Isolation of volatile N-nitrosamines in edible vegetable oils and cooked bacon fat.
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Cooking↗
Biomedical subjects
D C Havery
Publications and source records attributed to D C Havery.
Volatile N-nitrosamines in Polish malt and beer.
A survey of Polish malt and beer for volatile N-nitrosamines has been conducted. N-Nitrosodimethylamine was found in malt at levels ranging from 0.2 to 3.6 micrograms/kg (average 1.5 micrograms/kg) and in beer at levels up to 0.3 microgram/kg (average 0.2 micrograms/kg). The use of indirect malt dryers is credited with the low levels of N-nitrosamines found.
Beer↗
Determination of N-nitroso compounds by high-performance liquid chromatography with postcolumn reaction and a thermal energy analyzer.
Carcinogenic nonvolatile N-nitroso compounds have been difficult to determine in foods and other consumer products because of the incompatibility of aqueous high-performance liquid chromatography (HPLC) mobile phases with the thermal energy analyzer (TEA), a sensitive and selective detector for N-nitroso compounds. A postcolumn technique has been developed that permits the use of aqueous mobile phases with an interfaced liquid chromatograph/TEA. This system was linear from 3.5 to 900 ng of N-nitrosoproline injected. Coefficients of variation of 3.0 and 5.1%, respectively, were obtained when N-nitrosoproline and N-nitrosotrimethylurea were repeatedly injected at the 80- to 90-ng level. Mixtures of volatile and nonvolatile N-nitroso compounds as well as N-nitrosodipeptides were separated and quantitated by HPLC/TEA with a water/acetonitrile gradient.
Chemistry Techniques, Analytical↗
Occurrence of 1,4-dioxane in cosmetic raw materials and finished cosmetic products.
Surveys of cosmetic raw materials and finished products for the presence of the carcinogen 1,4-dioxane have been conducted by the U.S. Food and Drug Administration since 1979. Analytical methods are described for the determination of 1,4-dioxane in ethoxylated cosmetic raw materials and cosmetic finished products. 1,4-Dioxane was isolated by azeotropic atmospheric distillation and determined by gas chromatography using n-butanol as an internal standard. A solid-phase extraction procedure based on a previously published method for the determination of 1,4-dioxane in cosmetic finished products was also used. 1,4-Dioxane was found in ethoxylated raw materials at levels up to 1410 ppm, and at levels up to 279 ppm in cosmetic finished products. Levels of 1,4-dioxane in excess of 85 ppm in children's shampoos indicate that continued monitoring of raw materials and finished products is warranted.
1-Butanol↗
Ethyl carbamate levels in selected fermented foods and beverages.
Ethyl carbamate (EC), also known as urethane, is an animal carcinogen and a by-product of fermentation. Because EC has been found in distilled spirits and wines, a variety of fermented foods and beverages were analyzed to assess its occurrence in other products. Previously described methods using a gas chromatograph-thermal energy analyzer with a nitrogen converter were modified for each matrix and gave recoveries of greater than 80%, with a limit of detection in the 1-2 micrograms/kg (ppb) range. A total of 152 test samples were analyzed; EC levels ranged from none found to 3 ppb in 15 cheeses, 6 teas, 12 yogurts, and 8 ciders; from none found to 13 ppb in 30 breads and 69 malt beverages; and from none found to 84 ppb in 12 soy sauces. Gas chromatography/mass spectrometry/mass spectrometry was used to confirm EC identity and to quantitate EC in selected food extracts.
Alcoholic Beverages↗
Rapid gas chromatographic method for determining ethyl carbamate in alcoholic beverages with thermal energy analyzer detection.
