阅读说明：本技术 一种降低灵芝孢子油过氧化值及酸价的方法 (Method for reducing peroxide value and acid value of ganoderma lucidum spore oil ) 是由 黄守文 于 2021-09-15 设计创作，主要内容包括：本发明公开了一种降低灵芝孢子油过氧化值及酸价的方法,包括以下步骤：1)灵芝孢子粉、淀粉、破壁酶、淀粉酶和维生素E粉末,依次加入液氮、纯化水及液氮,后水浴加热酶解反应3h；2)加NaHCO3调整pH至7.2,加入枯草芽孢杆菌的培育粉,38℃下恒温搅拌1h；3)低温压滤,将所得滤饼加入液氮冷冻成块,进行真空干燥,再吸附滤液上层油状物,再液氮冷冻成块,进行真空干燥；4)饼状物碾碎成粉末,进行超临界CO2萃取,得到孢子油后制成孢子油胶囊。本发明通过溶酶破壁和超临界萃取结合,通过两次液氮排除酶解体系中的游离氧,再加入可消耗溶解氧的枯草芽孢杆菌,最后超临界萃取,使整个生产过程中孢子油均无氧化反应,不易酸化腐败。(The invention discloses a method for reducing peroxide value and acid value of ganoderma lucidum spore oil, which comprises the following steps: 1) sequentially adding liquid nitrogen, purified water and liquid nitrogen into ganoderma lucidum spore powder, starch, wall-breaking enzyme, amylase and vitamin E powder, and then heating in a water bath for enzymolysis reaction for 3 hours; 2) adding NaHCO3 to adjust pH to 7.2, adding Bacillus subtilis culture powder, and stirring at constant temperature of 38 deg.C for 1 h; 3) performing low-temperature filter pressing, adding liquid nitrogen into the obtained filter cake, freezing into blocks, performing vacuum drying, adsorbing the oily matter on the upper layer of the filtrate, freezing into blocks by using liquid nitrogen, and performing vacuum drying; 4) grinding the cake into powder, performing supercritical CO2 extraction to obtain spore oil, and making into spore oil capsule. According to the invention, through the combination of enzyme-dissolving wall breaking and supercritical extraction, free oxygen in an enzymolysis system is removed through liquid nitrogen twice, then the bacillus subtilis capable of consuming dissolved oxygen is added, and finally the supercritical extraction is carried out, so that the spore oil has no oxidation reaction in the whole production process, and is not easy to acidify and decay.)

1. A method for reducing peroxide value and acid value of ganoderma lucidum spore oil is characterized by comprising the following steps:

1) adding 5 parts by weight of starch into 100 parts by weight of ganoderma lucidum spore powder, blending, adding 0.5 part by weight of wall breaking enzyme, 0.1 part by weight of amylase and 10 parts by weight of vitamin E powder, putting into a stirring container, stirring, slowly pouring liquid nitrogen until the temperature of the bottom of the container reaches about-50 ℃, and slowly pouring purified water five times the weight of the ganoderma lucidum spore powder until the temperature reaches 10 ℃;

2) stirring for 10min, stopping stirring, and pouring liquid nitrogen again until the temperature of the bottom of the container reaches-10 deg.C, sealing the sealing cover at the top of the container, opening the air release pipe at the top, and preventing the air release pipe from entering the container again through a water seal anti-suck back device;

3) heating the container in water bath until the temperature is 45 ℃, and carrying out constant-temperature enzymolysis reaction for 3 hours;

4) closing the gas release pipe, and adding NaHCO from the feeding port₃Adjusting pH to 7.2, air cooling to 38 deg.C, adding Bacillus subtilis powder, stirring, and stirring at 38 deg.C for 1 hr to obtain suspended substance;

5) carrying out low-temperature filter pressing on the suspended matters to obtain filter cakes, washing the filter cakes for 3 times by butane, layering the obtained filtrate to obtain upper-layer oily matters, adding liquid nitrogen into the obtained filter cakes to freeze the filter cakes into blocks, carrying out vacuum drying to obtain dried porous filter cakes, adsorbing the obtained upper-layer oily matters by the obtained porous filter cakes, freezing the filter cakes into blocks by the liquid nitrogen, and carrying out vacuum drying to obtain bright cakes;

6) grinding the cake to a powder, and pouring the powder into supercritical CO₂The extraction conditions in the extraction kettle are 25MPa of pressure and 45 ℃, the extraction time is 3h, the conditions in the separation kettle I are 8.5MPa of temperature and 30 ℃, the spore oil products are obtained from the separation kettle I, and gelatin is used for wrapping the spore oil products to prepare the spore oil capsules.

2. The method for reducing peroxide number and acid value of ganoderma lucidum spore oil according to claim 1, wherein the ganoderma lucidum spore powder is spore powder with water content not more than 10% after cleaning and drying, and the starch is ultrafine starch powder treated by a vulcanization drying bed.

