Journal of Chromatography A ( IF 3.8 ) Pub Date : 2021-03-18 , DOI: 10.1016/j.chroma.2021.462080 Heng Zhu , Iftikhar Ali , Hidayat Hussain , Manzoor Hussain , Xing-Bao Wang , Xiangyun Song , Ge Luo , Zhenfang Zhang , Zhigang Wang , Daijie Wang
Acorus tatarinowii Schott is a traditional Chinese medicine used to treat memory and cognitive dysfunction. Because of their efficacy and lower toxic effects, research on α- and β-asarone, the phytoconstituents, has attracted attention owing to their remarkable pharmacological activities. Silver ion coordination complexation high-speed counter-current chromatography was used to separate these isomers from A. tatarinowii extract, coupled with accelerated solvent extraction. Accelerated solvent extraction parameters were investigated with single-factor and orthogonal testing. A two-phase solvent system composed of n-hexane-ethyl acetate-ethanol-water (2:1:2:1, v/v) with 0.50 mol/L silver ions was selected for separation. From 2.0 g crude extract, 1.4 g of β-asarone and 0.09 g of α-asarone were obtained with purities over 98% by sequential sample loading in 20 h. The isolated compounds were identified by electrospray ionization mass spectrometry, 1H and 13C NMR. Silver ions significantly increased the separation factor and retention of the stationary phase. The chromatographic behavior indicated that cis-configuration was more strongly complexed with the silver ion. This was further demonstrated with the help of computational analysis. In conclusion, the established method could be employed to separate other cis-trans or E/Z isomers that form coordination complexes.
中文翻译:
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哥白A中顺/反式细辛的提取和纯化:加速溶剂萃取和银离子配位高速逆流色谱法
Acorus tatarinowii Schott是用于治疗记忆力和认知功能障碍的传统中药。由于它们的功效和较低的毒性作用,由于其出色的药理活性,对植物成分α-和β-花生四烯酮的研究引起了人们的关注。银离子配位络合高速逆流色谱法用于从塔氏曲霉提取物中分离出这些异构体,并进行了加速溶剂提取。通过单因素试验和正交试验研究了加速的溶剂萃取参数。组成的两相溶剂体系Ñ 1:2:1,己烷-乙酸乙酯-乙醇-水(2体积/体积选择0.50 mol / L的银离子进行分离。通过在20 h内连续加载样品,从2.0 g粗提物中获得1.4 g的β-细辛醚和0.09 g的α-细辛醚。通过电喷雾电离质谱,1 H和13 C NMR鉴定分离的化合物。银离子显着提高了固定相的分离系数和保留率。色谱行为表明,顺式构型与银离子更强地络合。这在计算分析的帮助下得到了进一步证明。总之,所建立的方法可用于分离其他顺式-反式 或形成配位化合物的E / Z异构体。