Präßler Hans, Siemens Kathy, Willems Sabrina, Winterhalter Peter, Almeida Roberto Baptista Pereira, Lago Joao Henrique Ghilardi, Jerz Gerold
Technische Universität Braunschweig, Institute of Food Chemistry, 38106 Braunschweig, Germany.
Departamento de Botânica, Universidade de São Paulo, Instituto de Biociências, São Paulo, SP, Brazil.
J Chromatogr A. 2025 Sep 13;1758:466190. doi: 10.1016/j.chroma.2025.466190. Epub 2025 Jul 3.
Bixa orellana (Bixaceae) seeds are widely used as food colouring and spice, but also as traditional medicine for treatment of several diseases. Terpenoids from Bixa orellana seeds were extracted by n-hexane and separated by semi-preparative high-performance countercurrent chromatography (HPCCC) and then scaled-up to a high speed countercurrent chromatography apparatus (HSCCC) operated in head-to-tail mode. Evaluation of five biphasic solvent systems led to the suitable system consisting of n-hexane, ethyl acetate, methanol and water (8:2:8:2, v/v/v/v). The CCC-experiments were monitored by off-line atmospheric pressure chemical ionisation mass-spectrometry (APCI-MS/MS) in positive ionisation mode to project single ion traces of target compounds. Off-line mass profiles were converted to column-graphs which showed co-elution effects and areas of pure recoverable substances. Four major compounds bixin (1), alismol (2), geranyl-geraniol (3), δ-tocotrienol (4) were targeted and HPCCC and HSCCC experiment performance was compared by their specific partition ratio values K, the separation factor α, as well as the resolution factor R.
红木（紫葳科）种子被广泛用作食用色素和香料，同时也作为治疗多种疾病的传统药物。用正己烷提取红木种子中的萜类化合物，并用半制备高效逆流色谱（HPCCC）进行分离，然后放大到以头对尾模式运行的高速逆流色谱仪（HSCCC）上进行分离。对五种双相溶剂体系进行评估，得出了由正己烷、乙酸乙酯、甲醇和水组成的合适体系（8:2:8:2，v/v/v/v）。通过离线大气压化学电离质谱（APCI-MS/MS）在正电离模式下监测CCC实验，以绘制目标化合物的单离子轨迹。将离线质谱图转换为柱状图，该图显示了共洗脱效应和纯可回收物质的面积。以四种主要化合物胭脂树橙（1）、泽泻醇（2）、香叶基香叶醇（3）、δ-生育三烯酚（4）为目标，并通过它们的特定分配比值K、分离因子α以及分辨率因子R比较了HPCCC和HSCCC实验性能。
