Method for extracting terpene compounds

Abstract

The invention discloses a method for extracting terpene compounds, which comprises the following steps: (1) dehydrating, drying and crushing pine needle leaves to obtain pine needle leaf powder; (2) performing steam distillation or supercritical CO2 extraction on the pine needle leaf powder obtained in the step (1) to obtain an extracting solution containing terpene compounds; (3) carrying out rotary evaporation or vacuum concentration on the extracting solution containing the terpene compound obtained in the step (2) to obtain a concentrated terpene compound; and (4) separating and purifying the concentrated terpene compound obtained in the step (3) by adopting a chromatographic separation method to obtain the terpene compound. According to the method provided by the invention, the terpene compounds in the pine needle leaf oil can be effectively concentrated and purified, the extraction, concentration and purification efficiency of the terpene compounds is improved, the cost is reduced, and the product quality and safety are ensured.

Description

Technical Field

[0001] The present application relates to a method for extracting terpene compounds, and belongs to the field of natural product chemistry. Background Art

[0002] Pine needles are rich in terpene compounds, which have wide application value in the fields of medicine, food, and spices. However, terpene compounds are usually highly volatile, which makes them easy to lose during the extraction and concentration process. In addition, many terpene compounds are sensitive to high temperatures and are prone to degradation or chemical changes. Based on the high volatility and strong heat sensitivity of terpene compounds, traditional extraction methods have problems such as low efficiency and large losses, and it is difficult to meet the requirements of high purity and high yield. Therefore, it is particularly important to develop an efficient and environmentally friendly extraction method. Summary of the invention

[0003] The purpose of the present invention is to provide a two-stage method for efficiently extracting terpene compounds from pine needles, which can significantly improve the extraction efficiency and purity of terpene compounds and reduce thermal degradation and oxidation losses.

[0004] In one aspect of the present application, a method for extracting terpene compounds is provided, the method comprising:

[0005] (1) dehydrating, drying, and crushing pine needles to obtain pine needle powder;

[0006] (2) subjecting the pine needle powder obtained in step (1) to steam distillation or supercritical CO2 extraction to obtain an extract containing terpene compounds;

[0007] (3) subjecting the extract containing terpene compounds obtained in step (2) to rotary evaporation or vacuum concentration to obtain concentrated terpene compounds;

[0008] (4) Separating and purifying the concentrated terpene compounds obtained in step (3) by a chromatographic separation method to obtain terpene compounds.

[0009] Optionally, in step (1),

[0010] The drying temperature is 25 to 70°C;

[0011] The moisture content of pine needles after drying is less than 10%;

[0012] The particle size of the pine needle powder is 0.5 to 1 mm.

[0013] Optionally, in step (2),

[0014] The method of the steam distillation comprises:

[0015] Mix pine needle powder with 5 to 10 times the amount of water for 3 to 6 hours, and distill it using steam distillation for 1 to 3 hours.

[0016] Optionally, in step (2),

[0017] The supercritical CO2 extraction method comprises:

[0018] The temperature of supercritical CO2 extraction is 35-40°C, the pressure is 15-25MPa, and the flow rate of CO2 is 10-20L / h.

[0019] Optionally, in step (3),

[0020] The parameters of the vacuum concentration include:

[0021] Vacuum degree is 0.05~0.1MPa;

[0022] The distillation temperature is 40-60°C.

[0023] Optionally, in step (4),

[0024] The chromatographic separation method includes at least one of column chromatography, high performance liquid chromatography, and gas chromatography.

[0025] Optionally, the column chromatography is selected from at least one of silica gel column chromatography and aluminum oxide column chromatography.

[0026] The beneficial effects of this application include:

[0027] 1) The method provided in the present application can effectively concentrate and purify terpene compounds in pine needle oil, improve the extraction, concentration and purification efficiency of terpene compounds, reduce costs, and ensure product quality and safety.

