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采用大孔树脂柱层析法制备富含莽草酸的银杏叶提取物的有效而全面的优化策略。

An effective and comprehensive optimization strategy for preparing Ginkgo biloba leaf extract enriched in shikimic acid by macroporous resin column chromatography.

机构信息

Pharmaceutical Informatics Institute, College of Pharmaceutical Sciences, Zhejiang University, Hangzhou, China.

College of Pharmaceutical Sciences, Taizhou University, Jiaojiang, China.

出版信息

Phytochem Anal. 2024 Aug;35(6):1428-1442. doi: 10.1002/pca.3375. Epub 2024 May 9.

DOI:10.1002/pca.3375
PMID:38725319
Abstract

INTRODUCTION

Previously reported preparation methods of Ginkgo biloba leaf extract (EGBL) have mainly focused on the enrichment of flavonoid glycosides (FG) and terpene trilactones (TT), which led to the underutilization of G. biloba leaves (GBL).

OBJECTIVES

To make full use of GBL, in this study, a comprehensive optimization strategy for preparing EGBL by macroporous resin column chromatography was proposed and applied to enrich FG, TT, and shikimic acid (SA) from GBL.

METHODOLOGY

Initially, the static adsorption and desorption were executed to select suitable resin. Then, the influences of solution pH were investigated by the static and dynamic adsorption. Subsequently, eight process parameters were systematically investigated via a definitive screening design (DSD). After verification experiments, scale-up enrichment was carried out, investigating the feasibility of the developed strategy for application on an industrial scale.

RESULTS

It was found that XDA1 was the most appropriate adsorbent for the preparation of EGBL at solution pH 2.0. Furthermore, based on the constraints of the desired quality attributes, the optimized ranges of operating parameters were successfully acquired, and the verification experiments demonstrated the accuracy and reliability of using DSD to investigate the chromatography process for the preparation of EGBL. Finally, magnified experiments were successfully performed, obtaining the EGBL containing 26.54% FG, 8.96% TT, and 10.70% SA, which reached the SA level of EGB761, an international standard EGBL.

CONCLUSION

The present study not only provided an efficient and convenient approach for the preparation of EGBL enriched in SA but also accelerated efforts to high-value utilization of GBL.

摘要

简介

先前报道的银杏叶提取物(EGBL)的制备方法主要集中在黄酮苷(FG)和萜类三内酯(TT)的富集上,这导致银杏叶(GBL)的利用率较低。

目的

为充分利用GBL,本研究提出了一种用大孔树脂柱色谱法制备 EGBL 的综合优化策略,并将其应用于从 GBL 中富集 FG、TT 和莽草酸(SA)。

方法

首先进行静态吸附和解吸实验,选择合适的树脂。然后,通过静态和动态吸附实验研究溶液 pH 的影响。随后,通过完全析因设计(DSD)系统研究了八个工艺参数。经过验证实验后,进行了放大浓缩实验,考察了所开发策略在工业规模上应用的可行性。

结果

结果发现,在溶液 pH 2.0 下,XDA1 是制备 EGBL 的最适宜吸附剂。此外,基于所需质量属性的约束条件,成功获得了操作参数的优化范围,并通过验证实验证明了使用 DSD 研究制备 EGBL 色谱过程的准确性和可靠性。最后,成功进行了放大实验,得到了含有 26.54%FG、8.96%TT 和 10.70%SA 的 EGBL,达到了国际标准 EGB761 中规定的 SA 水平。

结论

本研究不仅为制备富含 SA 的 EGBL 提供了一种高效便捷的方法,而且加速了 GBL 的高值化利用。

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