Preparation method of robinin-7-O-glucuronide

A technology of glucuronide and acacia can be used in the preparation of sugar derivatives, chemical instruments and methods, medical preparations containing active ingredients, etc. short, simple effects

Inactive Publication Date: 2017-05-31
石河子大学医学院第一附属医院
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Problems solved by technology

[0009] At present, there is no commercially available pure locust-7-O-glucuronide, and its pharmacological activity has not been reported

Method used

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  • Preparation method of robinin-7-O-glucuronide

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preparation example Construction

[0029] The preparation method of acaciacin-7-O-glucuronide provided by the present invention comprises the steps of obtaining the extract of Cymbidium chinensis, further chromatography and HPLC preparation of the extract. The method provided by the present invention will be described in detail below in conjunction with the accompanying drawings.

[0030] Such as figure 1 As shown, firstly, the dry aerial part of 1 part by weight of Cymbidium is pulverized, and extracted by percolation with 40-75 vol% ethanol solution in 30-40 times by weight. Then, the extract is concentrated, for example, the method of concentrating under reduced pressure can be used, and the extract is in the form of paste after concentration. Then the paste is dried, for example, the paste can be made into extract powder by vacuum drying.

[0031] The extract powder was subjected to polyamide column chromatography. The steps of chromatography can be as follows: dissolve the extract powder with high-conce...

Embodiment 1

[0037] Embodiment 1: The method for extracting and isolating acaciacetin-7-O-glucuronide from sweet green orchid is carried out according to the following steps:

[0038] a. Grinding the dried aerial part of the orchid, soaking it with 5 times the amount of 40% ethanol for 12 hours to obtain an extract;

[0039] b. Using the percolation method, the ratio of 3 kg of Chinese orchid medicinal material to 40% ethanol is 1:30, the flow rate is 1 mL / min, and the ethanol percolation liquid of 15 times the amount before is collected;

[0040] c. The percolate is filtered once with a mesh with a pore size of 0.1 mm, and the filtrates are combined;

[0041] d. Using a decompression concentration device, at a pressure of 0.08Mpa and a temperature of 30°C, the ethanol was distilled off to obtain a thick extract of 0.8g / mL; after drying in a water bath, 250g of extract powder was obtained;

[0042] e. Dissolve 100g of extract powder in 70% ethanol and dry mix the sample, apply 100-200 mes...

Embodiment 2

[0055] Embodiment 2: The method for extracting and isolating acaciacetin-7-O-glucuronide from sweet green orchid is carried out according to the following steps:

[0056] a. Crush the dried aboveground part of Cymbidium, soak in 10 times the amount of 75% ethanol for 24 hours;

[0057] b. Using the percolation method, the ratio of 4kg of Chinese orchid medicinal material to 75% ethanol is 1:40, the flow rate is 6mL / min, and 15 times the ethanol percolation fluid before collection;

[0058] c, the percolation liquid is filtered 5 times with a mesh with an aperture of 10mm, and the filtrates are combined;

[0059] d. Using a vacuum concentration device, under pressure: 0.1Mpa, temperature: 60°C, distill and remove ethanol to obtain 1.2g / mL thick extract; after drying in a water bath, obtain extract powder 305g;

[0060] e. Dissolve 100g of extract powder in 70% ethanol and dry mix the sample, apply 100-200 mesh polyamide for column chromatography, 30-75% ethanol 80000mL gradien...

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Abstract

The invention relates to a method for obtaining robinin-7-O-glucuronide through extraction and separation from Dracocephalum moldavica. The method is characterized by comprising the following steps: smashing the dry overground part of the Dracocephalum moldavica, obtaining a percolating solution through collection and extraction by adopting a percolating method, and obtaining a thick extract through vacuum concentration; and obtaining extract powder after water-bath drying. The extract powder is stirred by adopting a dry method after being dissolved with high concentration alcohol, polyamide column and ODS column chromatography is carried out, and after elution, an eluant is evaporated to dryness to obtain a white crystal, namely compound robinin-7-O-glucuronide, through a reduced pressure distillation device.

Description

technical field [0001] The invention relates to a method for extracting and isolating acaciacetin-7-O-glucuronide from sweet green orchid. Background technique [0002] Liu Jinqi (Research on the chemical constituents of Gongju [J]. Chinese Journal of Traditional Chinese Medicine, 2001, 26(8): 547-548.) reported for the first time the structure of locustine-7-O-glucuronide isolated from Gongju plant, The process uses extraction, silica gel column chromatography, polyamide column chromatography, recrystallization and other technologies to separate and obtain 200 mg of acaciacin-7-O-glucuronide from 2.5 kg of chrysanthemum chrysanthemum. The operation is complicated and the steps are cumbersome. [0003] The structural formula of locust-7-O-glucuronide is: [0004] [0005] Yang Jianbo (Study on the chemical constituents of Artemisia chinensis [J]. Chinese herbal medicine, 2008, 39(8): 1125-1127.) using ethanol reflux extraction, extraction, silica gel column, polyamide co...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
CPCA61K31/7048C07H1/08C07H17/07
Inventor 王新春袁勇邢建国赵洁王晓义陈卫军黄川生
Owner 石河子大学医学院第一附属医院
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