Fardin-Kia Ali Reza, Delmonte Pierluigi, Kramer John K G, Jahreis Gerhard, Kuhnt Katrin, Santercole Viviana, Rader Jeanne I
Office of Regulatory Science, Center for Food Safety and Applied Nutrition, HFS-717, US Food and Drug Administration, 5100 Paint Branch Pkwy, College Park, MD, 20740, USA,
Lipids. 2013 Dec;48(12):1279-95. doi: 10.1007/s11745-013-3830-2. Epub 2013 Sep 17.
The fatty acids contained in marine oils or products are traditionally analyzed by gas chromatography using capillary columns coated with polyethylene glycol phases. Recent reports indicate that 100 % cyanopropyl siloxane phases should also be used when the analyzed samples contain trans fatty acids. We investigated the separation of the fatty acid methyl esters prepared from menhaden oil using the more polar SLB-IL111 (200 m × 0.25 mm) ionic liquid capillary column and the chromatographic conditions previously optimized for the separation of the complex mixture of fatty acid methyl esters prepared from milk fat. Identifications of fatty acids were achieved by applying Ag(+)-HPLC fractionation and GC-TOF/MS analysis in CI(+) mode with isobutane as the ionization reagent. Calculation of equivalent chain lengths confirmed the assignment of double bond positions. This methodology allowed the identification of 125 fatty acids in menhaden oil, including isoprenoid and furanoid fatty acids, and the novel 7-methyl-6-hexadecenoic and 7-methyl-6-octadecenoic fatty acids. The chromatographic conditions applied in this study showed the potential of separating in a single 90-min analysis, among others, the short chain and trans fatty acids contained in dairy products, and the polyunsaturated fatty acids contained in marine products.
传统上,使用涂有聚乙二醇固定相的毛细管柱通过气相色谱法分析海洋油类或产品中所含的脂肪酸。最近的报告表明,当分析样品中含有反式脂肪酸时,也应使用100%氰丙基硅氧烷固定相。我们使用极性更强的SLB-IL111(200 m×0.25 mm)离子液体毛细管柱以及先前针对乳脂肪制备的脂肪酸甲酯复杂混合物分离优化的色谱条件,研究了鲱鱼油制备的脂肪酸甲酯的分离。通过应用Ag(+)-HPLC分级分离以及以异丁烷为电离试剂在CI(+)模式下进行GC-TOF/MS分析来鉴定脂肪酸。等效链长的计算证实了双键位置的归属。该方法能够鉴定鲱鱼油中的125种脂肪酸,包括类异戊二烯和呋喃类脂肪酸,以及新型的7-甲基-6-十六碳烯酸和7-甲基-6-十八碳烯酸。本研究中应用的色谱条件显示出在单次90分钟分析中分离多种物质的潜力,其中包括乳制品中的短链和反式脂肪酸以及海产品中的多不饱和脂肪酸。