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Trace anti-inflammatory β-carboline alkaloid identified in Arenaria kansuensis by two-dimensional chromatography coupled with UniElut C18AEX based solid-phase extraction re-enrichment technology
Journal of Chromatography B ( IF 3 ) Pub Date : 2017-10-31 , DOI: 10.1016/j.jchromb.2017.10.058
Yulei Cui , Na Shen , Shuo Wang , Lijuan Mei , Zenggen Liu , Jun Dang , Yanduo Tao

Traditional Chinese medicine is important for discovery of drug precursors. However, information about trace chemical composition of them is very limited due to the lack of appropriate enrichment and chromatographic purification methods In our work, A. kansuensis was taken as an example, a novel two-dimensional reversed-phase/hydrophilic interaction liquid chromatography coupled with UniElut C18AEX solid-phase extraction re-enrichment method based on anti-inflammatory bioactivity-guided assay was developed for gathering and purifying trace β-carboline alkaloids with high purity from the ethyl acetate extract of A. kansuensis. Extraction with ethyl acetate as the first enrichment method, then, a UniElut C18AEX column was employed to re-enrich trace fraction which was hardly detected by diode array detector during high performance liquid chromatography analysis, eighteen grams of UniElut C18AEX was used as sorbent material to pack a 60 mL pipette tip for the extraction of β-carboline alkaloids from 100 mL of ethyl acetate sample. The whole extraction process was finished in 10 min, and the volume of eluent used was only 120 mL. The enriching fraction (100 mg) was used for the following two-dimensional purification. First-dimensional preparation was carried on a RP-Megress-C18 prep column, and four anti-inflammatory fractions were obtained from the 100 mg re-enriching sample with a recovery of 66.9%. A HILIC-XAmide prep column was selected for the second dimensional preparation. Finally, two pair of analogue β-carboline alkaloids and one other β-carboline alkaloid were purified from A. kansuensis. The purity of the isolated compounds was ≫>98%, which indicated that the method was efficient to re-enrich and manufacture single trace β-carboline alkaloids with high purity from A. kansuensis. Additionally, this method showed great potential to serve as a good example for the purification and enrichment of analogue structure anti-inflammation carboline alkaloids from other plant materials.



中文翻译:

二维色谱-基于UniElut C18AEX的固相萃取富集技术鉴定甘肃细叶中的痕量抗炎β-咔啉生物碱

中药对于发现药物前体很重要。然而,由于缺乏适当的富集和色谱纯化方法,有关它们的微量化学组成的信息非常有限。在我们的工作中,以甘肃曲霉为例,提出了一种新型的二维反相/亲水相互作用液相色谱法。研发了基于抗炎生物活性指导法的UniElut C18AEX固相萃取再富集方法,从甘肃曲霉的乙酸乙酯提取物中收集和纯化高纯度的痕量β-咔啉生物碱。首先以乙酸乙酯萃取为富集方法,然后使用UniElut C18AEX柱重新富集痕量级分,该级分在高效液相色谱分析中很难被二极管阵列检测器检测到,十八克UniElut C18AEX被用作吸附剂。用60 mL移液器吸头从100 mL乙酸乙酯样品中提取β-咔啉生物碱。整个萃取过程在10分钟内完成,洗脱液的用量仅为120 mL。富集级分(100mg)用于以下二维纯化。在RP-Megress-C18制备柱上进行一维制备,从100 mg富集样品中获得了四个抗炎组分,回收率为66.9%。选择HILIC-XAmide制备柱进行第二维制备。最后,从中纯化了两对类似的β-咔啉生物碱和另一对β-咔啉生物碱。A.甘肃。分离出的化合物的纯度> 98%,表明该方法可有效地富集和生产甘肃曲霉的单痕量β-咔啉生物碱。此外,该方法显示出巨大的潜力,可以作为从其他植物材料中纯化和富集类似结构抗炎性咔啉生物碱的良好实例。

更新日期:2017-10-31
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