WO2023237058A1 - Method for removing free fatty acids from ganoderma spore powder - Google Patents

Abstract

A method for removing free fatty acids from a Ganoderma spore powder, the method comprising the following steps: carrying out wall-breaking and granulation on the Ganoderma spore powder; adding same into an extraction kettle of a supercritical CO 2 extraction device, with an extraction pressure of 12-25 MPa, an extraction temperature of 35-55ºC, and a flow of CO 2 of 50-90 L/h; controlling the pressure of a separation kettle I to be 7-12 MPa and the temperature to be 35-55ºC; controlling the pressure of a separation kettle II to be 4-6 MPa and the temperature to be 25-45ºC; carrying out extraction, with an extraction time of 0.5-3 h; and taking out an extract after extraction is completed.

Description

A method for removing free fatty acids from Ganoderma lucidum spore powder Technical field

The invention belongs to the field of Ganoderma lucidum processing, and specifically relates to a method for removing free fatty acids from Ganoderma lucidum spore powder.

Background technique

Ganoderma lucidum is a fungus with both medicinal and edible uses. It has always been known as "Ruicao" and "Xiancao" and has a history of thousands of years in my country. Modern scientific research shows that Ganoderma lucidum contains a variety of active ingredients, such as ganoderic acid, ergosterol, polysaccharides, etc. Ganoderma spore powder, as the germ cells ejected during the mature stage of Ganoderma lucidum, contains all the genetically active substances of Ganoderma lucidum, and its active ingredients can be said to be much higher than those of Ganoderma lucidum. Ganoderma spore powder contains sugars, peptides, triterpenes, sterols, alkaloids, vitamins, fatty acids and other active ingredients. Over the years, domestic and foreign research institutions have confirmed that Ganoderma spore powder has the ability to enhance human immunity, Anti-cancer, lowering blood lipids, lowering blood sugar, protecting liver and many other effects.

Because Ganoderma spore powder has two layers of outer walls made of chitin, it is difficult to be digested and absorbed by the human body. It requires the cooperation of gastric acid and biological enzymes in the body to slowly dissolve it. Therefore, it takes a long time for the human body to absorb the effective intracellular contents. Active ingredients. However, because the Ganoderma spore powder stays in the human body for a short time and the outer wall has no time to be dissolved, the absorption rate of the active ingredients is greatly reduced. Therefore, it is necessary to break the chitin outer wall so that the active ingredients in the broken Ganoderma spore powder can be digested, absorbed and utilized by the human body to the greatest extent.

The oil content in Ganoderma spore powder is about 30%. The Ganoderma spore oil in the Ganoderma spore powder is exposed after the wall is broken. When the oil is placed in the air, it will be decomposed by oxygen, moisture, light or microorganisms, producing relatively small molecular weight. Carboxylic acids, aldehydes or ketones produce unpleasant odors and some products harmful to human health, which is called rancidity of oils. Compared with other oil components, free fatty acids have worse oxidative stability and are more prone to rancidity. Therefore, the broken Ganoderma spore powder is easily affected by factors such as oxygen, moisture, and light, resulting in reduced edible quality of Ganoderma spore powder and shortened storage time. In addition, free fatty acids will be transferred into the oil during the extraction process of Ganoderma lucidum spore oil, which will reduce the quality of the oil, and the storage time will also affect the quality of the oil. shorten.

As a "green" extraction technology, the principle of supercritical CO ₂ extraction technology is to control the pressure and temperature beyond the critical point of the substance itself, so that it can selectively dissolve components with different polarities, boiling points and molecular weights. Compared with traditional enzymatic or molecular distillation methods for removing free fatty acids, the method of the present invention has the following advantages: ① Free fatty acids can be removed by supercritical _CO2 at low temperatures, avoiding the impact of high temperatures on heat-sensitive substances in Ganoderma spore powder, Retain the activity of the active ingredients to the maximum extent; ② There will be no consumption and residue of chemical substances during the removal process, and the extraction agent is safe, non-toxic and easy to recycle; ③ The process is simple, high efficiency and low energy consumption. There are currently no reports utilizing this technology for the removal of free fatty acids.

