CN104946383B - A kind of supercritical CO2The method that composite microwave auxiliary extraction prepares ganoderma lucidum spore oil - Google Patents

Abstract

The present invention relates to a kind of method that supercritical CO 2 composite microwave auxiliary extraction prepares ganoderma lucidum spore oil, preparation method is（1）First physical wall breaking further walks dry-pressing granulation processing Reishi sporule（2）Add in entrainer ethanol water supercritical CO₂Composite microwave auxiliary extraction technology prepares ganoderma lucidum spore oil, is centrifuged after re-grading decompression and obtains refined ganoderma lucidum spore oil；Solve the problems, such as slug during SCF-CO 2 and even if adds in entrainer extraction effect it is not ideal enough, the recovery rate of ganoderma lucidum spore oil is than conventional supercritical fluid fluid extraction technique raising 20 ~ 35%.

Description

A kind of supercritical CO2The method that composite microwave auxiliary extraction prepares ganoderma lucidum spore oil

Technical field

The present invention relates to the deep process technologies of lucidum spore powder, particularly relate to utilize supercritical CO₂Composite microwave auxiliary extraction The method that technology is taken to prepare ganoderma lucidum spore oil.

Background technology

Ganoderma lucidum is referred to as " celestial grass " since ancient times, has the long history of 5,000 years in China, is always worked as by ancient times emperor Make " miraculous cure ", be considered as the symbol of " having good luck ", be known as " magical east mushroom " by westerner.Now, ganoderma lucidum by China's pharmacopeia is recorded, and is the Chinese medicine of state approval and the important source material of health food.

Reishi sporule is the seed that ganoderma lucidum development and maturation phase ejects, and is the reproduction cell of ganoderma lucidum, is biologically known as Basidiospore.Be known as conidia powder after sporocyst centralized collection, in conidia powder containing lipid, vitamins, carotenoid, triterpenes, A variety of active ingredients such as alkaloids, polysaccharide, sterols, protein and amino acids, due to the inside and outside bilayer of Reishi sporule Wall is hard chitin, if without broken wall, internal component is difficult to be extracted, and also is difficult to be inhaled by human body after taking It receives.

Reishi sporule can obtain spore oil, according to pharmacological research, Reishi sporule by after broken wall using supercritical CO_2 extraction Oil can enhance the immunity of body, antitumor, and liver protection nourishing the stomach has angiocardiopathy, hypertension, diabetes and neurasthenia Good healthcare function.Supercritical CO_2 extraction is nearly new and high technology to grow up for 30 years, using technology extraction Spore oil, than the chemical solvents such as conventional oil ether, n-hexane extraction spore oil have no solvent residue, it is pollution-free, avoid extracting The thermal cracking of object at high temperature is taken, is conducive to the extraction of liposoluble substance and heat-sensitive substance, and simple for process, low energy consumption, extraction The advantages that taking agent nontoxic, easily recycling, has been widely used in the extraction of medicinal herb components and fragrance.

At present, the patent report using SCF-CO 2 ganoderma lucidum spore oil is more, in order to solve lucidum spore powder powder Too thin, in SCF-CO 2, the problem of easily causing material spray under high pressure, patent CN1239100C is disclosed with broken The Reishi sporule of wall is raw material, dry method of being pelletized with the ethanol water that volume fraction is 5%~95%, but using ethyl alcohol Solution is pelletized, and heated-air drying, and ethyl alcohol is inflammable, and the program is dangerous.In patent CN1094766C using lucidum spore powder add water, The method of gelatin, starch, at room temperature extrusion forming, but may pollute extract because adding in auxiliary material.

During SCF-CO 2, the polarity of CO2 is weak, it is only capable of very small to nonpolar state ingredient and polarity Ingredient extracted, the ingredient effect of extracting larger to polarity is bad, and the triterpene compound chemistry knot in Reishi sporule Structure complexity is various, and polarity range is wide, needs higher extraction conditions that can just extract, although existing in the prior art by adopting With ethanol water as entrainer come the scheme of auxiliary extraction, face as patent CN102041163A discloses a kind of more body multistages and surpasses The method of boundary's CO2 Ganoderma Lucidum Spores Oil Extracteds, using ethanol water as entrainer, by being classified the method for decrease temperature and pressure by ganoderma lucidum spore Seed oil is separated, but ethanol water carrys out the scheme of auxiliary extraction as entrainer, and the extraction effect of ethyl alcohol is not ideal enough.

