222 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS (18) (19) (20) (21) (22) mination of nitrite and nitrosamines in cosmetic raw materials and finished products, J. Soc. Cosmet. Chem., 30, 127-135 (1979). I. E. Rosenberg, J. Gross, and T. Spears, Analysis of nitrosamines in cosmetic raw materials and finished product by high pressure liquid chromatography,J. Soc. Cosmet. Chem., 31,237-252 (1980). I. E. Rosenberg, J. Gross, and T. Spears, Analysis of N-nitrosodiethanolamine in linoleamide DEA by high pressure liquid chromatography and UV detection, J. Soc. Cosmet. Chem., 31, 323-327 (1980). W. Mitchell and P. Rahn, High performance liquid chromatography in cosmetic analysis, Drug Cosmet. Ind., 123 (5), 56-66, 126, 130 (November 1978). J. L. Ho, H. H. Wisneski, and R. L. Yates, High pressure liquid chromatographic-thermal energy determination of N-nitrosodiethanolamine in cosmetics, J. Assoc. Off. Anal. Chem., 64 (4), 800-804 (1981). W. Fiddler, R. C. Doerr, and E. G. Piotrowski, "Observations on the Use of the Thermal Energy Analyzer as a Specific Detector for Nitrosamines," in Environmental Aspects of N-Nitroso Compounds, E. Walker, L. Griciute, M. Castegnaro, and R. E. Lyle, Eds., IARC Scientific Publication No. 19 (International Agency for Research on Cancer, Lyon, France, 1978), pp 33-39.

.]. Soc. Cosmet. Chem., 36, 223-230 (May/June 1985) Determination of N-nitrosodiethanolamine (NDELA) in cosmetic ingredients MITCHELL D. ERICKSON, DUANE B. LAKINGS, ARBOR D. DRINKWINE, and JAMES L. SPIGARELLI, Midwest Research Institute, 425 Volker Boulevard, Kansas City, MO 64110. Received December 1 O, 1984. Presented in part at the Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy, Atlantic City, N J, March 10-14, 1980. Synopsis Methods for the extraction and cleanup of several cosmetic ingredient matrices are presented. Diethanoi- amine and triethanolamine matrices were diluted with ethyl acetate and dried with sodium sulfate. Amphoteric and quaternium matrices were slurried with silica gel and methanol and then evaporated to dryness. The dried sample was then transferred to a silica gel column and eluted with acetone/methylene chloride (60/40). Morpholine matrices were diluted with methanol/methylene chloride (2/98). All samples were analyzed by high performance liquid chromatography-thermal energy analyzer. Recovery corrections for losses during extraction and cleanup were based on the recovery of •4C-N-nitrosodiethanolamine mea- sured by scintillation counting. The methods were validated, showing an accuracy of 99% and a precision of + 22% over a range of about 50-1,000 ng/g. Detection limits are estimated to be below 50 ng/g for all matrices studied. INTRODUCTION N-Nitrosamines have long been recognized as a group of hazardous compounds about 80% of those tested have been found to be carcinogenic to test animals (1-4). Their carcinogenicity, mutagenicity, health effects, environmental presence, and occurrence in commercial products have been reviewed (1-11). In 1977, it was reported that N- nitrosodiethanolamine (NDELA) had been found in cutting fluids (12), tobacco (13), cosmetics (14), lotions (14), and shampoos (14). Subsequently, NDELA was shown to be a carcinogen in the rat (15). Since these reports, scientists in industry and govern- ment have been working to develop and improve upon analytical methods for detecting NDELA (16). NDELA can be formed in cosmetics or their ingredients as a reaction product of alkanolamines such as triethanolamine, alkanolamides, and other amino compounds used in cosmetic formulations with a nitrosating agent, possibly 2-bromo- 2-nitro- 1,3-propanediol ( 17, 18). Since prevention of human exposure to NDELA is of paramount interest, determination of NDELA in cosmetics and their ingredients is necessary for adequate consumer pro- tection. Although the procedure used by Fan et al. (14) in the original work was apparently adequate for certain matrices, it has been reported (18) to be unreliable, especially with aqueous matrices. 223