Misir R, Laarveld B, Blair R
J Chromatogr. 1985 Aug 30;331(1):141-8. doi: 10.1016/0021-9673(85)80015-7.
The major limitation to fatty acid analysis by gas-liquid chromatography is associated with preparation of fatty acid methyl esters (FAME). In the present study, FAME preparations were made from plant oils (corn, olive, sunflower), sunflower oil margarine, lard and various animal tissue fats by a rapid transesterification involving tetramethylammonium hydroxide in methanol, and also by a longer conventional saponification-esterification method. Fats from animal (beef, mutton, pork) adipose tissues were extracted by a simpler modified procedure and also by the Folch method prior to the rapid and the conventional FAME preparations, respectively. FAME analysis on a gas-liquid chromatograph equipped with a Silar 10C glass capillary column indicated similar fatty acid composition of a given fat or oil, whether FAME was prepared by the rapid or the longer conventional method. The data obtained by both methods were very highly correlated for all the fats (r = 0.9895 - 0.9999). However, the rapid method showed a tendency for enhanced recoveries of lower chain fatty acids (e.g. 14:0), and also of unsaturated C18 isomers. Possibly, losses of fatty acids that occurred during the lengthy fat extraction, fatty acid esterification or ether-evaporation FAME concentration steps (conventional method) were minimised by the single transesterification step (rapid method). This rapid transesterification method appears to be an attractive alternative to FAME preparation from a wide variety of different fats for gas-liquid chromatographic analysis.
气相色谱法分析脂肪酸的主要限制与脂肪酸甲酯(FAME)的制备有关。在本研究中,通过在甲醇中使用氢氧化四甲铵进行快速酯交换反应,以及采用较长时间的传统皂化 - 酯化方法,从植物油(玉米、橄榄、向日葵)、向日葵油人造黄油、猪油和各种动物组织脂肪中制备FAME。在分别进行快速和传统的FAME制备之前,采用一种更简单的改良方法以及Folch法从动物(牛肉、羊肉、猪肉)脂肪组织中提取脂肪。在配备Silar 10C玻璃毛细管柱的气相色谱仪上进行FAME分析表明,无论FAME是通过快速方法还是较长时间的传统方法制备,给定脂肪或油的脂肪酸组成相似。两种方法获得的数据在所有脂肪中都具有非常高的相关性(r = 0.9895 - 0.9999)。然而,快速方法显示出较低链脂肪酸(例如14:0)以及不饱和C18异构体回收率提高的趋势。可能是由于单一的酯交换步骤(快速方法)将在漫长的脂肪提取、脂肪酸酯化或醚蒸发FAME浓缩步骤(传统方法)中发生的脂肪酸损失降至最低。这种快速酯交换方法似乎是从各种不同脂肪中制备FAME用于气相色谱分析的一种有吸引力的替代方法。