Microwave is the electromagnetic wave that a kind of frequency range is 300MHz ~ 300GHz, in microwave heating process, heated material Molecular polarity orientation year this external electric field variation and change, the rotation of microwave induced dipolar nature or ionic conduction are quickly by targeted Object is closed to extract.Microwave auxiliary extraction（MAE）Good with penetrability, thermal inertia is small, selects heating property, and the scope of application is wide, extraction It takes efficient, saves the time, save reagent, pollute the features such as small, have application in multiple fields such as traditional Chinese medicine extractions.

Invention content

Present invention aim to address the defects of the prior art, provide a kind of supercritical CO 2 composite microwave auxiliary extraction system The method of standby ganoderma lucidum spore oil, simple for process, oil yield is high.

The present invention is achieved by the following technical programs.

A kind of method that supercritical CO 2 composite microwave auxiliary extraction prepares ganoderma lucidum spore oil, preparation method are as follows：

(1) processing of Reishi sporule

1. it is preferred that Reishi sporule and drying 3 ~ 5 hours at 50 DEG C；

It 2. will be through step（1）1. obtained Reishi sporule is put into broken wall in micronizer, the Reishi sporule of broken wall is obtained Powder, sporoderm-broken rate is up to more than 99%；

3. the lucidum spore powder of broken wall one-step-granulating method dry pressing is pelletized, the particle of 40 ~ 60 mesh is made；

（2）Prepare ganoderma lucidum spore oil

1. Reishi sporule powder particles are put into the SCF-CO 2 kettle equipped with microwave generator, with ethanol water For entrainer, ethanol water that every kilogram of material adds in 30 ~ 150ml in extraction kettle mass concentration is 75% ~ 95% is then logical Entering supercritical CO 2 to be extracted, CO2 flows are 10 ~ 40L/h, and extracting pressure is 20~30MPa, and extraction temperature is 30~50 DEG C, Extraction time is 1~3 hour, while opens a microwave generator every 20 ~ 30min, carries out microwave treatment 3 ~ 8 minutes, micro- Wave microwave power is 1kw ~ 100kw.

2. by step（2）1. obtained substance is passed through level-one separating still and carries out decompression separation, pressure is 10 ~ 12MPa, temperature It is 30 ~ 50 DEG C, collects ganoderma lucidum spore oil at this time, is carried out being refining to obtain essence with 5000 ~ 15000 turns per minute of supercentrifugal process Ganoderma lucidum spore oil processed；

3. step will be passed through（2）2. the substance after level-one decompression is passed through the second-order separation kettle, pressure is 5MPa~7Mpa, temperature It is 30 ~ 50 DEG C, a small amount of water is released after separation, CO2 returns to storage tank recycling.

The method that a kind of above-mentioned supercritical CO 2 composite microwave auxiliary extraction prepares ganoderma lucidum spore oil, wherein, that is told is refined The gross mass degree of organic acid and fatty acid is 85 ~ 93% in ganoderma lucidum spore oil, the mass percent of ergosterol class Content is 0.5 ~ 3.5%, and the mass percentage content of triterpenes is 0.2 ~ 2.5%.

Beneficial effects of the present invention are：

The present invention obtains the lucidum spore powder of broken wall, then prepare particle with a step dry pressing using physical method, does not add Any auxiliary material and adhesive in the process also without heating and drying, efficiently solve since lucidum spore powder is too thin, cause to surpass Slug and the incomplete problem of extraction during critical CO2 extractions, and it is simple for process, the pollution of extract will not be caused and because of heating Active ingredient caused by and is destroyed.

