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A method for preparing high-purity 1-deoxynojirimycin by combining membrane separation and column chromatography

A deoxynojirimycin and column chromatography technology, which is applied in the field of combined membrane separation and column chromatography to enrich 1-deoxynojirimycin, can solve the problems of mixed organic solvent, complicated processing technology, limited sample loading and the like , to achieve the effect of high efficiency, good separation selectivity and reasonable membrane separation process

Inactive Publication Date: 2015-07-29
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although high-purity DNJ can be obtained, there are disadvantages such as complicated treatment process, long elution time, and mixed organic solvents.
CN101654428A patent uses the gel filtration method to purify DNJ, the amount of sample loading is limited each time, and the cost is relatively high
In China, the combined application of microfiltration, ultrafiltration and nanofiltration membrane technology and column chromatography to enrich DNJ has not been reported.

Method used

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  • A method for preparing high-purity 1-deoxynojirimycin by combining membrane separation and column chromatography
  • A method for preparing high-purity 1-deoxynojirimycin by combining membrane separation and column chromatography
  • A method for preparing high-purity 1-deoxynojirimycin by combining membrane separation and column chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] process such as figure 1 ,Specific steps are as follows:

[0032] (1) Ultrasonic water extraction: crush and sieve the dry raw materials to obtain coarse powder. Weigh an appropriate amount of coarse powder, add distilled water at a liquid-to-solid ratio (mL / g) of 40:1, heat in a water bath at 70°C for 30 minutes with ultrasonic treatment, centrifuge and filter, collect the supernatant, repeat the extraction of the precipitate once according to the above steps, and combine twice The supernatant is the extract.

[0033] (2) Pretreatment: centrifuge the extract obtained in step (1), and then pass it through a 2.0 μm microporous membrane to obtain an ultrafiltration feed solution.

[0034] (3) Secondary ultrafiltration: the first ultrafiltration membrane of the ultrafiltration feed liquid obtained in step (2), during the ultrafiltration process, add deionized water to the feed liquid tank, and collect the first ultrafiltration permeate ; Then the permeate is treated wit...

Embodiment 2

[0039] In step (1) ultrasonic water extraction, use a liquid-to-material ratio of 10:1 (mL / g), and then use an ultrafiltration membrane with a molecular weight cut-off of 20kDa for the first ultrafiltration in step (3), The operating pressure is 0.8MPa, and the feed liquid temperature is 30°C; during the second ultrafiltration, an ultrafiltration membrane with a molecular weight cut-off of 1.0kDa is preferred, preferably 1.2MPa. Other operations are the same as in Example 1. The purity of the final DNJ refined sample was 83.56%.

Embodiment 3

[0041]In step (1) ultrasonic water extraction, use a liquid-to-material ratio of 20:1 (mL / g), and then use an ultrafiltration membrane with a molecular weight cut-off of 8kDa for the first ultrafiltration in step (3), The operating pressure is 0.8MPa, and the feed liquid temperature is 30°C; during the second ultrafiltration, the ultrafiltration membrane with a molecular weight cut-off of 1.0kDa is preferred, preferably 1.2MPa; Filtrate permeate for treatment, the preferred operating pressure is 1.2MPa. Other operations are the same as in Example 1. The purity of the final DNJ refined sample is 85.24%

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Abstract

The invention relates to the field of separation and purification of active ingredients of a natural product, in particular to a method for preparing high-purity 1-deoxynojirimycin with a combined membrane separation and column chromatography technology. According to the method, raw materials of silkworm and white mulberry is subjected to water extraction in aid of ultrasonic waves; an ultrafiltration feeding liquid is obtained through centrifugation and micro-filtration membrane treatment; and a 1-deoxynojirimycin product with purity larger than 80% is obtained through steps of secondary ultrafiltration, nanofiltration, cation exchange resin chromatography and dextrane gel chromatography. The method has the advantages of simple process, high efficiency, safety and environment protection.

Description

technical field [0001] The invention relates to the field of separation and purification of effective components of natural products, in particular to a method for enriching 1-deoxynojirimycin by combining membrane separation and column chromatography techniques. Background technique [0002] 1-deoxynojirimycin (DNJ for short) is a piperidine polyhydroxyalkaloid. The structure of DNJ is similar to that of glucose, which can competitively inhibit α-glucosidase, affect the carbohydrate metabolism and bioprocessing of organisms, and has various pharmacological activities such as lowering blood sugar, lowering blood fat, virus, anti-tumor and anti-inflammation . Therefore, the development and research of its related products have broad prospects for development. [0003] Studies have shown that the natural sources of DNJ mainly include sericulture resources such as mulberry leaves, mulberry branches, mulberry bark and silkworm. However, there are many kinds of substances in s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/46
Inventor 徐鑫刘国艳叶群张田田
Owner YANGZHOU UNIV
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