[0028] 2) The present application provides an efficient and environmentally friendly method for extracting terpene compounds from pine needles. By optimizing the extraction and purification process, the extraction efficiency and purity of terpene compounds are significantly improved, and the application prospect is broad. DETAILED DESCRIPTION

[0029] The present application is described in detail below with reference to embodiments, but the present application is not limited to these embodiments.

[0030] Unless otherwise specified, the raw materials in the examples of this application were purchased through commercial channels.

[0031] Example 1

[0032] 1. Take 5kg of pine needles, clean them, and dry them at below 70℃ to a moisture content of 8%.

[0033] 2. Grind the dried pine needles into 0.6 mm powder and put them into the extraction tank of the supercritical CO2 extraction device.

[0034] 3. Set the extraction temperature to 40°C, pressure to 20 MPa, CO2 flow rate to 15 L / h, and extraction time to 2 hours.

[0035] 4. The extraction product was decompressed to normal pressure to obtain 150 g of crude terpene extract.

[0036] 5. Transfer the crude terpene extract to a vacuum distillation apparatus, set the distillation temperature to 50°C and the vacuum degree to 0.08 MPa for distillation.

[0037] 6. Purify and collect using silica gel column chromatography to obtain 50 g of compound.

[0038] After testing and analysis, the purity of terpene compounds was 98%.

[0039] Example 2

[0040] 1. Take 5kg of pine needles, clean them, and dry them at below 60℃ until the moisture content is 10%.

[0041] 2. Grind the dried pine needles into 0.8 mm powder, mix the pine needle powder with 10 times the water for 6 hours, and distill it for 3 hours by steam distillation to obtain 150 g of crude terpene extract.

[0042] 4. Transfer the crude terpene extract to a vacuum distillation apparatus, set the distillation temperature to 40°C and the vacuum degree to 0.1 MPa for distillation.

[0043] 6. Purify and collect using silica gel column chromatography to obtain 50 g of compound.

[0044] After testing and analysis, the purity of terpene compounds is 99%.

[0045] The above are only a few embodiments of the present application and do not constitute any form of limitation to the present application. Although the present application is disclosed as above with preferred embodiments, it is not intended to limit the present application. Any technician familiar with the profession, without departing from the scope of the technical solution of the present application, using the technical content disclosed above to make slight changes or modifications are equivalent to equivalent implementation cases and fall within the scope of the technical solution.

Claims

1. A method for extracting terpene compounds, characterized in that: The method comprises: (1) dehydrating, drying, and crushing pine needles to obtain pine needle powder; (2) subjecting the pine needle powder obtained in step (1) to steam distillation or supercritical CO2 extraction to obtain an extract containing terpene compounds; (3) subjecting the extract containing terpene compounds obtained in step (2) to rotary evaporation or vacuum concentration to obtain concentrated terpene compounds; (4) Separating and purifying the concentrated terpene compounds obtained in step (3) by a chromatographic separation method to obtain terpene compounds.

2. The method according to claim 1, characterized in that In step (1), The drying temperature is 25 to 70°C; The moisture content of pine needles after drying is less than 10%; The particle size of the pine needle powder is 0.5 to 1 mm.

3. The method according to claim 1, characterized in that In step (2), The method of the steam distillation comprises: Mix pine needle powder with 5 to 10 times the amount of water for 3 to 6 hours, and distill it using steam distillation for 1 to 3 hours.

4. The method according to claim 1, characterized in that: In step (2), The supercritical CO2 extraction method comprises: The temperature of supercritical CO2 extraction is 35-40°C, the pressure is 15-25MPa, and the flow rate of CO2 is 10-20L / h.

5. The method according to claim 1, characterized in that In step (3), The parameters of the vacuum concentration include: Vacuum degree is 0.05~0.1MPa; The distillation temperature is 40-60°C.

6. The method according to claim 1, characterized in that In step (4), The chromatographic separation method includes at least one of column chromatography, high performance liquid chromatography, and gas chromatography.

7. The method according to claim 6, characterized in that The column chromatography is selected from at least one of silica gel column chromatography and aluminum oxide column chromatography.