The present invention adds in ethanol water in SCF-CO 2 as entrainer, enhances the dissolving of supercritical CO 2 Power and selectivity, when solving conventional supercritical fluid CO2 extraction process due to supercritical CO 2 to low molecule, low polarity, lipophilicity, Low-boiling ingredient such as volatile oil, hydrocarbon, ester, lactone, ether, epoxide etc. show excellent dissolubility, but to pole Property group compound, the more, just more difficult extraction, for the high compound of molecular weight, molecular weight is higher, is more difficult to extract for polarity group The problem of taking, causing extraction yield not high.Simultaneously using Microwave Assisted Extraction Technique, entrainment is added in the prior art even if solving The problem of agent, effect of extracting is also not ideal enough, and the entrainer ingredient that the present invention uses is single, is easily isolated, it will not be to extraction Object pollutes.Final CO2 can return to holding vessel recycling, reach the closure production of process route.

It should be pointed out that the process conditions narrated using the present invention, intermittent unlatching microwave radiation technology equipment, will not produce Raw higher temperature, therefore the active ingredient of ganoderma lucidum spore oil will not be damaged.

Microwave Assisted Extraction Technique is combined by preparation method provided by the present invention with supercritical liquid extraction technique, The recovery rate of ganoderma lucidum spore oil can improve 20 ~ 35%, and the supercritical fluid under identical extraction time than supercritical fluid extraction Temperature and pressure during extraction is lower, and extraction time is shorter under identical extraction temperature and pressure, saves cost.

Specific embodiment

The specific embodiment of the present invention is described in further detail below by way of specific embodiment.

Embodiment 1

A kind of method that supercritical CO 2 composite microwave auxiliary extraction prepares ganoderma lucidum spore oil, preparation method are as follows：

(1) processing of Reishi sporule

1. it is preferred that Reishi sporule and drying 4 hours at 50 DEG C；

It 2. will be through step（1）1. obtained Reishi sporule 20kg is put into broken wall in micronizer, the ganoderma lucidum of broken wall is obtained Conidia powder, sporoderm-broken rate is up to more than 99%；

3. the lucidum spore powder of broken wall one-step-granulating method dry pressing is pelletized, the particle of 40 mesh is made；

（2）Prepare ganoderma lucidum spore oil

1. Reishi sporule powder particles 2kg is put into SCF-CO 2 kettles of the 5L equipped with microwave generator, with ethanol water Solution is entrainer, and the ethanol water that 260ml mass concentrations are 75% is added in extraction kettle, is subsequently passed supercritical CO 2 progress Extraction, CO2 flows are 15L/h, and extracting pressure 30MPa, extraction temperature is 40 DEG C, and extraction time is 3 hours, while every 25min opens a microwave generator, carries out microwave treatment 4.5 minutes, and microwave microwave power is 30kw；

2. by step（2）1. obtained substance is passed through level-one separating still and carries out decompression separation, pressure 11MPa, temperature is 35 DEG C, ganoderma lucidum spore oil at this time is collected, is carried out being refining to obtain refining ganoderam lucidum spore with 10000 turns per minute of supercentrifugal process Oily 655g, oil yield 32.75%；

3. step will be passed through（2）2. the substance after level-one decompression is passed through the second-order separation kettle, pressure 6Mpa, temperature 45 DEG C, a small amount of water is released after separation, CO2 returns to storage tank recycling.

Monitor in refining ganoderam lucidum spore oil the gross mass degree of organic acid and fatty acid be 92%, ergot steroid The mass percentage content of alcohols is 3.0%, and the mass percentage content of triterpenes is 2.35%.

Embodiment 2

A kind of method that supercritical CO 2 composite microwave auxiliary extraction prepares ganoderma lucidum spore oil, preparation method are as follows：

(1) processing of Reishi sporule

1. it is preferred that Reishi sporule and drying 3 hours at 50 DEG C；

It 2. will be through step（1）1. obtained Reishi sporule 15kg is put into broken wall in micronizer, the ganoderma lucidum of broken wall is obtained Conidia powder, sporoderm-broken rate is up to more than 99%；

3. the lucidum spore powder of broken wall one-step-granulating method dry pressing is pelletized, the particle of 60 mesh is made；

