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采用假分子印迹固相萃取和高效液相色谱法对中草药中的马兜铃酸 I 进行选择性分析。

Selective analysis of aristolochic acid I in herbal medicines by dummy molecularly imprinted solid-phase extraction and HPLC.

机构信息

Faculty of Pharmacy, School of Medicine, Xi'an Jiaotong University, Xi'an, Shaanxi, P.R. China.

出版信息

J Sep Sci. 2017 Jul;40(13):2791-2799. doi: 10.1002/jssc.201700116. Epub 2017 Jun 19.

Abstract

In this study, surface molecularly imprinted polymers were prepared as the selective sorbents for separation of aristolochic acid I in herbal medicine extracts by a facile approach. A less toxic dummy template, ofloxacin, was used to create specific molecule recognition sites for aristolochic acid I in the synthesized polymers. The polymers were characterized by Fourier-transfer infrared spectroscopy, scanning electron microscopy, thermogravimetric analysis, elemental analysis, and nitrogen adsorption-desorption test. The adsorption capacity was calculated using adsorption kinetics, selectivity, and recycling experiments. The obtained polymers exhibited high thermostability, fast equilibrium time, and excellent binding ability. Subsequently, the polymers applied as the solid-phase extraction absorbent was proposed and used for the enrichment and analysis of aristolochic acid I in herbal plants. The result showed that the aristolochic acid I was enriched up to 16 times after analysis by using high-performance liquid chromatography. The good linearity for aristolochic acid I was obtained in the range of 0.1-200 μg/mL (R  = 0.9987). The recovery and precision values were obtained (64.94-77.73%, RSDs% ≤ 0.8%, n = 3) at three spiked concentration levels. This work provided a promising method for selective enrichment, extraction, and purification of aristolochic acid I from complex herbal plants.

摘要

在这项研究中,通过一种简便的方法制备了表面分子印迹聚合物,作为从草药提取物中分离马兜铃酸 I 的选择性吸附剂。使用毒性较小的假模板氧氟沙星在合成聚合物中为马兜铃酸 I 创建特定的分子识别位点。通过傅里叶变换红外光谱、扫描电子显微镜、热重分析、元素分析和氮气吸附-解吸试验对聚合物进行了表征。通过吸附动力学、选择性和回收实验计算了吸附容量。所得聚合物表现出高热稳定性、快速平衡时间和优异的结合能力。随后,提出并使用聚合物作为固相萃取吸附剂,用于草药中马兜铃酸 I 的富集和分析。结果表明,通过高效液相色谱分析后,马兜铃酸 I 的富集倍数高达 16 倍。马兜铃酸 I 在 0.1-200μg/mL 范围内具有良好的线性关系(R = 0.9987)。在三个加标浓度水平下,回收率和精密度值为 64.94-77.73%(RSD%≤0.8%,n=3)。这项工作为从复杂的草药中选择性富集、提取和纯化马兜铃酸 I 提供了一种很有前途的方法。

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