# US 7,608,741 B2 · Mass separation method of magnolol from Magnoliae cortex radix

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- Number: US 7,608,741 B2
- Document ID: US7608741B2
- Status: Granted
- Kind: B2
- Application number: 11/915,721
- Filed: 2005-06-21
- Published: 2008-08-07
- Granted: 2009-10-27
- Earliest claimed: 2005-05-30
- Assignees: Korea Institute of Oriental Medicine
- Inventors: Jin Sook Kim; Yun Mi Lee; Dae Sik Jang
- Web page: https://patentgrep.com/patent/US7608741B2

## CPC

- C07C 37/82: by solid-liquid treatment; by chemisorption
- A61P 1/08: for nausea, cinetosis or vertigo; Antiemetics
- A61P 1/12: Antidiarrhoeals
- A61P 11/10: Expectorants
- A61P 17/02: for treating wounds, ulcers, burns, scars, keloids, or the like
- C07C 37/004: {by obtaining phenols from plant material or from animal material}
- C07C 37/685: {Processes comprising at least two steps in series}
- C07C 37/84: by crystallisation
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- A61P: SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS

## Abstract

The present invention related to method for the mass separation of magnolol from Magnoliae cortex or Magnoliae radix. The method comprises the steps of: 1) crushing Magnoliae cortex or Magnoliae radix, extracting the crushed material with organic solvent, adding n-hexane to the extract so as to obtain a n-hexane layer; 2) concentrating the n-hexane layer in a water bath at a temperature of 30-40° C. and a revolution speed of 40-200 RPM under reduced pressure so as to form a crude crystal; and 3) removing the n-hexane from the crude crystal, completely dissolving the crude crystal in chloroform, adding n-hexane to the n-hexane-containing solution, and leaving the solution to stand at room temperature so as to recrystallize the solution. In the method, a column chromatography step which is necessarily carried out in the general separation process is omitted so that separation process steps are reduced, leading to a saving in separation time. Also, expensive equipment is not required, leading a reduction in separation cost. Accordingly, the method is effective for the mass separation of expensive magnolol.

## Claims

### Claim 1

A method for a mass separation of magnolol from Magnoliae cortex or Magnoliae radix comprising the steps of:
1) crushing Magnoliae cortex or Magnoliae radix, extracting the crushed material with organic solvent, adding n-hexane to the extract so as to-obtain a n-hexane layer;
2) concentrating the n-hexane layer in a water bath at a temperature of 30-40° C. and a revolution speed of 40-200 RPM under reduced pressure so as to form a crude crystal; and
3) removing the n-hexane from the crude crystal, completely dissolving the crude crystal in chloroform, adding n-hexane to the solution, and leaving the n-hexane-containing solution to stand at room temperature so as to recrystallize the solution,
wherein the mass separation does not include a column chromatography step.

### Claim 2 (depends on 1)

The method of claim 1, wherein the organic solvent in the step 1) is water-soluble alcohol.

### Claim 3 (depends on 1)

The method of claim 1, wherein the n-hexane in the step 1) is substituted with one among petroleum ether, chloroform and dichloromethane.

### Claim 4 (depends on 1)

The method of claim 1, wherein the step 3) is repeated in order to obtain a crystal with higher purity.

### Claim 5 (depends on 1)

The method of claim 1, wherein said mass separation does not utilize a supercritical extractor or HPLC.

### Claim 6

A method for the mass separation of magnolol from Magnoliae cortex or Magnoliae radix consisting of:
1) crushing Magnoliae cortex or Magnoliae radix, extracting the crushed material with organic solvent, adding n-hexane to the extract so as to obtain a n-hexane layer;
2) concentrating the n-hexane layer in a water bath at a temperature of 30-40° C. and a revolution speed of 40-200 RPM under reduced pressure so as to form a crude crystal; and
3) removing the n-hexane from the crude crystal, completely dissolving the crude crystal in chloroform, adding n-hexane to the solution, and leaving the n-hexane-containing solution to stand at room temperature so as to recrystallize the solution.