PubMed · 13102409
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W MERKEL. 1953. [Hypercodin, new cough drug].. https://pubmed.ncbi.nlm.nih.gov/13102409/
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Dextromethorphan, the innocuous non-narcotic antitussive agent, is the most widely used probe drug to assess CYP2D6 function both in vivo and in vitro. For this reason a simple and selective high performance liquid chromatography method with fluorimetric detection for simultaneous quantitation of dextromethorphan, and its main metabolites in human plasma was developed and validated. The method involved a simple and rapid protein precipitation protocol, using a mixture of ZnSO(4) and methanol. The analysis was performed on a 3 microm, C(18) Tracer Excel 15 cm x 0.4 cm i.d. column by gradient elution in which Mobile phase A consisted of potassium dihydrogen phosphate buffer (pH = 3, 0.01 M):methanol:tetrahydrofuran (68.5:31:0.5), and mobile phase B consisted of methanol:tetrahydrofuran (93.25:6.75). Linear calibration curves were obtained in the range of 10-500 ng/ml for dextromethorphan, dextrorphan and hydroxymorphinan. The limit of quantitation (LOQ) was 10 ng/ml for each compound. The maximum within and between days precisions were 7.4 and 7.8%, respectively. The accuracies at four different concentration levels ranged from 88.2 to 111.5%. The recoveries were between 88.0 and 108.6%. The assay method was successfully applied to determine dextromethorphan metabolic ratio after an oral dose of 30 mg of dextromethorphan hydrobromide.
Two potential oxidation degradants of oxymetazoline have been isolated by liquid chromatography and monitored by electrospray single quadrupole mass spectrometry. The structures of the products are shown to be oxymetazoline N-oxide and hydroxyamine by multiple-stage fragmentation ion trap mass spectrometry. The product ion spectra were installed in a library database and the library was used to examine an aged commercial product; one of the degradants was detected, but at a level of less than 0.1% of the parent.