Contents of the invention

The purpose of the present invention is to overcome the above-mentioned shortcomings and provide a safe, efficient, simple process, and high-temperature-avoiding supercritical CO ₂ extraction method for removing free fatty acids from Ganoderma lucidum spore powder.

The purpose of the present invention is achieved in the following ways:

A method for removing free fatty acids from Ganoderma lucidum spore powder includes the following steps:

1) Break the walls of Ganoderma lucidum spore powder, with a wall breaking rate of more than 95%, and granulate;

2) Put the particles obtained in step 1) into the extraction kettle of the supercritical CO ₂ extraction device, the extraction pressure is 12-25Mpa, the extraction temperature is 35-55°C, and the CO ₂ flow rate is 50-90L/h;

3) Control the pressure of the separation kettle I to 7~12MPa and the temperature to 35~55℃;

4) Control the pressure of the separation kettle II to 4~6MPa and the temperature to 25~45℃;

5) The extraction time is 0.5 to 3 hours. After the extraction is completed, the extract is taken out to obtain spore powder with free fatty acids removed.

In the above-mentioned method of removing free fatty acids from Ganoderma spore powder, the granulation method in step 1) is: the weight ratio of Ganoderma spore powder and water is 1:0.5~1:1.5, the particle size of the particles is 0.5~10mm, and drying The temperature is 50~80℃, and the moisture content of Ganoderma spore powder particles is controlled at 3~10%.

Preferably, the extraction pressure in step 2) is 18-22MPa, the extraction temperature is 50-55°C, and the CO ₂ flow rate is 50-80L/h. Further preferably, the extraction pressure in step 2) is 18MPa, the extraction temperature is 50°C, and the CO ₂ flow rate is 80L/h.

Preferably, the pressure of the separation tank I in step 3) is 7.5-8MPa, and the temperature is 45-50°C. Further preferably, the pressure of the separation tank I in step 3) is 8MPa, and the temperature is 50°C.

Preferably, the pressure of the separation kettle II in step 4) is 4-5MPa, and the temperature is 30-35°C. Further preferably, the pressure of the separation kettle II in step 4) is 4MPa, and the temperature is 30°C.

Preferably, the extraction time in step 5) is 1.5-2h. Further preferably, the extraction time in step 5) is 1.5h.

The inventor found that the ability of _CO2 to dissolve substances is closely related to the temperature and pressure where it is located. The present invention controls the extraction pressure to 12-25Mpa, the extraction temperature to 35-55°C, especially under the conditions of the extraction pressure of 18-22MPa, the extraction temperature of 50-55°C, and the CO ₂ flow rate of 50-80L/h, so that The CO ₂ in the extraction kettle is in a supercritical state and the density is not too high. In this way, the CO ₂ dissolves free fatty acids in a targeted manner and avoids the extraction of a large amount of oil. The mixture in the supercritical region is then allowed to pass through the separation kettle I for further changes. Pressure, let the density of supercritical CO ₂ drop sharply, reduce the solubility of free fatty acids, and achieve the purpose of separation. Finally, by changing the pressure and temperature of the separation kettle II, other substances with smaller molecular weights can be separated, while the CO ₂ fluid sublimates. After recycling.

Comparing the beneficial effects of the present invention with the existing technology: the present invention uses a supercritical CO ₂ extraction device to remove free fatty acids from Ganoderma lucidum spore powder. The process is simple, and the CO ₂ used is safe and non-toxic, and can be completely volatilized without causing pollution to the product. At the same time, avoiding high temperatures can retain the activity of the active ingredients in Ganoderma spore powder to the maximum extent, and can effectively remove free fatty acids in Ganoderma spore powder.

Detailed ways

The present invention will be further described below with reference to specific examples, but is not limited thereto.

The following examples were all performed in a supercritical CO ₂ extraction device, which was purchased from Jiangsu Nantong Huaan Supercritical Extraction Co., Ltd., model HA220-50-06-C.

The following examples use the acid value as the evaluation criterion for whether to remove free fatty acids, and measure it according to the method specified in the national standard GB 5009.229-2016 "National Food Safety Standard for Determination of Acid Value in Foods".