3. The method for reducing peroxide number and acid value of ganoderma lucidum spore oil according to claim 1, wherein the wall-breaking enzyme is chitinase.

4. The method of claim 1, wherein the metabolites of Bacillus subtilis are enzymes such as self-synthesized alpha-amylase, protease, lipase, chitinase and cellulase.

Technical Field

The invention relates to the technical field of ganoderma lucidum spore oil purification, in particular to a method for reducing peroxide value and acid value of ganoderma lucidum spore oil.

Background

The peroxide value represents an index of the degree of oxidation of fats and oils, fatty acids, and the like. Is the active oxygen content in the 1 kg sample, expressed as millimoles of peroxide. Indicating whether the sample has been deteriorated by oxidation. The quality and the degree of deterioration of foods made from fats and oils are judged by detecting the peroxide value of the foods.

Acid value is an indicator of the free fatty acid content of fat, which is slowly hydrolyzed by the action of microorganisms, enzymes and heat during long-term storage to produce free fatty acids. And the quality of fat is related to the content of free fatty acids therein. Acid value is generally used as one of the metrics. The acid value can be used as an indicator of the degree of hydrolysis under the conditions of fat production and as an indicator of rancidity under the conditions of preservation. The smaller the acid value, the better the grease quality, the better the freshness and the degree of refining.

Under general conditions, the ganoderma lucidum spore oil is easy to deteriorate and generate peculiar smell due to excessively high acid value and peroxide value, the shelf life of the spore oil product is too short, the taste and the product quality are influenced, and the health of a human body is possibly damaged.

The current method for reducing the excessive acid value and peroxide value in ganoderma spore oil is molecular distillation, which is a distillation method operated under high vacuum, and the mean free path of vapor molecules is larger than the distance between an evaporation surface and a condensation surface, so that the liquid mixture can be separated by utilizing the difference of the evaporation rates of all components in feed liquid.

The acid value and the peroxide value in the ganoderma lucidum spore powder can be increased along with the prolonging of the exposure time in the air, the ganoderma lucidum spore oil extracted from the ganoderma lucidum spore powder is more rapidly deteriorated, and the acid value and the peroxide value can be increased in the processes of transportation, bagging, pharmacy and packaging, so that the invention tries to protect the product before the wall breaking of the spore powder so as to avoid new hidden troubles brought to the product by the subsequent wall breaking, purification and related transportation production processes.

Disclosure of Invention

The invention aims to solve the defects in the prior art and provides a method for reducing the peroxide value and the acid value of ganoderma lucidum spore oil.

In order to achieve the purpose, the invention adopts the following technical scheme:

a method for reducing peroxide value and acid value of ganoderma lucidum spore oil comprises the following steps:

1) adding 5 parts by weight of starch into 100 parts by weight of ganoderma lucidum spore powder, blending, adding 0.5 part by weight of wall breaking enzyme, 0.1 part by weight of amylase and 10 parts by weight of vitamin E powder, putting into a stirring container, stirring, slowly pouring liquid nitrogen until the temperature of the bottom of the container reaches about-50 ℃, and slowly pouring purified water five times the weight of the ganoderma lucidum spore powder until the temperature reaches 10 ℃;

2) stirring for 10min, stopping stirring, and pouring liquid nitrogen again until the temperature of the bottom of the container reaches-10 deg.C, sealing the sealing cover at the top of the container, opening the air release pipe at the top, and preventing the air release pipe from entering the container again through a water seal anti-suck back device;

3) heating the container in water bath until the temperature is 45 ℃, and carrying out constant-temperature enzymolysis reaction for 3 hours;

4) closing the air release pipe, adding NaHCO3 from the feeding port to adjust the pH value to 7.2, cooling the air to 38 ℃ at the bottom of the container, adding the bacillus subtilis culture powder, uniformly stirring, and stirring for 1h at the constant temperature of 38 ℃ to obtain suspended matters;

5) carrying out low-temperature filter pressing on the suspended matters to obtain filter cakes, washing the filter cakes for 3 times by butane, layering the obtained filtrate to obtain upper-layer oily matters, adding liquid nitrogen into the obtained filter cakes to freeze the filter cakes into blocks, carrying out vacuum drying to obtain dried porous filter cakes, adsorbing the obtained upper-layer oily matters by the obtained porous filter cakes, freezing the filter cakes into blocks by the liquid nitrogen, and carrying out vacuum drying to obtain bright cakes;

6) crushing the cake into powder, pouring the powder into an extraction kettle of supercritical CO2, extracting for 3h under the conditions of 25MPa of pressure and 45 ℃ of temperature, separating the product in the separation kettle I under the conditions of 8.5MPa of temperature and 30 ℃ of temperature, obtaining spore oil products from the separation kettle I, and wrapping the spore oil products by gelatin to prepare spore oil capsules.