A rapid column elution method has been developed for the determination of ethyl carbamate (EC) in alcoholic beverages. The beverage is mixed with Celite and packed in a column containing deactivated alumina capped with a layer of sodium sulfate. EC is then eluted with methylene chloride. The method, using a gas chromatograph-thermal energy analyzer with a nitrogen converter for detection and quantitation of EC, has been applied to a variety of alcoholic beverages. Recoveries +/- standard deviations of EC in wine and whisky fortified at the 20 and 133 micrograms/kg (ppb) levels averaged 87.3 +/- 5.3 and 88.7 +/- 3.6%, respectively. The method has a limit of detection of 1.5 ppb. Gas chromatography/mass spectrometry/mass spectrometry was used to confirm the identity and quantitation of EC in selected beverage extracts.
Alcoholic Beverages↗
Current trends in levels of volatile N-nitrosamines in fried bacon and fried-out bacon fat.
Commercially processed bacon samples purchased from the Washington, DC, retail market have been periodically analyzed since 1971 for the presence of volatile N-nitrosamines in the fried product. During that time, a downward trend in the concentration of N-nitrosopyrrolidine has been observed, and between 1978 and 1980 it plateaued at 4-30 ppb, with an average of 11 ppb. A recent survey, however, indicates a change in this downward trend, with N-nitrosopyrrolidine found at levels ranging from 1 to 65 ppb, average 21 ppb. Volatile N-nitrosamines were found at levels up to 110 ppb in the fried product and up to 85 ppb in the fried-out bacon fat.
Animals↗
Rapid column method for determination of N-nitrosodimethylamine in malt.
A rapid column elution method has been developed for the determination of N-nitrosodimethylamine (NDMA) in malt. The average recovery of NDMA added to malt at the 10 ppb level was 87%. When a single malt sample was analyzed 10 times, the NDMA found averaged 8.1 ppb with a coefficient of variation of 3.93%. In a study of 15 malt samples, data obtained by the column elution method were in good agreement with those from a vacuum distillation method.
Chromatography↗
Determination of musk ambrette in fragrance products by capillary gas chromatography with electron capture detection: interlaboratory study.
A gas chromatographic method that uses an internal standard additions techniques is described for the determination of musck ambrette (MA) in fragrance products. A solution containing the product and a known amount of an internal standard, musk tibetene (MT), is injected directly into a gas chromatograph equipped with an electron capture detector. The chromatographic separation of the components on a wide-bore fused silica capillary column is recorded and a response constant is calculated from MA and MT peak heights. A similar response constant is also calculated for a standard solution containing known concentrations of MA and MT. The MA content of the fragrance product is then calculated. Average recoveries of MA from fragrance products ranged from 97.6 to 102.3%. The method was also evaluated collaboratively by 6 laboratories. In this study, the reproducibility relative standard deviation for MA in 6 fragrance test samples ranged from 2.78 to 22.87%.
Chromatography, Gas↗
Determination of 2-ethylhexyl 4-(N-methyl-N-nitrosamino) benzoate in commercial sunscreens and cosmetic products.
An analytical method has been developed for determination of 2-ethylhexyl 4-(N-methyl-N-nitrosamino) benzoate (NMPABAO), a nitrosamine contaminant in sunscreen products containing 2-ethylhexyl 4-(N,N-dimethylamino) benzoate (Padimate O). The method involves extraction of NMPABAO by column chromatography followed by liquid chromatographic separation and analysis wit a nitric oxide detector. To confirm the presence of NMPABAO in sunscreen products, the N-nitrosamine was synthesized and its structure was determined by infrared spectrophotometry, nuclear magnetic resonance spectrometry, and mass spectrometry (MS). For method validation, recovery studies were performed on a commercial suntan lotion, cream, and gel. Recoveries of NMPABAO added to representative test samples averaged 83%. The method has an estimated detection limit of 30 ppb. The method was used to analyze 25 commercial cosmetic and sunscreen products containing Padimate O. Eleven products contained NMPABAO at levels ranging from 160 to 21000 ppb. NMPABAO presence in 4 products was confirmed by MS at levels > or = 4000 ppb. The highest levels of NMPABAO were associated with products that contained the nitrite-releasing preservative 2-bromo-2-nitro-1,3-propanediol.
Carcinogens↗