed. Five impurities were analyzed by liquid chromatography–mass spectrometry (LC-MS). Moreover, two of them were simultaneously characterized by LC-MS, IR and NMR. Conclusion: The HPLC and GC methods were developed and optimized, which could be applied for quantitative detection of the impurities, and further stability study of perampanel.

Spectrophotometric study of the reactions of lanthanoids with bromopyrogallol red in the presence of cation active tensides

1982 ◽  
Vol 47 (2) ◽  
pp. 503-508 ◽  
Author(s):  
Irena Němcová ◽  
Pavla Plocková ◽  
Tran Hong Con
Keyword(s):  
Absorption Spectra ◽  
Photometric Determination ◽  
Spectrophotometric Study ◽  
Ternary Complexes ◽  
Optimal Conditions ◽  
Bromopyrogallol Red ◽  
Binary Complexes

The absorption spectra of the binary complexes of lanthanoids with bromopyrogallol red were measured and the formation of ternary complexes with cation active tenside, Septonex, was studied. Optimal conditions were found for the formation of these complexes and the possibility of their use in the photometric determination of lanthanoids was demonstrated on several examples.

scholarly journals Second derivative synchronous fluorescence determination of avanafil in the presence of its acid-induced degradation product aided by powerful Lean Six Sigma tools augmented with D-optimal design

RSC Advances ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 3834-3842
Author(s):  
Khalid A. M. Attia ◽  
Ahmad A. Mohamad ◽  
Mohamed S. Emara ◽  
Ahmed M. Abdel-Raoof ◽  
Mohamed A. Hasan ◽  
...  
Keyword(s):  
Optimal Design ◽  
Quantitative Determination ◽  
Degradation Product ◽  
Six Sigma ◽  
Lean Six Sigma ◽  
Synchronous Fluorescence ◽  
Second Derivative ◽  
Fluorescence Determination ◽  
Spectrofluorimetric Method

In this work, the quantitative determination of an erectile dysfunctional drug avanafil in the presence of its acid-induced degradation product was achieved via the application of a pre-optimized novel spectrofluorimetric method.

Determination of process-related impurities in N-acetylglucosamine prepared by chemical and enzymatic methods: structural elucidation and quantification

2016 ◽  
Vol 39 (7) ◽  
pp. 937-945
Author(s):  
Yi Soo Kim ◽  
Sung Joong Lee ◽  
Jin Young Choi ◽  
Yun-Hi Kim ◽  
Kebede Taye Desta ◽  
...  
Keyword(s):  
Structural Elucidation ◽  
Related Impurities ◽  
Enzymatic Methods

Simultaneous Determination of Several Elements by Spectrochemical Addition Method … (II) (Tabulation of Analytical Value)

1968 ◽  
Vol 22 (6) ◽  
pp. 749-752 ◽  
Author(s):  
Isoo Masuda ◽  
Tamon Inouye
Keyword(s):  
Simultaneous Determination ◽  
Order Approximation ◽  
Analytical Data ◽  
Zero Order ◽  
Dilution Factor ◽  
Improved Method ◽  
Addition Method ◽  
Zero Order Approximation ◽  
First Approximation

An improved method for the tabulation of analytical data, obtained by addition and successive dilution procedures for spectrochemical analysis, is presented. The author's previous work shows that the solution of the first approximation diverges at some dilution factor smaller than unity when the slope of the working curve of added series is greater than that of unadded series. By obtaining the distance between this position and the origin, and taking it as a correction factor for zero-order approximation, tabulation of the analytical value, in the case of β>α, is carried out. One parameter of the calculation is deleted by normalizing the spectral intensity; therefore, the tabulation can be simplified.

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