scholarly journals High-performance Enantiomer Separation of Nonsteroidal Anti-inflammatory Drugs (NSAIDs) by 3 ^|^mu;m Reversed-phase Chiral Columns and Application to the Optical Purity Testing of Naproxen Drug Substances and Its Formulations

2014 ◽  
Vol 30 (3) ◽  
pp. 397-406
Author(s):  
Moe TANAKA ◽  
Kumi NAGAMATSU ◽  
Hiroyuki NISHI
Keyword(s):  
High Performance ◽  
Enantiomer Separation ◽  
Optical Purity ◽  
Reversed Phase ◽  
Drug Substances ◽  
Purity Testing ◽  
Inflammatory Drugs ◽  
Anti Inflammatory ◽  
Optical Purity Testing

scholarly journals Identification of benzydamine and its metabolit in the presence of certain anti-inflammatory non-steroidal drugs

2021 ◽  
pp. 43-50
Author(s):  
Olga Chorna ◽  
Vasyl Chornyi ◽  
Oleksandr Сhubenko ◽  
Ihor Hrubnyk ◽  
Volodymyr Mishchenko
Keyword(s):  
Biological Material ◽  
High Performance ◽  
Screening Method ◽  
Subsequent Development ◽  
Reference Method ◽  
Pharmacological Action ◽  
Reversed Phase ◽  
Routine Identification ◽  
Inflammatory Drugs ◽  
Anti Inflammatory

The aim of the work. Currently, a large number of cases of non-medical use of benzydamine hydrochloride have been described. The identification of benzydamine and its metabolite, benzydamine N-oxide, in the presence of some non-steroidal anti-inflammatory drugs, has been insufficiently studied. Therefore, the development of a method for its identification in biological material is an urgent task. Materials and methods. The subjects of the study were benzydamine hydrochloride and its metabolite, as well as some non-steroidal anti-inflammatory drugs, which are its analogues in terms of pharmacological action. The studies were carried out by methods of thin layer chromatography and high-performance liquid chromatography. Results. At the first stage a screening method for benzydamine identification was studied using the extraction in acidic and basic conditions. It was shown that benzydamine can be isolated in both medias with subsequent development with a solution of iodoplatinate and Dragendorff's reagent according to Munier or with Mandelin reagent respectively. The mobile phase was selected and respective hRf for the target molecule were defined. After a preliminary identification of benzydamine a reference method for the final confirmation of the drug that had led to poisoning was proposed. A robust, specific and accurate reversed phase HPLC method was chosen. It was shown that benzydamine exists in biological material mainly in a form of metabolite – benzydamine N-oxide. The selected method was able to separate and determine key analytes in biological samples after a preparative isolation by TLC method. The comparison with UV spectra of the reference standard of benzydamine hydrochloride was proposed to avoid false positive conclusion of drug identification. Conclusions. Proposed methodology can be applied for routine identification of benzydamine poisoning in toxicological laboratories

scholarly journals Degradation of Benzo[a]pyrene by Mycobacterium vanbaalenii PYR-1

2004 ◽  
Vol 70 (1) ◽  
pp. 340-345 ◽  
Author(s):  
Joanna D. Moody ◽  
James P. Freeman ◽  
Peter P. Fu ◽  
Carl E. Cerniglia
Keyword(s):  
High Performance ◽  
Culture Media ◽  
Optical Purity ◽  
Fission Products ◽  
Reversed Phase ◽  
Environmental Pollutant ◽  
Ring Fission ◽  
Uv Visible ◽  
Derivatives Of ◽  
Absolute Stereochemistry

ABSTRACT Metabolism of the environmental pollutant benzo[a]pyrene in the bacterium Mycobacterium vanbaalenii PYR-1 was examined. This organism initially oxidized benzo[a]pyrene with dioxygenases and monooxygenases at C-4,5, C-9,10, and C-11,12. The metabolites were separated by reversed-phase high-performance liquid chromatography (HPLC) and characterized by UV-visible, mass, nuclear magnetic resonance, and circular dichroism spectral analyses. The major intermediates of benzo[a]pyrene metabolism that had accumulated in the culture media after 96 h of incubation were cis-4,5-dihydro-4,5-dihydroxybenzo[a]pyrene (benzo[a]pyrene cis-4,5-dihydrodiol), cis-11,12-dihydro-11,12-dihydroxybenzo[a]pyrene (benzo[a]pyrene cis-11,12-dihydrodiol), trans-11,12-dihydro-11,12-dihydroxybenzo[a]pyrene (benzo[a]pyrene trans-11,12-dihydrodiol), 10-oxabenzo[def]chrysen-9-one, and hydroxymethoxy and dimethoxy derivatives of benzo[a]pyrene. The ortho-ring fission products 4-formylchrysene-5-carboxylic acid and 4,5-chrysene-dicarboxylic acid and a monocarboxylated chrysene product were formed when replacement culture experiments were conducted with benzo[a]pyrene cis-4,5-dihydrodiol. Chiral stationary-phase HPLC analysis of the dihydrodiols indicated that benzo[a]pyrene cis-4,5-dihydrodiol had 30% 4S,5R and 70% 4R,5S absolute stereochemistry. Benzo[a]pyrene cis-11,12-dihydrodiol adopted an 11S,12R conformation with 100% optical purity. The enantiomeric composition of benzo[a]pyrene trans-11,12-dihydrodiol was an equal mixture of 11S,12S and 11R,12R molecules. The results of this study, in conjunction with those of previously reported studies, extend the pathways proposed for the bacterial metabolism of benzo[a]pyrene. Our study also provides evidence of the stereo- and regioselectivity of the oxygenases that catalyze the metabolism of benzo[a]pyrene in M. vanbaalenii PYR-1.

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