Structural properties, antioxidant and hypoglycemic activities of polysaccharides purified from pepper leaves by high-speed counter-current chromatography

Background:Stenoloma chusanum (L.) Ching is a Chinese traditional medicinal fern with high total flavonoid and total phenolic content. Traditionally, phenolic compounds were separated by using column chromatography, which is relatively inefficient. </P><P> Objective: This study aims to use an efficient method to separate natural products from S. chusanum by Medium-Pressure Liquid Chromatography (MPLC) and High-Speed Counter-Current Chromatography (HSCCC).Methods:In the present research, firstly, a sample (2.5 g) from the dichloromethane extract of S. chusanum was separated by MPLC. Next, fraction P5 was purified by HSCCC with a two-phase solvent system composed of hexane-ethyl acetate-methanol-water (HEMWat) at a volume ratio of 2:4:1:4 (v/v/v/v). </P><P> Result: Four phenolic acids were obtained and their structures were identified by means of NMR and ESI-mass analysis. They were identified as: 1) protocatechuic acid (34 mg, purity 90.1%), 2) syringic acid (66 mg, purity 99.0%), 3) p-hydroxybenzoic acid (5 mg, purity 91.2%) and 4) vanillic acid (6 mg, purity 99.3%).Conclusion:The combination of MPLC and HSCCC is a high-efficiency separation method for natural products. This is the first report with regard to the separation of four phenolic acids in one step by MPLC and HSCCC from S. chusanum (L.) Ching.

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HSCCC Separation of Three Main Compounds from the Crude Extract of Dracocephalum Tanguticum by Using Dimethyl Sulfoxide as Cosolvent

Journal of Chromatographic Science ◽

10.1093/chromsci/bmaa094 ◽

2020 ◽

Author(s):

Xue Yang ◽

Yongling Liu ◽

Tao Chen ◽

Nana Wang ◽

Hongmei Li ◽

...

Keyword(s):

Acetic Acid ◽

Ethyl Acetate ◽

Dimethyl Sulfoxide ◽

Efficient Method ◽

Crude Extract ◽

High Speed ◽

Glacial Acetic Acid ◽

Butyl Alcohol ◽

Preparative Hplc ◽

Counter Current

Abstract Separation of natural compounds directly from the crude extract is a challenging work for traditional column chromatography. In the present study, an efficient method for separation of three main compounds from the crude extract of Dracocephalum tanguticum has been successfully established by high-speed counter-current chromatography (HSCCC). The crude extract was directly introduced into HSCCC by using dimethyl sulfoxide as cosolvent. Ethyl acetate/n-butyl alcohol/0.3% glacial acetic acid (4: 1: 5, v/v) system was used and three target compounds with purity higher than 80% were obtained. Preparative HPLC was used for further purification and three target compounds with purity higher than 98% were obtained. The compounds were identified as chlorogenic acid, pedaliin and pedaliin-6″-acetate.

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Scale-Up Preparation of Crocins I and II from Gardeniajasminoides by a Two-Step Chromatographic Approach and Their Inhibitory Activity Against ATP Citrate Lyase

Molecules ◽

10.3390/molecules26113137 ◽

2021 ◽

Vol 26 (11) ◽

pp. 3137

Author(s):

Shuguang Guan ◽

Qiaoli Pu ◽

Yinan Liu ◽

Honghong Wu ◽

Wenbo Yu ◽

...

Keyword(s):

Inhibitory Activity ◽

High Speed ◽

Scale Up ◽

Cost Effective ◽

Atp Citrate Lyase ◽

Gardenia Jasminoides ◽

Citrate Lyase ◽

Human Disorders ◽

Ic50 Values ◽

Counter Current

Crocins are highly valuable natural compounds for treating human disorders, and they are also high-end spices and colorants in the food industry. Due to the limitation of obtaining this type of highly polar compound, the commercial prices of crocins I and II are expensive. In this study, macroporous resin column chromatography combined with high-speed counter-current chromatography (HSCCC) was used to purify crocins I and II from natural sources. With only two chromatographic steps, both compounds were simultaneously isolated from the dry fruit of Gardenia jasminoides, which is a cheap herbal medicine distributed in a number of countries. In an effort to shorten the isolation time and reduce solvent usage, forward and reverse rotations were successively utilized in the HSCCC isolation procedure. Crocins I and II were simultaneously obtained from a herbal resource with high recoveries of 0.5% and 0.1%, respectively, and high purities of 98.7% and 99.1%, respectively, by HPLC analysis. The optimized preparation method was proven to be highly efficient, convenient, and cost-effective. Crocins I and II exhibited inhibitory activity against ATP citrate lyase, and their IC50 values were determined to be 36.3 ± 6.24 and 29.7 ± 7.41 μM, respectively.

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