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A method that uses sugar to prefer reverse chromatography solvents

A countercurrent chromatography and solvent technology, applied in the field of countercurrent chromatography, can solve the problems of long time consumption and complicated solvent selection, and achieve the effects of reducing energy consumption, improving production efficiency, and facilitating automated production.

Active Publication Date: 2018-08-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for using sugar to optimize the solvent of countercurrent chromatography in view of the shortcomings of complex solvent selection, time-consuming, and professional knowledge in the above-mentioned existing countercurrent chromatographic separation process. This method is verified by a large number of experiments. And simple solvent selection strategy, can quickly separate high-purity flavonoids and podophyllotoxins

Method used

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  • A method that uses sugar to prefer reverse chromatography solvents
  • A method that uses sugar to prefer reverse chromatography solvents
  • A method that uses sugar to prefer reverse chromatography solvents

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The determination of the physical properties of flavonoids and podophyllotoxins comprises the following steps:

[0023] 1. Extraction and enrichment

[0024] First, the star anise lotus extract was directly subjected to column chromatography adsorption and enrichment, and then eluted with petroleum ether and ethyl acetate at a volume ratio of 2:1 to remove large polar impurities, and the eluate was collected. The physical properties of the compounds in the eluate were calculated according to ChemBioOffice Ultra 13.0, Cambridge Soft and are shown in Table 1. The crude product obtained when the volume ratio of petroleum ether and ethyl acetate was 2:1 was eluted, including hydrophilic podophyllotoxins and hydrophobic flavonoids.

[0025]

[0026]

[0027] Table 1. Physical Properties of Selected Compounds b

[0028] b Calculated according to ChemBioOffice Ultra 13.0, Cambridge Soft

Embodiment 2

[0030] The determination of the partition coefficient of flavonoids and podophyllotoxins in the n-hexane-ethyl acetate-methanol-water (4:6:4:6, v / v) system with sucrose as an additive comprises the following steps:

[0031] 1. Extraction and enrichment

[0032] Similar to Example 1, the star anise lotus extract was directly subjected to column chromatography adsorption and enrichment, and then eluted with petroleum ether and ethyl acetate at a volume ratio of 2:1 to remove large polar impurities and collect the eluate.

[0033] 2. Sugar solution preparation

[0034] Dissolving sucrose into certain quality water is prepared to form sugar solutions with mass concentration of 10%, 20% and 30% respectively.

[0035] 3. Determination of partition coefficients of compounds in star anise lotus in n-hexane-ethyl acetate-methanol-water (4:6:4:6, v / v) system with sucrose as additive

[0036] Add the crude star anise lotus to a 2mL centrifuge tube containing a two-phase system with a v...

Embodiment 3

[0038] The determination of the partition coefficient of flavonoids and podophyllotoxins in the n-hexane-ethyl acetate-methanol-water (5:5:5:5, v / v) system with sucrose as an additive comprises the following steps:

[0039] 1. Extraction and enrichment

[0040] Similar to Example 1, the star anise lotus extract was directly subjected to column chromatography adsorption and enrichment, and then eluted with petroleum ether and ethyl acetate at a volume ratio of 2:1 to remove large polar impurities and collect the eluate.

[0041] 2. Sugar solution preparation

[0042] Dissolving sucrose into certain quality water is prepared to form sugar solutions with mass concentration of 10%, 20% and 30% respectively.

[0043] 3. Determination of partition coefficients of compounds in star anise lotus in n-hexane-ethyl acetate-methanol-water (5:5:5:5, v / v) system with sucrose as additive

[0044] Add the crude star anise lotus to a 2mL centrifuge tube containing a two-phase system with a v...

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Abstract

The invention provides a method using sugar to preferably select a counter-current chromatography solvent. The method is characterized in that the sugar is used for increasing the distribution coefficient of a natural product and selecting the counter-current chromatography solvent, and specifically comprises the following steps of adding a series of different amounts of sugar into the selected two phase system, thoroughly mixing, analyzing the relationship of sugar amount and distribution coefficient, and determining the sugar amount according to the relationship, so as to determine the proper composition of the counter-current chromatography solvent. The method has the advantages that the proper solvent can be easily obtained, the target compound has a proper K value in the solvent, the method is especially suitable for the natural product with complicated component, the method is simple and practical, the selection difficulty of counter-current chromatography solvent is greatly decreased, the selection time is shortened, and the method is suitable for popularizing and applying.

Description

technical field [0001] The invention belongs to the technical field of countercurrent chromatography, relates to a method for determining a countercurrent chromatographic solvent, in particular to a method for using sugar to optimize a countercurrent chromatographic solvent. Background technique [0002] Countercurrent chromatography is a kind of full-liquid-liquid partition chromatography that does not need a solid phase carrier. Because it does not use a solid phase carrier but only uses a liquid phase as a stationary phase, compared with other chromatography, countercurrent chromatography has significant advantages. It can not only Avoiding adverse factors such as adsorption, denaturation, and tailing caused by solid phase carriers, the sample is almost 100% recovered, and it often has better selectivity for some compounds with similar structures but different distribution coefficients. In addition, countercurrent chromatography can be easily combined with other chromatog...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/42
CPCG01N30/42
Inventor 吴世华张利红
Owner ZHEJIANG UNIV
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