Method for separating 1-deoxidized nojirimycin monomer from mulberry leaf total alkaloid

A technology of deoxynojirimycin and total alkaloids, applied in the direction of organic chemistry, etc., to achieve the effects of cost reduction, low equipment requirements, and simple operation

Active Publication Date: 2008-12-03
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing separation schemes only obtained the total alkaloids of mulberry leaves, and furthe

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Get the total alkaloid powder of mulberry leaves and dissolve it in water to make the upper column liquid, which is adsorbed by the resin column of pretreated D151 resin. The inner diameter of the resin column is 1.5cm, and the length of the column is 60cm. 20. The processing capacity of the resin is 0.5mg total alkaloids of mulberry leaves / mL wet resin. After the adsorption is completed, it is eluted with water, and the elution flow rate is 1.0mL / min. Carry out qualitative detection, compare with 1-deoxynojirimycin reference substance, combine the single-component eluate with 1-deoxynojirimycin reference substance in the same position and show the same color spot, concentrate under reduced pressure and vacuum dry, Then carry out recrystallization with methanol / acetone (1:5), the melting temperature is 60°C, the heating time is 10min, let it stand for natural cooling to crystallize, repeat 3 times, and obtain a white solid sample, which is detected by high performance li...

Embodiment 2

[0025] Get the total alkaloid powder of mulberry leaves and dissolve it in water to make the upper column liquid, which is adsorbed by the resin column of pretreated Amberlite CG-50 resin. The inner diameter of the resin column is 1.5cm, and the length of the column is 60cm. 1:30, the treatment capacity of the resin is 0.8mg mulberry leaf total alkaloids / mL wet resin, after the adsorption is completed, it is eluted with 10% methanol, and the elution flow rate is 1.5mL / min. The collected eluate was qualitatively detected, compared with the 1-deoxynojirimycin reference substance, and the single-component eluate at the same position and showing the same color spots as the 1-deoxynojirimycin reference substance was combined, and the Concentrate under pressure and dry in vacuo, then recrystallize with methanol / acetone (1:3), dissolving temperature is 50°C, heating time is 15min, let stand to cool and crystallize naturally, repeat 5 times, get white solid sample, after high performan...

Embodiment 3

[0027] Get the total alkaloid powder of mulberry leaves and dissolve it in water to make the upper column liquid, which is adsorbed by the resin column of pretreated D152 resin. The inner diameter of the resin column is 1.5cm, and the length of the column is 60cm. 10. The processing capacity of the resin is 0.4 mg mulberry leaf total alkaloids / mL wet resin. After the adsorption is completed, it is eluted with 5% ethanol, and the elution flow rate is 0.5 mL / min. The eluate is collected in sections, and the collected The eluate was qualitatively detected, compared with the 1-deoxynojirimycin reference substance, and the single-component eluate at the same position and showing the same color spots as the 1-deoxynojirimycin reference substance was combined, concentrated under reduced pressure and Vacuum drying, then recrystallization with methanol / acetone (1:4), melting temperature 70°C, heating time 10min, natural cooling and static crystallization, repeated 2 times to obtain a wh...

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Abstract

The invention relates to the technology field of effective ingredient separation of the Chinese traditional medicine, particularly a method for separating 1-desoxy nojirimycin monomer from total alkaloid of mulberry leaf. The method comprises the steps as follows: preparing a sample solution; pretreating adsorbent and packing into a column; passing through the resin column at the room temperature; collecting eluates part by part; subjecting to the qualitative detection; mixing the eluates with the same composition; concentrating under the reduced pressure; vacuum-drying; and recrystallizing to obtain 1-desoxy nojirimycin crystals. According to the high-efficiency liquid chromatography measurement, the purity of the crystal is higher than 95% and the yield of the crystal is higher than 75%.

Description

technical field [0001] The invention relates to the technical field of separation of effective components of traditional Chinese medicine, in particular to a method for separating 1-deoxynojirimycin monomer from total alkaloids of mulberry leaves. Background technique [0002] Mulberry leaves were first recorded in "Shen Nong's Materia Medica". It tastes bitter, sweet, and cold in nature. It returns to the lung and liver meridian. It is recorded in Chinese medicine books of past dynasties that mulberry leaves can treat diabetes, and modern doctors often use mulberry leaves to treat diabetes, and have achieved satisfactory results. 1-deoxynojirimycin (1-deoxynojirimycin, DNJ) is one of the active ingredients in mulberry leaves for lowering blood sugar. Modern pharmacological studies have shown that it is a variety of α-glucosidase inhibitors in the human small intestine, which can prevent α-glucosidase from interacting with two The combination of sugars blocks the absorption...

Claims

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Application Information

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IPC IPC(8): C07D211/40
Inventor 欧阳臻孟夏常钰杨雨
Owner JIANGSU UNIV
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