The detection of the active ingredient polysaccharide is in accordance with the "Announcement of the State Administration for Market Regulation, National Health Commission and State Administration of Traditional Chinese Medicine on the Release of the Catalog of Five Health Food Raw Materials including Coenzyme Q10" No. 54 Annex 2 "Health Food Raw Material Catalog Broken Ganoderma Spore Powder" Measured by the method specified in 》. Total triterpenes were determined according to the methods specified in the "Technical Guiding Principles for Inspection and Evaluation of Physical, Chemical and Hygienic Indicators of Health Foods" (2020 Edition).

Example 1

Weigh 2kg of broken Ganoderma lucidum spore powder (wall breaking rate 98%, detected acid value 4.84mg/g, polysaccharide content 1.92%, total triterpene content 2.71%), add 2kg water to make particles with a particle size of 2mm , dried at 70°C to obtain 1.95kg of broken Ganoderma spore powder particles, and the moisture content of the Ganoderma spore powder particles was controlled at 3%. The prepared particles are loaded into the extraction kettle of the supercritical CO ₂ extraction device. The loading amount is 1.6kg. The extraction pressure is 18MPa and the temperature is 50°C. The pressure of the separation kettle I is 8MPa and the temperature is 50°C. The pressure of the separation kettle II is 4MPa, temperature 30°C; CO ₂ flow rate 80L/h, extraction 1.5h. Take out the Ganoderma lucidum spore powder in the extraction kettle, and the acid value is 0.29mg/g, the polysaccharide content is 1.91%, and the total triterpene content is 2.69%. The material in the separation kettle I is released to be 35.81g, and the acid value is 24.21mg/g. The material in the separation kettle II was released to be 9.2g, and the acid value was detected to be 7.5mg/g.

Example 2

Weigh 6kg of broken Ganoderma lucidum spore powder (wall breaking rate 98%, detected acid value 5.26mg/g, polysaccharide content 1.97%, total triterpene content 2.76%), add 3.6kg water to make a particle size of 1.18mm The particles were dried at 65°C to obtain 5.88kg of broken Ganoderma spore powder particles, and the moisture content of the Ganoderma spore powder particles was controlled at 3%. The prepared particles are loaded into the extraction kettle of the supercritical CO ₂ extraction device. The loading amount is 2.4kg. The extraction pressure is 20MPa and the temperature is 45°C. The pressure of the separation kettle I is 8MPa and the temperature is 50°C. The pressure of the separation kettle II is 5MPa, temperature 35°C; CO ₂ flow rate 60L/h, extraction 1.5h. Take out the Ganoderma lucidum spore powder in the extraction kettle, and the acid value is 0.45 mg/g, the polysaccharide content is 1.95%, and the total triterpene content is 2.75%. The material in the separation kettle I is released to be 51.17g, and the acid value is 21.88 mg/g. The material in the separation kettle II was discharged to 14.37g, and the acid value was detected to be 6.37mg/g.

Example 3

Weigh the same batch of particles in Example 2 and put them into the extraction kettle of the supercritical CO ₂ extraction device. The loading amount is 2kg. The extraction pressure is 18MPa and the temperature is 45°C; the pressure of the separation kettle I is 7.5MPa and the temperature is 45°C. Ⅱ The pressure is 4MPa, the temperature is 30°C; the CO ₂ flow rate is 70L/h, and the extraction is carried out for 2 hours. Take out the Ganoderma lucidum spore powder in the extraction kettle, and the acid value is 0.37mg/g, the polysaccharide content is 1.96%, and the total triterpene content is 2.75%. The material in the separation kettle I is released to be 47.35g, and the acid value is 20.3mg/g. The material in the separation kettle II was discharged to 10.7g, and the acid value was detected to be 6.92mg/g.

