University of Pisa, Department of Chemistry and Industrial Chemistry, Italy.
J Chromatogr A. 2013 Sep 20;1308:114-24. doi: 10.1016/j.chroma.2013.08.015. Epub 2013 Aug 8.
A new method for the analysis of triglycerides (TAGs) in vegetable oils was developed using a Poroshell 120 EC-C18 column (3.0 mm×50 mm, 2.7 μm) with a high resolution ESI-Q-ToF tandem mass spectrometer as detection system. We used an Agilent Poroshell column, which is characterized by a recently developed stationary phase based on non-porous core particles. The results highlighted the advantages of this column in terms of the dramatic improvement in the number of theoretical plates and in low column backpressure. The developed method enabled us to analyze complex mixtures of more than 40 TAGs within less than 25 min and with a low backpressure (lower than 100 bar), and represents the first application of a core-shell stationary phase in reverse phase HPLC using an ESI-Q-ToF as detection system. The method was optimized on standards of TAGs, validated and applied to several plant oils. By a quantitative point of view, the method showed a very good linearity (r(2)>0.999) in the range 0.1-2.4 μg/g; high intra- and inter-day precision both in terms of retention times (RSD%<0.04%) and peak areas (RSD%<0.3%). Limits of detection and quantitation were lower than 0.03 μg/g and 0.10 μg/g, respectively.
开发了一种新的植物油中甘油三酯(TAGs)分析方法,使用 Poroshell 120 EC-C18 柱(3.0mm×50mm,2.7μm)和高分辨率 ESI-Q-ToF 串联质谱作为检测系统。我们使用了 Agilent Poroshell 柱,其特点是基于无孔核颗粒的最近开发的固定相。结果突出了该柱的优势,在理论塔板数和低柱背压方面有了显著提高。所开发的方法能够在不到 25 分钟的时间内分析超过 40 种 TAG 的复杂混合物,并且柱背压低(低于 100 巴),这是首次在反相 HPLC 中使用 ESI-Q-ToF 作为检测系统应用核壳固定相。该方法在 TAG 标准品上进行了优化、验证并应用于几种植物油。从定量的角度来看,该方法在 0.1-2.4μg/g 的范围内表现出非常好的线性(r(2)>0.999);保留时间(RSD%<0.04%)和峰面积(RSD%<0.3%)的日内和日间精密度均很高。检测限和定量限分别低于 0.03μg/g 和 0.10μg/g。