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A kind of separation and purification method of gamma cyclodextrin

A gamma cyclodextrin, separation and purification technology, applied in the field of drug separation and purification, can solve the problems of inability to achieve secondary purification, large solvent consumption, and high purification cost, and achieve environmental protection, instrument cost saving, and separation efficiency that are beneficial to the solvent. high effect

Active Publication Date: 2022-03-22
杭州泽邦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although the methods for purifying gamma cyclodextrins have been reported in the above literatures, there is no obvious cocoa method that is fast and beneficial to industrial scale-up. Due to the large polarity and many structural analogues of gamma-cyclodextrin, the structure is relatively It is complex and contains multiple chiral centers, and there is almost no retention in the preparation of chromatography. After the first purification, the secondary purification cannot be achieved, so the purification cost is high and the amount of solvent is large. The above methods have certain disadvantages and limitations.

Method used

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  • A kind of separation and purification method of gamma cyclodextrin
  • A kind of separation and purification method of gamma cyclodextrin
  • A kind of separation and purification method of gamma cyclodextrin

Examples

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Embodiment 1

[0074] Separation and purification of gamma cyclodextrin: take gamma cyclodextrin and add methanol / water (v / v, 1 / 1) to prepare a solution with a concentration of 2 g / mL, and adjust the pH to 1-2 with 5% trifluoroacetic acid aqueous solution. After the solution was clarified, it was filtered through a filter membrane with a pore size of 0.45 μm, and the filtrate was collected for later use. A self-assembled column is used, and the column packing model is SiliaSphere series ODS, with a particle size of 50 μm and a pore size of 0.1% trifluoroacetic acid aqueous solution was used as mobile phase A, methanol was used as mobile phase B, and the flow rate was 80 mL / min. Such as figure 1 As shown, the equilibration time of the first column and the second column is about 15min, and the crude product loading is carried out by the first pump ( figure 1 Marked by solid line), at 25min (that is, when the detector detects the target peak), switch valve 1, valve 2 and valve 3 sequentially...

Embodiment 2

[0076] Separation and purification of gamma cyclodextrin: take gamma cyclodextrin and add methanol / water (v / v, 1 / 1) to prepare a solution with a concentration of 2 g / mL, and adjust the pH to 1-2 with 5% trifluoroacetic acid aqueous solution. After the solution was clarified, it was filtered through a filter membrane with a pore size of 0.45 μm, and the filtrate was collected for later use. A self-assembled column is used, and the column packing model is SiliaSphere series ODS, with a particle size of 50 μm and a pore size of 0.1% trifluoroacetic acid aqueous solution was used as mobile phase A, methanol was used as mobile phase B, and the flow rate was 80 mL / min. Such as figure 1 As shown, the equilibration time of the first column and the second column is about 15min, and the crude product loading is carried out by the first pump ( figure 1 Marked by the solid line), at 45min (the detector detects the target peak), switch valve 1, valve 2 and valve 3 sequentially and press...

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Abstract

The invention discloses a method for separating and purifying gamma cyclodextrin. Method First, the gamma cyclodextrin sample was dissolved in a mixed solution, and the insoluble matter was filtered out; then the filtered sample solution was loaded onto the ODS column; then the single-column internal circulation mode or the double-column internal circulation mode was used for separation; finally, the The mixed solvent is used as the mobile phase sample for gradient elution or isocratic elution, the target peak is collected in segments, and the components that meet the requirements of the target peak are collected to obtain the purified sample. The method of the present invention has the advantages of mild separation conditions, high separation efficiency, fast separation speed, strong versatility, etc., and can realize the separation and purification of gamma cyclodextrin samples very well, and can realize enrichment in a short time, and can be obtained by changing the elution conditions and Switching valve purification and even other types of compounds have good application prospects.

Description

technical field [0001] The invention belongs to the field of separation and purification of medicines, and in particular relates to a separation and purification method of gamma cyclodextrin, which uses assembled single-column or double-column internal circulation to enhance the column efficiency mode circulation equipment, adopts 0.1% trifluoroacetic acid water and Using methanol or acetonitrile as the mobile phase, high-purity gamma cyclodextrin can be obtained. Background technique [0002] Gamma cyclodextrin (γ-Cyclodextrin) is a cyclic oligosaccharide composed of 8 D-glucopyranose units. The main molecule of gamma cyclodextrin can form a conical cylinder with a wide top and a narrow bottom with open ends. This cavity can contain a wide range of guest molecules, thereby improving the solubility of the guest molecules and increasing the stability of the guest molecules. Therefore, gamma cyclodextrin is widely used in the fields of medicine, cosmetics, food and chemical in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/16
CPCC08B37/0012C08B37/0003
Inventor 潘远江谭艳云林德转王伟黄德权
Owner 杭州泽邦科技有限公司
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