Method for analyzing trace levels of semi-volatile nitrosamines in solid samples
AssigneeMerck Sharp & Dohme Corp.
InventorsRebecca Evans, Xinxin Han, Daniel E. Lee, Christine L. Radich, Jinjian Zheng
Life of this patent
Estimating the term…
Abstract
This invention describes a novel method encompassing preparing a nitrosamine sample, adding in relevant chemicals that reduces or eliminates in situ nitrosamine formation, utilizing full evaporation static headspace gas chromatograph coupled with nitrogen phosphorous detector (FE-SHSGC-NPD), and analysis of rapid results in the gaseous phase for sensitive detection of semi-volatile nitrosamines, including NDMA.
Claims17
A method for analyzing nitrosamines in a pharmaceutical sample wherein in situ nitrosamine formation is reduced or eliminated comprising:
- a) heating a pharmaceutical sample suspected of containing one or more nitrosamines in the presence of one or more nitrosating inhibitors,
- b) displacing the nitrosamines from the pharmaceutical sample into a gaseous phase;
- and
- c) analyzing the nitrosamines in the gaseous phase;
- wherein the nitrosating inhibitor is selected from pyrogallol, phloroglucinol, pyrrole, 2,5-dimethylpyrrole, catechol, ascorbic acid, hydrazine, propylgallate, and gallic acid in combination with diphenylamine, or N-methyl aniline.
A method for analyzing nitrosamine analytes in pharmaceutical samples wherein in situ nitrosamine formation is reduced or eliminated, comprising:
- a) heating a pharmaceutical sample suspected of containing one or more nitrosamine analytes in the presence of one or more nitrosating inhibitors selected from the group consisting of pyrogallol, phloroglucinol, pyrrole, 2,5-dimethylpyrrole, catechol, ascorbic acid, hydrazine, propylgallate, and/or gallic acid in combination with diphenylamine, or N-methyl aniline;
- b) displacing the nitrosamine(s) analytes into a gaseous phase;
- and
- c) analyzing the nitrosamine analytes.
Dependencies are inferred from the claim text.