Analysis of Volatile Compounds in Beef Fat by Dynamic‐Headspace Solid‐Phase Microextraction Combined with Gas Chromatography–Mass Spectrometry

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ABSTRACT:  A solid‐phase microextraction (SPME) technique has been applied to the determination of the volatile compounds, including diterpenoids and lactones, in cooked beef fat. The ability of static‐headspace SPME to extract lactones was disappointing, regardless of the type of SPME fiber or the temperature used. Dynamic‐headspace SPME extraction with 50‐/30‐μm divinylbenzene‐Carboxen on a polydimethylsiloxane fiber at 100 °C, by contrast, enabled the analysis of volatiles, including delta‐lactones, gamma‐lactones, and diterpenoids, with 50‐/30‐μm divinylbenzene‐Carboxen on a polydimethylsiloxane fiber at 100 °C. Fifty‐three compounds were identified from only 0.20 g of rendered beef fat, and 76% of these showed reliable peak size repeatability: the coefficient of variation was less than 10% on the total ion chromatograms obtained from gas chromatography–mass spectrometry (GC–MS) analysis. Some lactones showed higher CV values (>10%), but single‐ion mode GC–MS analysis reduced them to 10% or less. In a study of beef samples available to the Japanese market, our analytical procedure revealed significantly higher levels of 1‐hexanol, octadecane, ethyl tetradecanoate, gamma‐nonalactone, but lower levels of delta‐decalactone, delta‐dodecalactone, and neophytadiene, in Japanese Black cattle than in beef imported from Australia.

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