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Joint International Conference on Long-term Experiments ...

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DETERMINATION OF NITROGEN-CONTAINING POLYNUCLEAR AROMATIC<br />

HYDROCARBONS IN SMOKED FOODS BY LIQUID CHROMATOGRAPHY<br />

Lucian Bara<br />

University of Oradea, Faculty of Envir<strong>on</strong>mental Protecti<strong>on</strong><br />

26, General Magheru Street, Oradea<br />

ABSTRACT<br />

Several smoked foods were analyzed for basic nitrogen-c<strong>on</strong>taining polynuclear aromatic<br />

hydrocarb<strong>on</strong> (NPAH) c<strong>on</strong>tent by a relatively rapid liquid chromatographic (LC) technique.<br />

The analyzed products included both domestic and imported market basket commodities.<br />

Nanogram quantities of NPAH standards were detected by UV and fluorescence detectors<br />

c<strong>on</strong>nected in series. The NPAHs were extracted from basic aqueous ethanolic soluti<strong>on</strong> into<br />

cyclohexane, extracted from cyclohexane into 6N HCl, and extracted back into cyclohexane<br />

after neutralizati<strong>on</strong> of the acid.<br />

The NPAHs were then purified by filtering the extract through deactivated basic<br />

alumina. The eluate from this step was c<strong>on</strong>centrated to dryness, and the residue was<br />

dissolved in 95% ethanol and analyzed by LC, using a Vydac C-18 column and acet<strong>on</strong>itrilewater<br />

(9 + 1) as the mobile phase. Recoveries of 3 NPAHs, 5,7-dimethylbenz acridine,<br />

dibenz acridine, and dibenz acridine, each added to salm<strong>on</strong> and sausage at the 5 ppb level,<br />

ranged from 62 to 101% by fluorescence measurement and from 64 to 106% by UV<br />

measurement. N<strong>on</strong>e of the NPAHs used, as standards were found by either fluorescence or<br />

UV detecti<strong>on</strong> at levels greater than or equal to 5 ppb in any of the foods analyzed.<br />

INTRODUCTION<br />

Interest in the producti<strong>on</strong> of petroleum substitutes from shale oil and coal has increased. The<br />

increasing use of coal and synthetic fuels may significantly increase the levels of<br />

heterocyclic nitrogen compounds in the envir<strong>on</strong>ment because of the charasterically higher<br />

level of organic nitrogen in coal and its by-products, compared to other fossil fuels. Many<br />

nitrogen bases, thought to be products of incomplete combusti<strong>on</strong> of organic matter that<br />

c<strong>on</strong>tains nitrogen or to be derived from hydrolytic processes similar to those producing<br />

polynuclear aromatic hydrocarb<strong>on</strong>s, have been shown by various types of skin tests to be<br />

toxic, carcinogenic, and mutagenic to terrestrial and aquatic organisms.<br />

Many azaarenes have been identified in sources such as tobacco, automobile exhaust,<br />

high boiling petroleum distillates, crude oil, shale oil, and lake sediments.<br />

The purpose of our investigati<strong>on</strong> was to develop an analytical method for the<br />

extracti<strong>on</strong>, cleanup, and LC analysis of the basic NPAH fracti<strong>on</strong>s obtained from some<br />

smoked foods. The foods analyzed included both domestic and imported products.<br />

528

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