Preferably, the ganoderma lucidum spore powder is spore powder with the water content of not more than 10% after cleaning and drying, and the starch refers to ultrafine starch powder processed by a vulcanization drying bed.

Preferably, the wall breaking enzyme is in particular chitinase, for lytic wall breaking.

Preferably, the metabolites of bacillus subtilis are self-synthesized enzymes such as alpha-amylase, protease, lipase, chitinase, and cellulase, which can promote further wall breaking.

Compared with the prior art, the invention has the beneficial effects that:

1. firstly, combining enzyme-dissolving wall breaking and supercritical extraction to obtain a spore oil product; secondly, in order to prevent the accidents of oxidation and acidification in the production process, the free oxygen in an enzymolysis system is removed by liquid nitrogen twice; then adding bacillus subtilis capable of consuming dissolved oxygen, matching with glucose generated by enzymolysis of starch as nutrition, and further consuming, wherein excessive surplus bacillus subtilis is left in the filter cake for further protecting spore powder; after two times of liquid nitrogen freezing and vacuum drying, removing water and inactivating enzyme and bacillus subtilis; and finally, carrying out supercritical extraction on the powder obtained by grinding, wherein the acid value of the obtained spore oil is less than 1.0mgKOH/g of oil, and the peroxide value is less than 4 mmol/kg.

2. The product obtained by the invention, namely the spore oil capsule, contains trace vitamin E, NaHCO3, the bacillus subtilis inactivated at low temperature and metabolites thereof besides the spore oil, and the oxygen in the system is consumed by the bacillus subtilis in the whole process, and redundant acid is consumed by the reductive vitamin E and the alkaline NaHCO3, so that the spore oil has no oxidation reaction in the whole process and is not easy to acidify and corrupt.

Detailed Description

Example 1:

a method for reducing peroxide value and acid value of ganoderma lucidum spore oil comprises the following steps:

1) adding 5 parts by weight of starch into 100 parts by weight of ganoderma lucidum spore powder, blending, adding 0.5 part by weight of wall breaking enzyme, 0.1 part by weight of amylase and 10 parts by weight of vitamin E powder, putting into a stirring container, stirring, slowly pouring liquid nitrogen until the temperature of the bottom of the container reaches about-50 ℃, and slowly pouring purified water five times the weight of the ganoderma lucidum spore powder until the temperature reaches 10 ℃;

2) stirring for 10min, stopping stirring, and pouring liquid nitrogen again until the temperature of the bottom of the container reaches-10 deg.C, sealing the sealing cover at the top of the container, opening the air release pipe at the top, and preventing the air release pipe from entering the container again through a water seal anti-suck back device;

3) heating the container in water bath until the temperature is 45 ℃, and carrying out constant-temperature enzymolysis reaction for 3 hours;

4) closing the air release pipe, adding NaHCO3 from the feeding port to adjust the pH value to 7.2, cooling the air to 38 ℃ at the bottom of the container, adding the bacillus subtilis culture powder, uniformly stirring, and stirring for 1h at the constant temperature of 38 ℃ to obtain suspended matters;

5) carrying out low-temperature filter pressing on the suspended matters to obtain filter cakes, washing the filter cakes for 3 times by butane, layering the obtained filtrate to obtain upper-layer oily matters, adding liquid nitrogen into the obtained filter cakes to freeze the filter cakes into blocks, carrying out vacuum drying to obtain dried porous filter cakes, adsorbing the obtained upper-layer oily matters by the obtained porous filter cakes, freezing the filter cakes into blocks by the liquid nitrogen, and carrying out vacuum drying to obtain bright cakes;

6) crushing the cake into powder, pouring the powder into an extraction kettle of supercritical CO2, wherein the extraction conditions are 25MPa of pressure and 45 ℃ of temperature, the extraction time is 3h, the conditions of a separation kettle I are 8.5MPa of temperature and 30 ℃, a spore oil product is obtained from the separation kettle I, gelatin is used for wrapping the spore oil products to prepare a spore oil capsule, the spore oil capsule contains trace vitamin E, NaHCO3, the bacillus subtilis after low-temperature inactivation and metabolites thereof, and oxygen in a bacillus subtilis consumption system, reductive vitamin E and alkaline NaHCO3 consume redundant acid in the whole process, so that the spore oil has no oxidation reaction and is not easy to acidify and decay in the whole process.

Example 2:

compared with the example 1, the rest conditions are unchanged, and the conditions of the separation kettle I of the supercritical extraction are changed into 9MPa and the temperature is 40 ℃.

Example 3:

compared with the example 1, the rest conditions are unchanged, and the conditions of the separation kettle I of the supercritical extraction are changed into 9.5MPa and the temperature is 50 ℃.

Example 4:

compared with the example 1, the rest conditions are unchanged, and the conditions of the separation kettle I of the supercritical extraction are changed into 10MPa and the temperature is 60 ℃.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.