（2）Prepare ganoderma lucidum spore oil

1. Reishi sporule powder particles 1.5kg is put into SCF-CO 2 kettles of the 5L equipped with microwave generator, with ethyl alcohol Aqueous solution is entrainer, and the ethanol water that 180ml mass concentrations are 95% is added in extraction kettle, be subsequently passed supercritical CO 2 into Row extraction, CO2 flows are 15L/h, and extracting pressure 30MPa, extraction temperature is 40 DEG C, and extraction time is 3 hours, while every 30min opens a microwave generator, carries out microwave treatment 5.5 minutes, and microwave microwave power is 40kw；

2. by step（2）1. obtained substance is passed through level-one separating still and carries out decompression separation, pressure 12MPa, temperature is 40 DEG C, ganoderma lucidum spore oil at this time is collected, is carried out being refining to obtain refining ganoderam lucidum spore with 10000 turns per minute of supercentrifugal process Oily 454g, oil yield 30.26%；

3. step will be passed through（2）2. the substance after level-one decompression is passed through the second-order separation kettle, pressure 7Mpa, temperature 50 DEG C, a small amount of water is released after separation, CO2 returns to storage tank recycling.

Monitor in refining ganoderam lucidum spore oil the gross mass degree of organic acid and fatty acid be 90%, ergot steroid The mass percentage content of alcohols is 2.0%, and the mass percentage content of triterpenes is 1.05%.

As can be seen from the above-described embodiment, the oil yield of the invention for preparing ganoderma lucidum spore oil is apparently higher than conventional method, saves Solvent is saved, the production time is short, and ganoderma lucidum spore oil is quality.

Here description of the invention and application are illustrative, are not wishing to limit the scope of the invention to above-described embodiment In, therefore, the present invention is not limited by the present embodiment, and any technical solution obtained using equivalence replacement is protected in the present invention In the range of.

Claims (2)

1. a kind of supercritical CO₂The method that composite microwave auxiliary extraction prepares ganoderma lucidum spore oil, it is characterized in that, preparation method is such as Under：

(1) processing of Reishi sporule

1. it is preferred that Reishi sporule and drying 3~5 hours at 50 DEG C；

It 2. will be through step（1）1. obtained Reishi sporule is put into broken wall in micronizer, the lucidum spore powder of broken wall is obtained, is broken Wall rate is up to more than 99%；

3. the lucidum spore powder of broken wall one-step-granulating method dry pressing is pelletized, the particle of 40~60 mesh is made；

（2）Prepare ganoderma lucidum spore oil

1. Reishi sporule powder particles are put into the supercritical CO equipped with microwave generator₂In extraction kettle, using ethanol water as entrainment Agent, the ethanol water that the mass concentration that every kilogram of material adds in 30~150ml in extraction kettle is 75%~95%, is subsequently passed super Critical CO₂It is extracted, CO₂Flow is 10~40L/h, and extracting pressure is 20~30MPa, and extraction temperature is 30~50 DEG C, Extraction time is 1~3 hour, while opens a microwave generator every 20~30min, carries out microwave treatment 3~8 minutes, Microwave power is 1kw~100kw；

2. by step（2）1. obtained substance is passed through level-one separating still and carries out decompression separation, pressure is 10~12MPa, and temperature is 30~50 DEG C, ganoderma lucidum spore oil at this time is collected, is carried out being refining to obtain essence with 5000~15000 turns per minute of supercentrifugal process Ganoderma lucidum spore oil processed；

3. step will be passed through（2）2. the substance after level-one decompression is passed through the second-order separation kettle, pressure is 5MPa~7Mpa, temperature 30 ~50 DEG C, a small amount of water, CO are released after separation₂Return to storage tank recycling.

2. a kind of supercritical CO as described in claim 1₂The method that composite microwave auxiliary extraction prepares ganoderma lucidum spore oil, it is special It is 85~93% to levy as the gross mass degree of organic acid in the refining ganoderam lucidum spore oil and fatty acid, ergot steroid The mass percentage content of alcohols is 0.5~3.5%, and the mass percentage content of triterpenes is 0.2~2.5%.