Method for separating compound by off-line three-dimensional high-speed counter-current chromatography

A high-speed countercurrent chromatography and compound technology, which is applied in separation methods, separation/purification of carbonyl compounds, organic chemical methods, etc., can solve the problems of large sample loss, large solvent consumption, and the separation of effective chemical components of betel leaf by HSCCC. , to increase the productivity

CN114591309APending Publication Date: 2022-06-07上海致臻志臣科技有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2022-06-07

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Abstract

The invention provides a method for off-line three-dimensional high-speed counter-current chromatography separation of compounds. The invention also provides a method for separating the neolignan compound from the betel. According to the off-line three-dimensional high-speed counter-current chromatography compound separation method provided by the invention, the separation effect of a previous solvent system is kept by an in-situ concentration technology, and rapid separation of compounds with similar structures is realized by combining online storage and multi-stage circulating elution.
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Description

technical field

[0001] The invention relates to the technical field of natural medicines, in particular to a method for separating compounds by off-line three-dimensional high-speed countercurrent chromatography. More specifically, the present invention relates to a method for the separation and purification of compounds of natural origin using off-line three-dimensional high-speed countercurrent chromatography. Background technique

[0002] High-speed countercurrent chromatography (HSCCC) was first proposed by Ito et al. in the early 1960s, and then gradually developed. It is a unique solid support-free, liquid-liquid partition chromatography with the ability to eliminate irreversible samples on solid supports. The characteristic of adsorption is that the stationary phase is the mobile phase, which is a commonly used recyclable organic reagent. Compared with traditional separation techniques, HSCCC has the advantages of fast and efficient separation, simple operation, low ...

Examples

Embodiment 1

[0083] 1. Experimental medicinal materials

[0084] Piper betle.L belongs to a climbing plant belonging to the genus Piper of the family Piperaceae. The betel leaf samples were collected from Yunnan Province.

[0085] 2. Experimental reagents

[0086] Petroleum ether, ethyl acetate, methanol, and chloroform used for HSCCC separation were all analytically pure reagents, purchased from Shanghai Sinopharm Chemical Reagent Company, China; HPLC methanol was obtained from CINC High Purity Solvent Company (Shanghai).

[0087] 3. Experimental equipment

[0088] High-speed countercurrent chromatograph (OptiChrome-300plus semi-preparative type), constant flow pump (CF-80), six-port valve, PTFE connecting tube (1.6*2.4mm), injection loop (120ml), multi-layer coil ( Internal diameter: 2.1mm; radius: 80mm) was provided by Jiangyin Countercurrent Chromatography Technology Co., Ltd.; UV detector (UV1001), purchased from Shanghai Sanwei Scientific Instrument Co., Ltd.; Nuclear Magnetic Reson...