Preparation method for purifying essential oil and ursolic acid from wild ledum palustre in great khingan

A technology of ursolic acid and essential oils, applied in the directions of essential oils/fragrance, fat production, bulk chemical production, etc., can solve the problems of unstable product quality, high operating temperature, easy decomposition of heat-sensitive substances, etc.

Active Publication Date: 2013-04-17
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The domestic general steam distillation method to extract essential oils has disadvantages such as high operating temperature, easy decomposition of heat-sensitive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: a kind of supercritical carbon dioxide extraction is adopted and coupled with molecular distillation technology, ultrasonic extraction is combined with column chromatography again, obtains the method for two kinds of compositions of essential oil, ursolic acid respectively, and its steps are as follows:

[0016] (1) 1000g of Ledum leaves were crushed to 40 mesh, extracted with supercritical carbon dioxide, extraction pressure 10Mpa, at 40°C, time 4h, CO 2 The flow rate is 1L / h, recovering CO 2 , to obtain crude essential oil;

[0017] (2) With a wiped-film molecular still, adopt two-stage separation, the first-stage distillation pressure is 3 Pa, distill at 1ml / min feed rate, wiped-film rotating speed 200r / min, and the distillation temperature is 90°C; the second-stage distillation pressure is 8 Pa, distilled at a feed rate of 1.2ml / min, a wiper speed of 250r / min, and a distillation temperature of 100°C to remove the odor of the essential oil, further pur...

Embodiment example 2

[0022] Implementation case 2: A method for obtaining two components of essential oil and ursolic acid respectively by using supercritical carbon dioxide extraction and coupling with molecular distillation technology, ultrasonic extraction and column chromatography, the steps are as follows:

[0023] (1) 1000g of Ledum leaves were crushed to 40 mesh, extracted with supercritical carbon dioxide, at 45°C, extraction pressure 12Mpa, time 5h, CO 2 The flow rate is 1.5L / h, recovering CO 2 , to obtain crude essential oil;

[0024] (2) With a wiped-film molecular still, adopt two-stage separation, the first-stage distillation pressure is 5 Pa, distill at 1.2ml / min feed rate, wiped-film rotating speed 280r / min, and the distillation temperature is 95°C; the second-stage distillation pressure 9 pa, distill at a feed rate of 1.5ml / min, a wiper speed of 300r / min, and a distillation temperature of 105°C to remove the odor of the essential oil, further purify, collect the essential oil, and...

Embodiment example 3

[0029] Implementation Case 3: A method for obtaining two components of essential oil and ursolic acid respectively by using supercritical carbon dioxide extraction and coupling with molecular distillation technology, ultrasonic extraction and column chromatography, the steps are as follows:

[0030] (1) 1000g of Ledum leaves were crushed to 60 mesh, extracted with supercritical carbon dioxide, at 45°C, extraction pressure 15Mpa, time 6h, CO 2 The flow rate is 2L / h, recovering CO 2 , to obtain crude essential oil;

[0031] (2) With a wiped-film molecular still, adopt two-stage separation, the first-stage distillation pressure is 6 Pa, distill at 1.5ml / min feed rate, wiped-film rotating speed 300r / min, and the distillation temperature is 95°C; the second-stage distillation pressure 10 Pa, distill at a feed rate of 2.0ml / min, a wiper speed of 360r / min, and a distillation temperature of 100°C to remove the odor of the essential oil, further purify, collect the essential oil, and ...

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PUM

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Abstract

The invention belongs to the field of natural organic chemistry, and discloses a method. The method has the advantages that 1, a supercritical CO2 extraction technology is adopted; a system is sealed in an extraction process; destroy of small-molecule volatile oil is avoided; the whole essential oil extraction process is conducted at an approximate room temperature; the activity loss is very little; 2, a molecular distillation technology is adopted for purifying essential oil; an operating temperature is far below a boiling temperature of a substance at atmospheric pressure; in addition, the heating time is very short; the substance cannot be destroyed; the separation and purification degree and the yield of the essential oil are high; and 3, ultrasonic extraction is conducted, so that the heating time of effective components is shortened; the bioactivity is high; a silica gel column chromatography purification technology can ensure that the purity of ursolic acid is further increased; the operation is simple and easy; and the production cost is lowered greatly. With the adoption of the method, the extraction time is shortened greatly; an extraction speed is increased; in addition, a purification effect is obvious; contents of the effective components are high; the essential oil and ursolic acid can be obtained simultaneously; the relative content of the essential oil reaches 77.4%; and the purity of ursolic acid is increased to 98.73%.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for extracting Ledum essential oil and ursolic acid from Daxinganling wild Ledum, in particular to a method for extracting with supercritical carbon dioxide and coupling with molecular distillation technology, ultrasonic extraction and recombination The method of column chromatography obtains the method for two kinds of components of essential oil and ursolic acid respectively. Background technique: [0002] Duxiang is a small evergreen shrub belonging to Rhododendronaceae, with a height of more than 50 cm, many branches, thin branches, slightly thick leaves, dense and alternate, strong fragrance, narrow linear, 2-4 cm long, wide 1.5-3 mm. Ledum is shade-tolerant, likes water and humidity, and has low requirements on soil. It often grows in river valleys or mossy swamps, and grows in groups in patches. This species is mainly distributed in the temperate zone or ...

Claims

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Application Information

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IPC IPC(8): C11B9/02C07J63/00
CPCY02P20/54
Inventor 张亚红姚德坤姚德利万莉
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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