Process of extracting 1-deoxy nojirimycin

A technology of deoxynojirimycin and mulberry leaf extract, which is applied in the direction of pharmaceutical formulations, medical preparations containing active ingredients, plant raw materials, etc., can solve the problems of cumbersome process, inconvenient operation, and high cost, and achieve cost reduction and operation Simple, content-enhancing effect

Inactive Publication Date: 2007-08-22
ZHEJIANG UNIV
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

[0004] The existing mulberry leaf 1-deoxynojirimycin (DNJ) extraction method mainly contains two kinds, the content of the mulberry leaf extract 1-deoxynojirimycin obtained by the method of CN1579445A is only 1.0~3.0%, mainly by adding flocculation The agent is obtained after alcohol precipitation; the method of CN1430964A has obtained high-content total alkaloids of mulberry leaves and DNJ extract, but the process is cumbersome, and it needs to be extracted in the pretreatment process and then concentrated to the extract to a specific gravity of 1.12-1.20. Then add 1-5 times the amount of the original drug to dissolve in water, adjust the pH and then add flocculant to stand for 12 hours, and the subsequent separation process is also after the ion exchange resin is used to remove impurities, the resin needs to be poured out and placed in alkali Reflux extraction after 4 hours, many steps, inconvenient operation, high cost of industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The preparation of embodiment 1 mulberry leaf extract

[0016] Take about 200g of mulberry leaves and crush them, add 3 liters of water, reflux for extraction for 2.5 hours, filter the filter residue, add 3 liters of water and reflux for 2 hours, and combine the filtrates to make a total of 5.2L. The extract was acidified with 6N hydrochloric acid to pH 1~3, then refrigerated at -8°C for 2 hours, filtered to remove the precipitate, the filtrate was concentrated to 2L, passed through cation exchange resin 001×1.1, washed with water until colorless, and then added ammonia water to 50 % ethanol aqueous solution to make the content of ammonia water reach 50% for elution, collect this part of the eluate, concentrate it into an extract to obtain 1.8g, and measure the content of 1-deoxynojirimycin by HPLC method to be 11.8%.

Embodiment 2

[0017] Example 2 Preparation of Mulberry Leaf Extract

[0018] Take about 500 grams of medicinal materials and grind them, add 5 liters of 30% methanol to reflux for extraction for 2 hours, filter the filter residue and add 4 liters of 30% ethanol to reflux for 2 hours, and combine the filtrates to make a total of 8.2L. Acidify the extract with 5N sulfuric acid to pH 1~3, refrigerate at -15°C for 2 hours, filter to remove the precipitate, concentrate the filtrate to 5L, pass it through cation exchange resin 001×7, wash with water until neutral, and then wash with 30% methanol To colorless, then add diethylammonia to 70% methanol aqueous solution to make the content reach 20% to elute, collect this part of the eluate, concentrate it into an extract to obtain 4.1g, and measure the content of 1-deoxynojirimycin by HPLC was 13.1%.

Embodiment 3

[0019] Example 3 Preparation of Mulberry Leaf Extract

[0020] Take about 1kg of mulberry leaves and crush them, add 8 liters of 20% acetone, and reflux for 2.5 hours. After filtering, add 8 liters of 20% acetone to reflux for 2 hours, and combine the filtrates to make a total of 12.6L; Phosphoric acid was acidified to pH 1~3 and refrigerated at -30°C for 2 hours, filtered to remove the precipitate, the filtrate was concentrated to 6L and then passed through a cation exchange resin 001×14.5, washed with water until neutral, then washed with 60% acetone until colorless, and then added di Ethyl ammonia was added to 60% methanol aqueous solution to make the content reach 30% for elution, and this part of the eluate was collected and concentrated into an extract to obtain 9.6 g. The content of 1-deoxynojirimycin was determined by HPLC to be 12.6%.

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Abstract

The present invention is process of extracting 1-deoxy nojirimycin (DNJ) from mulberry leaf. Mulberry leaf extract is treated with inorganic acid, cooled to eliminate impurity and column chromatographically separated to obtain DNJ. Animal experiment of mouse shows that the mulberry leaf extract has obvious blood sugar reducing effect, so that the present invention may be used in preparing blood sugar reducing health product. The present invention has low preparation cost, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of plant extraction, in particular to an extract of active ingredients of mulberry leaves and a preparation method thereof. Background technique [0002] Mulberry leaves are called "immortal leaves" in "The Classic of Materia Medica", which has the effects of nourishing yin and blood, dispelling wind and heat dissipation, benefiting liver and ventilating, reducing blood pressure and diuresis. The pharmacological effects of mulberry leaves are recorded in the bibliographies such as "Compendium of Materia Medica", "Seeking the Truth of Materia Medica", "Diet Therapy Materia Medica", "Medicinal Tea and Medicinal Dew", "Chinese Medicine Prescriptions", and the ancient Japanese book "Eating Tea for Health". It is recorded that mulberry leaves have the effect of improving "drinking water disease" (ie diabetes). It can be seen that the medicinal value and health care function of mulberry leaves have a long history whether i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/40A61K31/445A61K36/605A61P3/10A61K127/00
Inventor 周长新莫建霞翁林佳肖昌钱张相宜
Owner ZHEJIANG UNIV
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