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

• Published in: Journal of food science Vol. 73; no. 5; pp. C420 - C425
• Main Authors: Watanabe, A, Ueda, Y, Higuchi, M, Shiba, N
• Format: Journal Article
• Language: English
• Published: Malden, USA Blackwell Publishing Inc 01.06.2008; Institute of Food Technologists; Wiley Subscription Services, Inc
• Subjects: animal fats and oils; Animals; Beef; beef cattle; beef fat; Biological and medical sciences; Cattle; cattle feeding; cooked foods; Diterpenes - analysis; diterpenoids; dynamic-headspace; Extraction processes; Fatty Acids, Volatile - analysis; food analysis; food composition; Food industries; Food processing industry; Food products; Food science; Fundamental and applied biological sciences. Psychology; gas chromatography; Gas Chromatography-Mass Spectrometry - methods; grain-fed livestock; grass-fed livestock; headspace analysis; lactones; Lactones - analysis; Mass spectrometry; Meat - analysis; Meat and meat product industries; microextraction; Odorants - analysis; Oils & fats; Phase transitions; sensory properties; solid phase extraction; Solid Phase Microextraction - methods; solid-phase microextraction; Species Specificity; Studies; Temperature; terpenoids; volatile compounds; Volatilization; Wagyu; Volatile compound; Terpenoid; terpenoids; Meat product; Lactone; solid-phase microextraction; Solid phase microextraction; Gas chromatography; beef fat; lactones; dynamic-headspace; Analysis; Fat; Headspace; Beef; Mass spectrometry
• ISSN: 0022-1147; 1750-3841
• DOI: 10.1111/j.1750-3841.2008.00764.x

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.