US Food and Drug Administration, National Center for Toxicological Research, Jefferson, AR, United States.
US Food and Drug Administration, National Center for Toxicological Research, Jefferson, AR, United States.
J Chromatogr B Analyt Technol Biomed Life Sci. 2020 Dec 15;1161:122415. doi: 10.1016/j.jchromb.2020.122415. Epub 2020 Oct 22.
The analysis of the fatty acid profile of triglycerides has long played a central role in the evaluation and classification of edible vegetable oils. However, the range of analytical procedures available to evaluate these profiles remains limited and are typically based on transesterification of the triglyceride fatty acid residues to methyl esters, followed by capillary gas-liquid chromatography (GC) coupled with flame ionization or mass spectrometry detection. Although robust and long-proven, these analytical methods tend to entail long chromatographic runs and are relatively insensitive. In order to expand the range of available techniques for the analysis of the fatty acid profile of triglycerides in vegetable oils, we report herein a novel method based upon a rapid and straightforward transesterification of the triglycerides with dimethylaminoethanol under alkaline conditions, followed by a "dilute-and-shoot" analysis by ultra-performance liquid chromatography coupled with electrospray tandem mass spectrometry. The chromatographic analysis is accomplished in 1.5 min, affording a high throughput of samples compared to techniques based upon GC approaches. The method performance was assessed intra- and inter-day with 10 representative saturated and unsaturated fatty acids ranging from C to C and afforded fatty acid profile accuracies of 93-108% and imprecisions of only 0.3-2.0%. The limit of quantification of the method, estimated as the minimum amount of derivatized oil sample capable of affording less than 20% accuracy and precision error was determined to be approximately 0.5 pg on-column, making this new method potentially valuable for fields where high sensitivity, precision, and accuracy may be required, such as in toxicology studies, forensics, archeology, or art analysis.
对甘油三酯脂肪酸谱的分析长期以来一直是评价和分类食用植物油的核心。然而,可用于评估这些图谱的分析程序范围仍然有限,并且通常基于将甘油三酯脂肪酸残基酯化为甲酯,然后进行毛细管气相色谱(GC)与火焰离子化或质谱检测相结合。虽然这些分析方法强大且久经考验,但它们往往需要长的色谱运行时间且相对不灵敏。为了扩大植物油中甘油三酯脂肪酸谱分析的可用技术范围,我们在此报告了一种基于在碱性条件下用二甲氨基乙醇快速简便地对甘油三酯进行酯交换,然后通过超高效液相色谱与电喷雾串联质谱进行“稀释和进样”分析的新方法。与基于 GC 方法的技术相比,色谱分析在 1.5 分钟内完成,提供了更高的样品通量。该方法的性能通过 10 种代表性的饱和和不饱和脂肪酸(从 C 到 C)进行了日内和日间评估,其脂肪酸谱准确度为 93-108%,精密度仅为 0.3-2.0%。该方法的定量限估计为能够提供低于 20%准确度和精密度误差的衍生油样品的最小量,约为 0.5pg 柱上,这使得这种新方法在需要高灵敏度、精密度和准确度的领域(如毒理学研究、法医学、考古学或艺术品分析)具有潜在的价值。