GRISEOVIRIDIN: THE C6 FRAGMENT

1960 ◽  
Vol 38 (6) ◽  
pp. 950-957 ◽  
Author(s):  
P. De Mayo ◽  
A. Stoessl
Keyword(s):  
Degradation Product ◽  
Hydrolytic Degradation ◽  
Sulphur Atom ◽  
Structural Environment ◽  
Part Structure

The structure of a hydrolytic degradation product from griseoviridin, isolated as the 2,4-dinitrophenylhydrazone, has been shown, by synthesis, to be IV. A by-product of the synthesis was the stereoisomeric 2,4-dinitrophenylhydrazone. This establishes IX as a part structure of griseoviridin. Evidence is provided that the previously proposed structural environment of the sulphur atom is incorrect, and that the sulphur may, in fact, be attached to the C6 fragment.

Simultaneous Determination of Floctafenine and its Hydrolytic Degradation Product Floctafenic Acid Using Micellar Liquid Chromatography with Applications to Tablets and Human Plasma

2013 ◽  
Vol 96 (6) ◽  
pp. 1315-1324 ◽  
Author(s):  
Mohamed I Walash ◽  
Fathalla Belal ◽  
Nahed El-Enany ◽  
Manal Eid ◽  
Rania N El-Shaheny
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Degradation Product ◽  
Mobile Phase ◽  
Sodium Dodecyl ◽  
Hydrolytic Degradation ◽  
Direct Determination ◽  
Micellar Liquid Chromatography ◽  
Main Metabolite

Abstract A stability-indicating micellar liquid chromatography (MLC) method was developed and validated for the assay of floctafenine (FLF) in the presence of its degradation product and main metabolite, floctafenic acid (FLA). The analysis was carried out on a CLC Shim-Pack octyl silane (C8) column (150 × 4.6 mm id, 5 μm particle size) using a micellar mobile phase consisting of 0.15 M sodium dodecyl sulfate, 10% n-propanol, and 0.3% triethylamine in 0.02 M orthophosphoric acid (pH = 3). The mobile phase was pumped at a flow rate of 1.0 mL/min with UV detection at 360 nm. The method showed good linearity for FLF and FLA over the concentration ranges of 0.5–25.0 and 0.4–10.0 μg/mL, with LODs of 0.16 and 0.12 μg/mL, respectively. The developed method was successfully applied to the determination of FLF in commercial dispersible tablets, with mean recovery of 98.87 ± 1.37%. Also, the proposed method was specific for the analysis of FLF in presence of the co-formulated drug thiocolchicoside in laboratory-prepared tablets, with mean recovery of 100.50 ± 1.07%. Statistical comparison of the results obtained by the proposed MLC method with those obtained by a comparison method showed good agreement. Moreover, the method was extended to study the degradation behavior of FLF under different International Conference on Harmonization recommended conditions such as alkaline, acidic, oxidative, thermal, and photolytic. The method was further applied for direct determination of FLA as the main metabolite of FLF in human plasma without prior extraction steps, with mean recovery of 110.50 ± 6.5%.

scholarly journals Studying Microwave-Assisted Hydrolytic Degradation of Colchicine using RP-Chromatographic Methods: In Silico ADME/Tox Profile and Molecular Docking

2019 ◽  
Author(s):  
nada abdelwahab ◽  
hossam mokhtar ◽  
asmaa aboulmaged
Keyword(s):  
Degradation Product ◽  
In Silico ◽  
Oral Absorption ◽  
Hydrolytic Degradation ◽  
High Sensitivity ◽  
Flash Chromatography ◽  
Stability Indicating ◽  
Microwave Assisted ◽  
Chromatographic Methods ◽  
Validation Parameters

Abstract Colchicine, is a natural amide containing anti-gout treatment with versatile applications. Microwave assisted hydrolytic degradation is a newly alternative method thought to be more promising than traditional procedures of heating. It is an ecofriendly method that has more reproducible results due to the control of parameters. From this point, carrying on hydrolytic degradation of colchicine was tested for the first time under acidic conditions with the aided of microwave. The drug was hydrolyzed with the formation of deacylated analogue. Isolation of the resulted degradate was carried out using flash chromatography, the isolated one was elucidated based on 1 H NMR data. Moreover, the results of human pharmacokinetic predictions conducted from in silico data showed that colchicine had higher blood brain barrier (BBB), plasma protein binding, and oral absorption than its deacylated derivative. The study was also extended to forecast the binding of colchicine and its degradate to the target protein. Furthermore, two stability indicating chromatographic methods were developed for quantification of the drug and its degradation product with high sensitivity. The first method was RP-TLC densitometric method that based on using a solvent mixture of water: methanol: diethylamine (70: 30: 15, by volume). The second one was RP-HPLC at which a mixture of water (containing 0.02% diethyl amine): methanol: acetonitrile (50: 20: 30, by volume) was the used mobile phase. Validation parameters were calculated according to ICH recommendations and all were within the acceptable limits. These methods were used for determination of colchicine in its available tablets. They are the first developed stability indicating methods for analysis of colchicine and its degradation product.

