Department of Analytical Chemistry, Faculty of Sciences, I. U. CINQUIMA, Analytical Chemistry Group (TESEA), University of Valladolid, C/ Paseo de Belén 5, Valladolid E-47011, Spain.
Department of Analytical Chemistry, Faculty of Sciences, I. U. CINQUIMA, Analytical Chemistry Group (TESEA), University of Valladolid, C/ Paseo de Belén 5, Valladolid E-47011, Spain.
J Chromatogr A. 2022 Dec 6;1685:463633. doi: 10.1016/j.chroma.2022.463633. Epub 2022 Nov 5.
The separation of ten flavanones (flavanone, 2'-hydroxyflavanone, 4'-hydroxyflavanone, 6-hydroxyflavanone, 7-hydroxyflavanone, naringenin, naringin, hesperetin, pinostrobin, and taxifolin) using supercritical fluid chromatography and considering achiral and chiral approaches has been studied in this work. For this purpose, different stationary phases and organic modifiers have been checked. Considering the achiral separation, the best results were obtained with the Lichrospher 100 Diol column at 35 °C, 3 mL/min, 150 bar and a gradient of 2-propanol from 5% to 50%. The baseline separation of the ten compounds was achieved in 18 min. Using the chiral column Chiralpak AD, the separation of the ten pairs of enantiomers was obtained in 32 min. In this case, the chromatographic conditions were 30 °C, 3 mL/min, 150 bar and the organic modifier was a mixture ethanol/methanol (80:20) containing 0.1% of trifluoroacetic acid applied in an elution gradient from 15% to 50%. The applicability of the proposed chiral method was assessed by analysing bee pollen samples and 2S-pinostrobin was determined in some of them.
本文研究了使用超临界流体色谱法分离十种黄烷酮（黄烷酮、2'-羟基黄烷酮、4'-羟基黄烷酮、6-羟基黄烷酮、7-羟基黄烷酮、柚皮苷、新橙皮苷、橙皮苷、根皮素和杨梅素），并考虑了手性和非手性方法。为此，检查了不同的固定相和有机溶剂。在手性分离方面，在 35°C、3mL/min、150 巴和 2-丙醇从 5%到 50%的梯度下，Lichrospher 100 Diol 柱获得了最佳结果。十种化合物在 18 分钟内实现了基线分离。使用手性柱 Chiralpak AD，十种对映异构体对得到了分离，用时 32 分钟。在这种情况下，色谱条件为 30°C、3mL/min、150 巴，有机溶剂为含有 0.1%三氟乙酸的乙醇/甲醇（80:20）混合物，采用从 15%到 50%的洗脱梯度。通过分析蜂花粉样品评估了所提出的手性方法的适用性，并在其中一些样品中测定了 2S-根皮素。
