High pressure liquid chromatographic-thermal energy determination of N-nitrosodiethanolamine in cosmetics

• Published in: Journal of the Association of Official Analytical Chemists Vol. 64; no. 4; p. 800
• Main Authors: Ho, J L, Wisneski, H H, Yates, R L
• Format: Journal Article
• Language: English
• Published: United States 01.07.1981
• Subjects: Carcinogens - analysis; Chromatography, High Pressure Liquid - methods; Cosmetics - analysis; Diethylnitrosamine - analogs & derivatives; Diethylnitrosamine - analysis; Gas Chromatography-Mass Spectrometry - methods; Nitrosamines - analysis; Spectrophotometry, Ultraviolet - methods; Thermodynamics
• ISSN: 0004-5756
• DOI: 10.1093/jaoac/64.4.800

Methods for the determination and confirmation of N-nitrosodiethanolamine (NDELA) in cosmetic products were developed. The NDELA fraction was isolated from a cosmetic product by a series of solvent extractions which were designed to concentrate the NDELA and remove ingredients deleterious to the analytical system. The isolated fraction was then analyzed for NDELA using a high pressure liquid chromatograph (HPLC) interfaced with a thermal energy analyzer (TEA). The compound was measured by comparison of detector response with those of known standards. NDELA was verified by gas chromatography-mass spectrometry of the silyl derivative after preliminary cleanup of the sample by gradient elution HPLC on a Partisil 10 PAC column. The limit of detection of NDELA by TEA is 2-3 ng, which corresponds to 20-30 ppb in the cosmetic product. Analysis of an emulsion cream and a hair grooming gel spiked at 3 and 4 ng concentration levels, respectively, yielded recoveries ranging from 71 to 103% (average 88%).