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基质固相分散结合高效液相色谱-紫外检测法同时提取、纯化和测定五味子果实中的六种木脂素

Matrix Solid-Phase Dispersion Coupled with HPLC-UV for Simultaneous Extraction, Purification and Determination of Six Lignans in Schisandra chinensis Fruits.

作者信息

Song Haiyan, Chang Kejian, Zhang Liang, Zhu Wenbo, Li Yingying, Hu Haobin, Zhang Xiaojuan, Xi Yongfeng, Li Lu

机构信息

College of Chemistry & Chemical Engineering, Longdong University, Qingyang 745000, P.R. China.

出版信息

J Chromatogr Sci. 2022 Apr 28;60(4):387-400. doi: 10.1093/chromsci/bmab083.

Abstract

An efficient method for simultaneous extraction, purification and determination of six lignans in Schisandra chinensis Baill was developed by employing matrix solid-phase dispersion (MSPD) extraction followed by HPLC-UV determination analysis. Several sorbent and desorption solvent that affected the extraction yield of lignans were investigated; neutral alumina and absolute ethanol were selected as the best dispersing material and desorption agent, respectively. Other extraction conditions for MSPD were optimized as follows: 1:2 of S. chinensis raw material to neutral aluminum oxide mass ratio, 1:30 (g/mL) of sample to absolute ethanol, 2.5 h of desorption time and 50°C of desorption temperature. Under the above conditions, the total extraction yield for six lignans have reached (16.99 ± 0.33) x 103 mg/kg with a higher content of 6.88 ± 0.25% in the extracts. Comparative studies were explored by conducting other six extraction approaches including Soxhlet extraction, heat reflux extraction, smashing tissue extraction, microwave-assisted extraction, ultrasonic-assisted extraction and ultrasonic-microwave synergistic extraction. Results showed MSPD technique not only improved the extraction yield, but also improved the purity of lignans, it can be generalized to more extraction of natural compounds. In addition, the validated HPLC-UV method had been successfully applied to analysis of lignans from 10 real S. chinensis samples.

摘要

采用基质固相分散(MSPD)萃取结合高效液相色谱 - 紫外检测分析,建立了一种同时提取、纯化和测定五味子中六种木脂素的有效方法。考察了几种影响木脂素提取率的吸附剂和解吸溶剂;分别选择中性氧化铝和无水乙醇作为最佳分散材料和解吸剂。MSPD的其他提取条件优化如下:五味子原料与中性氧化铝质量比为1:2,样品与无水乙醇比例为1:30(g/mL),解吸时间2.5小时,解吸温度50°C。在上述条件下,六种木脂素的总提取率达到(16.99±0.33)×103 mg/kg,提取物中含量较高,为6.88±0.25%。通过进行其他六种提取方法进行比较研究,包括索氏提取、热回流提取、组织捣碎提取、微波辅助提取、超声辅助提取和超声 - 微波协同提取。结果表明,MSPD技术不仅提高了提取率,还提高了木脂素的纯度,可推广应用于更多天然化合物的提取。此外,经过验证的高效液相色谱 - 紫外方法已成功应用于10个实际五味子样品中木脂素的分析。

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