Further Studies on the Colorimetric Determination of Ronidazole in Feeds

1978 ◽  
Vol 61 (6) ◽  
pp. 1523-1526
Author(s):  
David W Fink ◽  
James V Pivnichny ◽  
Jung-Sook K Shim ◽  
John W Tolan
Keyword(s):  
Sample Preparation ◽  
Degradation Product ◽  
Colorimetric Method ◽  
Hydrolytic Degradation ◽  
Colorimetric Determination ◽  
Analytical Technique ◽  
Per Se ◽  
The Stability ◽  
Medicated Feeds

Abstract A previously published colorimetric method for determining ronidazole, (l-methyl-5-nitroimidazoI- 2-yl) methyl carbamate, can be used as an analytical technique for measuring the stability of this drug in medicated feeds. Although the color reaction per se is not selective, elution profiles of ronidazole and its demonstrated hydrolytic degradation product, l-methyl-2-hydroxymethyl- 5-nitroimidazoIe, show that the chromatographic separation used in the sample preparation efficiently isolates the drug from the degradation product. No interference was found in feeds containing 0.010% ronidazole and up to 0.010% degradation product.

Synthesis of 3-hydroxy-3-(hydroxymethyl)-5-methylcyclohexane-1,2-dione dibenzoate, a reported hydrolytic degradation product of leucogenenol

1984 ◽  
Vol 49 (13) ◽  
pp. 2429-2433 ◽  
Author(s):  
D. John Aberhart ◽  
Jon Clardy ◽  
Pallab K. Ghoshal ◽  
He Cunheng ◽  
Qitai Zheng
Keyword(s):  
Degradation Product ◽  
Hydrolytic Degradation

HPLC analysis of a syrup containing nimesulide and its hydrolytic degradation product

2010 ◽  
Vol 64 (3) ◽  
Author(s):  
Milan Mokrý ◽  
Jiří Klimeš ◽  
Jana Pechová
Keyword(s):  
Degradation Product ◽  
Hplc Analysis ◽  
Pharmaceutical Preparation ◽  
Hydrolytic Degradation ◽  
Ammonium Phosphate ◽  
Reversed Phase ◽  
Pharmaceutical Formulation ◽  
Uv Detection ◽  
Hydroxybenzoic Acid

AbstractThe present paper deals with the evaluation of nimesulide, 2-phenoxy-4-nitroaniline, the main hydrolytic degradation product of nimesulide, of methylparaben and propylparaben, and eventually of 4-hydroxybenzoic acid by HPLC with UV detection at 254 nm in syrup as a pharmaceutical formulation. HPLC analysis was employed on the reversed phase C18 with methanol and 0.01 M dibasic ammonium phosphate (ρ r = 60: 40, pH 4.0). Validation was performed using standards and a pharmaceutical preparation containing the compounds described above.

Identification, isolation, structural characterisation, synthesis and in silico toxicity prediction of the alkaline hydrolytic degradation product of brivaracetam by using LC-PDA, preparative HPLC, LC/HESI/LTQ, FTIR, and 1H NMR

2020 ◽  
Vol 12 (14) ◽  
pp. 1868-1881
Author(s):  
Pankaj Bhamare ◽  
P. Umadoss ◽  
Neeraj Upmanyu ◽  
Rupal Dubey
Keyword(s):  
1H Nmr ◽  
Degradation Product ◽  
In Silico ◽  
Hydrolytic Degradation ◽  
Preparative Hplc ◽  
Limited Data ◽  
Toxicity Prediction ◽  
Degradation Behaviour ◽  
Structural Characterisation ◽  
In Silico Toxicity

Brivaracetam is a racetam derivative of levetiracetam with very limited data available on its degradation behaviour.

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