Example 4

Weigh 2kg of broken Ganoderma spore powder (wall breaking rate 99%, detected acid value is 4.93mg/g, polysaccharide content is 2.03%, total triterpene content is 2.82%), add 1.6kg water to make 4mm particle size The particles were dried at 65°C to obtain 1.94kg of broken Ganoderma lucidum spore powder particles. Load the produced particles into a supercritical _CO2 extraction device In the extraction kettle, the loading amount is 1.3kg, the extraction pressure is 22MPa, and the temperature is 55°C; the pressure of the separation kettle I is 8MPa, the temperature is 50°C, the pressure of the separation kettle II is 4.5MPa, the temperature is 30°C; the CO ₂ flow is 55L /h, extraction for 2h. Take out the Ganoderma lucidum spore powder in the extraction kettle, and the acid value is 0.34 mg/g, the polysaccharide content is 2.01%, and the total triterpene content is 2.77%). The material in the separation kettle I is released to be 42.62g, and the acid value is 23.4 mg/g. , the material released from the separation kettle II was 9.04g, and the acid value was detected to be 7.13mg/g.

Example 5

Weigh 2kg of broken Ganoderma spore powder (wall broken rate 98%, detected acid value 6.09mg/g, polysaccharide content 1.98%, total triterpene content 2.72%), add 2kg water to make 4.75mm particle size The particles were dried at 70°C to obtain 1.97kg of broken Ganoderma spore powder particles. The prepared particles are loaded into the extraction kettle of the supercritical CO ₂ extraction device. The loading amount is 1.5kg. The extraction pressure is 20MPa and the temperature is 55°C. The pressure of the separation kettle I is 8MPa and the temperature is 45°C. The pressure of the separation kettle II is 5MPa, temperature 30°C; CO ₂ flow rate 50L/h, extraction 1.5h. Take out the Ganoderma lucidum spore powder in the extraction kettle, and the acid value is 0.31mg/g, the polysaccharide content is 1.96%, and the total triterpene content is 2.71%. The material in the separation kettle I is released to be 50.01g, and the acid value is 21.19mg/g. The material in the separation kettle II was released to be 15.2g, and the acid value was detected to be 6.99mg/g.

Comparative example 1

Take 2kg of the same batch of broken Ganoderma spore powder in Example 1, granulate it in the same way as in Example 1, and put the prepared granules into the extraction kettle of the supercritical CO ₂ extraction device. The loading amount is 1.6kg. During the extraction The pressure is 8MPa and the temperature is 40℃; the pressure of the separation kettle I is 6MPa and the temperature is 40℃; the pressure of the separation kettle II is 4MPa and the temperature is 30℃; the CO ₂ flow rate is 60L/h, and the extraction is 1.5h. Take out the Ganoderma lucidum spore powder in the extraction kettle, and the acid value is 3.73mg/g, the polysaccharide content is 1.91%, and the total triterpene content is 2.71%. The material in the separation kettle I is released to be 5.81g, and the acid value is 5.21mg/g. The material in the separation kettle II was discharged to 1.2g, and the acid value was detected to be 2.5mg/g.

Comparative example 2

Take 2kg of the broken Ganoderma spore powder from the same batch as Example 1, granulate according to the same method as Example 1, and put the prepared particles into the extraction kettle of the supercritical CO ₂ extraction device. The loading amount is 1.5kg. During the extraction The pressure is 30MPa and the temperature is 55℃; the pressure of the separation kettle I is 8MPa and the temperature is 55℃; the pressure of the separation kettle II is 4MPa and the temperature is 35℃; the CO ₂ flow rate is 80L/h, and the extraction is 1.5h. Take out the Ganoderma lucidum spore powder from the extraction kettle. The acid value is 0.43 mg/g, the polysaccharide content is 0.28%, and the total triterpene content is 0.17%. The material in the separation kettle I is 385g. The acid value is 4.93 mg/g. Release The material in the separation kettle II is 41.2g, and the acid value detected is 3.81mg/g.

Comparative example 3

Take 2kg of the same batch of broken Ganoderma spore powder in Example 1, granulate it in the same way as in Example 1, and put the prepared granules into the extraction kettle of the supercritical CO ₂ extraction device. The loading amount is 1.8kg. During the extraction The pressure is 10MPa, the temperature is 32°C; the pressure of the separation kettle I is 8MPa, the temperature is 45°C, the pressure of the separation kettle II is 5MPa, the temperature is 35°C; CO ₂ flow rate is 70L/h, extraction is carried out for 2 hours. Take out the Ganoderma lucidum spore powder in the extraction kettle, and the acid value is 3.45 mg/g, the polysaccharide content is 1.89%, and the total triterpene content is 2.68%. The material in the separation kettle I is released to be 8.93g, and the acid value is 10.72 mg/g. The material in the separation kettle II was discharged to 4.33g, and the acid value was detected to be 5.6mg/g.

