Determination of Migration Levels of N-Nitrosamines and N-Nitrosatable Substances from Balloons by Gas Chromatography-Positive Chemical Ionization Mass Spectrometry
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Journal Article Gas Chromatography and Selective Detection of N-Nitrosamines Get access John W. Rhoades, John W. Rhoades Search for other works by this author on: Oxford Academic PubMed Google Scholar Donald E. Johnson Donald E. Johnson Southwest Research Institute, 8500 Culebra Road, San Antonio, Texas 78228 Search for other works by this author on: Oxford Academic PubMed Google Scholar Journal of Chromatographic Science, Volume 8, Issue 10, October 1970, Pages 616–617, https://doi.org/10.1093/chromsci/8.10.616 Published: 01 October 1970 Article history Received: 19 March 1970 Published: 01 October 1970
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A mass spectrometric method for quantitative determination of volatile N-nitrosamines, based on analysis of the derivatives formed from secondary amines produced by denitrosation of N-nitrosamines when they are reacted with 7-chlor-4-nitrobenzo-2-oxa-1,3-diazole, is proposed. The method has been applied to the quantitative analysis of 3-4 component mixtures of N-nitrosamines without preliminary separation. The detection limit was 1 ng with a relative standard deviation of 0.13–0.25. A gas chromatographic mass spectrometric method for the identification and quantification of multicomponent mixtures of N-nitrosamines was also developed with a detection limit of 1 ng μ1−1 and relative standard deviation of 0.11–0.22. These methods are recommended for N-nitrosamine determination in environmental samples and have the advantage that the standards can be prepared not from carcinogenic N-nitrosamines, but directly from the respective secondary amines.
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Reaction of 1-dimethylaminonaphthalene-5-sulphonyl chloride with the secondary amines produced by denitrosation of N-nitrosamines yields dansyl-amides suitable for the mass spectrometric determination of N-nitrosamines. The method has been applied to the quantitative analysis of 3-4 component mixtures of N-nitrosamines. The detection limit was 1 ng with a relative standard deviation of 0.15-0.31. A gas chromatographic mass spectrometric method for the identification and quantification of mixtures of N-nitrosamines was also developed with a detection limit of 1 ng μl−1 and relative standard deviation of 0.12-0.23. These methods are recommended for N-nitrosamine determination in environmental samples and have the advantage that the internal standard can be prepared directly from the respective secondary amine.
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ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTSemiquantitative analysis of low levels of volatile nitrosamines by gas chromatography-mass spectrometryThomas A. Bryce and Geoffrey M. TellingCite this: J. Agric. Food Chem. 1972, 20, 4, 910–911Publication Date (Print):July 1, 1972Publication History Published online1 May 2002Published inissue 1 July 1972https://pubs.acs.org/doi/10.1021/jf60182a031https://doi.org/10.1021/jf60182a031research-articleACS PublicationsRequest reuse permissionsArticle Views67Altmetric-Citations11LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InRedditEmail Other access optionsGet e-Alertsclose Get e-Alerts
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A method for rapid quantitative determination of N‐nitrosamines (N‐dimethylnitrosamine NDMA, N‐diethylnitrosamine NDEA, N‐dipropylnitrosamine NDPA, N‐dibutylnitrosamine NDBA) in pesticide samples was set up using the gas chromatographic‐mass spectrometric (GC‐MS) technique in the electron impact (EI) mode. SIR, with deuterium labelled NDPA as a standard, was used for detection and quantification. Calculations were made on the basis of calibration curves, obtained by injecting different amounts of nitrosamines against a fixed concentration of deuterated NDPA, with a good linearity. We analysed several batches of trifluralin samples [2,6‐dinitro‐N, N‐dipropyl‐4‐(trifluoromethyl) benzenamine], before and after purification steps. The sensitivity achieved by this method is lower than 2 ppb. This method can be easily used to detect N‐nitrosamine impurities in other pesticides, such as amides, carbamates, organophosphates, triazines, urea derivatives, other dinitroaniline‐type and miscellaneous nitrogen‐containing compounds.
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