Gas chromatographic-mass spectrometric analysis of volatiles in flavors and biological fluids

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1971

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Abstract

The volatile flavor components of two types of Cheddar cheese and a Cheddar cheese powder have been analyzed by gas-liquid chromatography and mass spectrometry. Techniques applied to prepare samples for analysis were the following: centrifugation of cheese with subsequent direct injection of the oil obtained, low temperature, vacuum distillations of cheese oil and whole cheese, and extraction of the oil with methanol. The compounds identified include ketones, aldehydes, alcohols, acids, esters, lactones, terpenes, alkanes, alkenes, alkyl benzenes, and some chlorinated compounds. A technique is described in which the oil obtained by centrifugation of cheese at room temperature is injected directly into the gas chromatograph in order to compare the volatile flavor components of several types of cheese. Chromatograms are shown for Roquefort, Blue, Romano, Limburger, and Cheddar cheeses. The method requires only 1 to 3 g of cheese and gives semiquantitative data. Roquefort cheese has the highest concentration of flavor compounds with ca. 110 ppm for 2-heptanone, whereas the most concentrated volatile components in Cheddar cheese do not exceed concentrations of 10 ppm. The volatile components of roast beef and roast beef drippings have been analyzed by gas-liquid chromatography (GLC) and mass spectrometry (MS). Samples were prepared by low temperature, vacuum distillation of meat and drippings followed by extraction of the distillates with diethyl ether. Major volatile components are alkanals, alk-2-enals and alka-2,4-dienals. In addition to these compounds the meat samples show high concentrations of 3-hydroxy-2-butanone and y-butyrolactone. Further classes of constituents are 2-n-alkylfurans, 2-alkanones, 3-alkanones, 2,3-alkadiones, pyrazines, primary and secondary alcohols, acids, y- and 6-lactones, alkanes, aromatic compounds, sulfur compounds and acetyl pyrrole. By comparing the lean meat portion and the fat portion of roast beef it was found that the fat is the prime site of the aldehydes. Finally, volatile urinary components from human urine were analyzed using ether-continuous liquid-liquid extractions and gas-liquid chromatography plus gas chromatography and mass spectrometry. Chromatograms from different subjects showed remarkable similarities. Pathological states could possibly be reflected by changes in these chromatographic patterns.

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