It can be seen from the comparison between the comparative examples and the examples that the pressure of the extraction kettle plays a key role in the removal of free fatty acids and the retention of active ingredients. If the pressure is too low, the free fatty acids cannot be completely removed. If the pressure is too high, although the free fatty acids can be removed to a certain extent, However, almost all the active ingredients in Ganoderma spore powder are lost. If the temperature is too high, the heat-sensitive secondary components in Ganoderma spore powder will be damaged. If the temperature is too low, the ability of _CO2 to dissolve free fatty acids will decrease. If the extraction time is too long, it will not only increase the loss of Ganoderma spore oil in Ganoderma spore powder, but also cause a waste of resources. If the extraction time is too short, the removal of free fatty acids will be incomplete and the expected effect cannot be achieved.

It can be seen from the acid value and the active ingredients polysaccharides and total triterpenes before and after treatment of Ganoderma lucidum spore powder in the Examples that the supercritical CO ₂ extraction method used in the present invention can effectively remove free fatty acids in Ganoderma lucidum spore powder and retain the active ingredients to the maximum extent.

Claims (10)

A method for removing free fatty acids from Ganoderma lucidum spore powder, which is characterized by including the following steps: (1) Break the walls of Ganoderma lucidum spore powder to a wall breaking rate of more than 95% and granulate; (2) Put the particles obtained in step (1) into the extraction kettle of the supercritical CO ₂ extraction device, the extraction pressure is 12-25Mpa, the extraction temperature is 35-55°C, and the CO ₂ flow rate is 50-90L/h; (3) Control the pressure of the separation kettle I to 7~12MPa and the temperature to 35~55℃; (4) Control the pressure of the separation kettle II to 4~6MPa and the temperature to 25~45℃; (5) The extraction time is 0.5 to 3 hours. After the extraction is completed, the extract is taken out to obtain Ganoderma spore powder with free fatty acids removed. The method for removing free fatty acids from Ganoderma lucidum spore powder according to claim 1, characterized in that the granulation method in step (1) is: the weight ratio of Ganoderma lucidum spore powder and water is 1:0.5~1:1.5, The particle size of the particles is 0.5~10mm, the drying temperature is 50~80°C, and the moisture content of the Ganoderma spore powder particles is controlled at 3~10%. The method for removing free fatty acids from Ganoderma lucidum spore powder according to claim 1, characterized in that the extraction pressure in step (2) is 18-22MPa, the extraction temperature is 50-55°C, and the CO ₂ flow rate is 50-80L/ h. The method for removing free fatty acids from Ganoderma lucidum spore powder according to claim 3, characterized in that the extraction pressure in step (2) is 18MPa, the extraction temperature is 50°C, and the _CO2 flow rate is 80L/h. The method for removing free fatty acids from Ganoderma lucidum spore powder according to claim 1, characterized in that the pressure of the separation kettle I in step (3) is 7.5-8MPa and the temperature is 45-50°C. The method for removing free fatty acids from Ganoderma lucidum spore powder according to claim 5, characterized in that the pressure of the separation kettle I in step (3) is 8MPa and the temperature is 50°C. The method for removing free fatty acids from Ganoderma lucidum spore powder according to claim 1, characterized in that the pressure of the separation kettle II in step (4) is 4-5MPa and the temperature is 30-35°C. The method for removing free fatty acids from Ganoderma lucidum spore powder according to claim 7, characterized in that the pressure of the separation kettle II is 4MPa and the temperature is 30°C. The method for removing free fatty acids from Ganoderma lucidum spore powder according to claim 1, characterized in that the extraction time in step (5) is 1.5-2h. The method for removing free fatty acids from Ganoderma lucidum spore powder according to claim 9, characterized in that, The extraction time in step (5) is 1.5h.