Preparation method of atractylenolide I

A technology of Atractylodes lactone and Atractylodes atractylodes, applied in the field of natural medicinal chemistry, can solve the problems of serious pollution, low yield, and large amount of reagents, and achieve the effects of large preparation, simple operation, and environmental friendliness

Inactive Publication Date: 2013-08-21
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Preparation of Angelica lactone I by conventional column for separation, low yield, large amount of reagents, serious pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Atractylodes rhizome raw material was pulverized, weighed 3kg, ultrasonically extracted with 15L 80% methanol solution for 30 minutes each time, extracted 3 times, the extract was concentrated under reduced pressure to 500ml, added an equal volume of chloroform for extraction 3 times, combined the extracts and recovered the chloroform to obtain the extract. Take chloroform, methanol, and water and mix them according to 5:2:3. After fully layering, take the upper phase and fill the high-speed countercurrent chromatography tube as the stationary phase, turn on the main engine at a speed of 800 rpm, and pump the lower phase into the flow phase at the same time. After the dynamic equilibrium is established, the flow rate is adjusted to 2ml / min, the extract is dissolved with the mobile phase, the sample is injected by the injection valve, the ultraviolet detector is monitored online, the target component is collected, the preparation is continuous, the fraction is recovered to...

Embodiment 2

[0016] The Atractylodes Rhizome raw material was pulverized, weighed 3kg, extracted twice with 30L 90% methanol solution ultrasonically for 30 minutes each time, the extract was concentrated under reduced pressure to 800ml, added an equal volume of chloroform for extraction twice, combined the extracts and recovered the chloroform to obtain the extract. Take chloroform, methanol, water, mix according to 10:4:7, after fully layering, take the upper phase and fill the high-speed countercurrent chromatography tube as the stationary phase, turn on the main engine at a speed of 900rpm, and pump the lower phase into the flow phasing at the same time, After the dynamic balance is established, the flow rate is adjusted to 3ml / min, the extract is dissolved with the mobile phase, the sample is injected by the injection valve, the ultraviolet detector is monitored online, the target component is collected, the preparation is continuous, and the fraction is recovered to obtain the atractylo...

Embodiment 3

[0018] The raw material of Atractylodes macrocephala was crushed, weighed 3kg, extracted twice with 20L85% methanol solution ultrasonically for 30 minutes each time, the extract was concentrated under reduced pressure to 700ml, added an equal volume of chloroform for extraction twice, combined the extracts and recovered the chloroform to obtain the extract. Take chloroform, methanol, and water, and mix them according to 7:3:6. After fully layering, take the upper phase and fill the high-speed countercurrent chromatography tube as the stationary phase, turn on the main engine at a speed of 750rpm, and pump the lower phase into the flow phase at the same time. After the dynamic balance is established, the flow rate is adjusted to 2ml / min, the extract is dissolved with the mobile phase, the sample is injected by the injection valve, the ultraviolet detector is monitored online, the target component is collected, the preparation is continuous, the fraction is recovered to obtain the...

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PUM

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Abstract

The invention discloses a preparation method of atractylenolide I, which is simple in operation and small in pollution. The method comprises the following steps: taking and crushing a bighead atractylodes rhizome raw material, adding a 70-100% methanol solution with an addition amount 5-10 times as large as the amount of the raw material into the raw material, and carrying out ultrasonic extraction on the obtained mixture 2-3 times; after an extracting solution is concentrated, carrying out extraction on the obtained product by using a chloroformic solution, collecting extract liquor and recovering a reagent, separating a concentrated solution again by using a high-speed countercurrent chromatograph, carrying out on-line monitoring on the obtained object by using an ultraviolet detector, and carrying out fraction collection and decompressed drying on the obtained product. In the preparation of atractylenolide I implemented by using the method, products are high in purity, and easy to realize industrialization amplification.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a preparation method of atractyloid I. Background technique [0002] Atractylodes lactone I, CAS73069-13-3, molecular formula C 15 h 18 o 2 , the molecular weight is 230.3, and the molecular structure formula is as follows: [0003] . [0004] Atractylodes lactone I is a lactone component in Atractylodes macrocephala, which has strong functions of enhancing salivary amylase activity, promoting intestinal absorption, regulating intestinal tract, and inhibiting tumor growth. [0005] The existing preparation method of Atractylodes lactone I mostly adopts silica gel column preparation. For example, in the literature "Chemical Components of Atractylodes Rhizoma Atractylodes Rhizoma and Anti-tumor Experimental Research", the method uses steam distillation to extract the volatile oil of Atractylodes Rhizoma Atractylodes Rhizome, and conventional silica gel column chrom...

Claims

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Application Information

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IPC IPC(8): C07D307/92
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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