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Method for preparing verbascoside standard product from callicarpa nudiflora leaf

A technology of acteoside and nude flower purple pearl, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of high manufacturing cost, undisclosed preparation methods of acteoside standard substances, complexity, etc., and achieve The effect of large mass transfer coefficient, high selectivity and mild operating temperature

Active Publication Date: 2015-04-22
JIANGXI POZIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the preparation of standard substances is often much more complicated than conventional analytical chemical reagents, often requires a variety of high-precision separation and purification steps (such as HPLC, etc.), and also causes its high manufacturing cost
[0006] In the prior art, although there are already verbascoside standard substances supplied, the preparation method of these verbascoside standard substances is not disclosed

Method used

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  • Method for preparing verbascoside standard product from callicarpa nudiflora leaf
  • Method for preparing verbascoside standard product from callicarpa nudiflora leaf
  • Method for preparing verbascoside standard product from callicarpa nudiflora leaf

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1. Preparation of verbascoside

[0024] The method for preparing and purifying verbascoside from the leaves of Auranthus nudiflora, the specific steps are as follows:

[0025] Weigh 1kg of Auranthus nudiflora leaves, dry and pulverize through an 80-mesh sieve, add 0.2kg of entraining agent (water: methanol: n-hexane: ammonia = 55%: 15%: 25%: 5 %), soaked for 12 hours, stirred evenly and added to the extraction kettle, the pressure in the kettle was set to 35MPa, using supercritical carbon dioxide extraction technology, after static extraction at a temperature of 30°C for 0.1 hour; then dynamically extracted 1.5 at 0.1L / min hour; collect and obtain 92.3 g of crude verbascoside (purity 82.1% as detected by HPLC).

[0026] Dissolve 50 g of the crude acteoside in 150 ml of methanol, add 150 ml of diethyl ether and refrigerate to obtain 38.8 g of it, and the purity of the actcoside is >99.5% as detected by HPLC. For the HPLC detection method, see Li Caitang et a...

Embodiment 2-3

[0028] Except technical parameter listed in the table below, other preparation methods are with embodiment 1

[0029]

[0030]

Embodiment 4

[0032] Stability test of pure verbascoside at room temperature

[0033] Randomly take the verbascoside sample prepared above, and place it at room temperature in the dark. After seven days, the measurement was carried out, and each point was measured 3 times, and the measurement results were used as the results of the stability test at room temperature. The test results are shown in the table below. From the test results, it can be seen that the verbascoside of the present invention is stable within one week at room temperature in the dark.

[0034] Room temperature storage stability test results (%)

[0035]

[0036] From the analysis of the above HPLC results, we have effectively separated and purified the crude verbascoside, reaching a purity of more than 99.5%, and the sample uniformity and stability are good, so it can be used as a standard substance. The above experimental results prove that the method for preparing verbascoside standard substance is stable, reliab...

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Abstract

The invention relates to a preparation method of verbascoside, particularly relates to a method for preparing a high-pure verbascoside product from callicarpa nudiflora by adopting a supercritical fluid extraction technique, and a use of the verbascoside product obtained by the preparation method as a standard substance. The supercritical fluid extraction technique adopts the following extraction conditions: the amount of an entrainer is 0.2-0.5 time of the raw material mass, soaking is carried out for 12-24 h, under the conditions of the pressure of 35 MPa and the temperature of 60-70 DEG C, static extraction is carried out for 0.1-0.5 h, and then dynamic extraction is carried out for 1.5-2 h at the speed of 0.1-1.0 L / min. The entrainer is composed of water, methanol, n-hexane and ammonia water with the volume percentage ratio of 55%:15%:25%:5%.

Description

technical field [0001] The present invention relates to a method for preparing verbascoside, in particular to a method for preparing a high-purity verbascoside product from A. nudiflora by means of supercritical fluid extraction technology, and the method for using the verbascoside product obtained by the preparation method as a standard substance. use. Background technique [0002] Verbacoside, also known as ergosteroside, is a phenylpropanoid monomer component that exists in plants of many families. Actascoside is a white needle crystal powder, easily soluble in ethanol, methanol or ethyl acetate, and its molecular formula is C 29 h 36 o 15 , the molecular weight is 624.59, the CAS number is 61276-17-3, and its structural formula is as follows: [0003] [0004] According to literature reports, verbascoside has obvious effects on nervous system and immune system, especially for senile diseases (senile dementia) and immune diseases (chronic nephritis). [0005] The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18C07H1/08
CPCC07H1/08C07H15/18Y02P20/54
Inventor 肖军平吴永忠康兴东陈梁周朝忠
Owner JIANGXI POZIN PHARMA
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