CN102041163A

CN102041163A - Multi-body multi-stage supercritical CO2 extraction method of ganoderma lucidum spore oil

Info

Publication number: CN102041163A
Application number: CN2011100010993A
Authority: CN
Inventors: 邓泽元; 章晋武; 李广焱
Original assignee: NANCHANG TONGXIN ZICHAO BIOENGINEERING CO Ltd
Current assignee: NANCHANG TONGXIN ZICHAO BIOENGINEERING CO Ltd
Priority date: 2011-01-05
Filing date: 2011-01-05
Publication date: 2011-05-04
Anticipated expiration: 2031-01-05
Also published as: CN102041163B

Abstract

The invention relates to a multi-body multi-stage supercritical CO2 extraction method of ganoderma lucidum spore oil, which is characterized by comprising the following steps: (1) carrying out ultra-fine pulverization for breaking walls to obtain ganoderma lucidum spore powder; (2) granulating the wall-broken ganoderma lucidum spore powder by a dry press method in a one-step granulator; (3) placing the ganoderma lucidum spore powder granules in three-stage separation supercritical CO2 extraction kettles; and (4) respectively obtaining ganoderma lucidum spore oil components of different solubilities from a separation kettle I and a separation kettle II, and discharging an entrainer mainly from a separation kettle III. The invention has the following technical advantages: 1. more functional components in ganoderma lucidum spores can be extracted more efficiently, thereby achieving high oil yield and increasing the triterpenoid constituent content in the ganoderma lucidum spore oil; 2. the multi-body multi-stage extraction can separate the ganoderma lucidum spore oil from carrying agents such as ethanol, water and other components more effectively, thereby ensuring better quality of the extract; and 3. the extraction is carried out in the absence of oxygen gas, thereby lowering the damage possibility of active components of the ganoderma lucidum spores.

Description

The multistage supercritical CO of a kind of many bodies 2The method of Ganoderma Lucidum Spores Oil Extracted

Technical field

The present invention relates to a kind of method of Ganoderma Lucidum Spores Oil Extracted, relate in particular to the multistage supercritical CO of a kind of many bodies ₂The method of Ganoderma Lucidum Spores Oil Extracted.

Background technology

Glossy ganoderma is the polyporaceae fungi, have the reputation of " celestial grass ", states clearly in the Pharmacopoeia of the People's Republic of China, glossy ganoderma has the function of " invigorating QI and tranquilization, relieving cough and asthma ", and " be used for dizzy egersis; shortness of breath and palpitation, consumptive disease is coughed and breathed heavily " is listed in first-selection in having the moving plant and biology of medicine food of antitumous effect.Ganoderma spore is the glossy ganoderma growth and maturity phase to produce the seed that discharges, sexual cell for glossy ganoderma, whole hereditary active substance with glossy ganoderma, it is the elite of glossy ganoderma, and comprised the triterpenes in the Ganoderma spore, fatty acid, sterols, polyose, alkaloids, and composition such as ucleosides in the Ganoderma spore oil, be the aggregate of Ganoderma spore effective constituent, have multiple physiologically active.Wherein the Ganoderma triterpenoids constituents is the main effective constituent of glossy ganoderma, because of the diversity of its chemical structure, make ganoderma lucidum triterpene compounds have antitumor, anti-oxidant, suppress that cholesterol is synthetic, anticoagulant, protect the liver, pharmacologically active more widely such as analgesia.At present glossy ganoderma medicine on the domestic market, healthcare products are of a great variety, and a lot of ganoderma lucidum prods are with total triterpene property functional component as a token of.Ganoderma lucidum triterpene compounds is not only the focus of current glossy ganoderma chemistry and pharmacological research, and has better industrial application prospects.In recent years, the Ganoderma spore oil production has become the treasure in the high-grade healthcare products, has crucial utility value and economic worth.

The traditional extracting method of Ganoderma spore oil generally adopts methyl alcohol or the lixiviate of ethanol equal solvent, and extraction efficiency is low, extraction time is many, energy consumption is high, solvent load is big, many shortcomings such as dissolvent residual are arranged but this method exists.Supercritical CO ₂Abstraction technique is the technology of emerging extraction, separation and a purifying of foodstuffs industry, compare with traditional solvent extration, have no solvent residue, pollution-free, avoid at high temperature thermo-cracking of extract, help the extraction of lipid-soluble substance and heat-sensitive substance, and technology is simple, energy consumption is low, advantages such as extraction agent is nontoxic, easy recovery have been widely used in the extraction of medicinal herb components and spices.

The patent application and the report of existing employing supercritical CO 2 Ganoderma Lucidum Spores Oil Extracted are more.It is that Ganoderma spore with broken wall is a raw material that patent CN1239100C discloses its method for preparing Ganoderma spore oil, with volume percent is after 5%～95% the aqueous ethanolic solution granulation drying, to use supercritical carbon dioxide extraction, but adopt ethanolic soln to granulate, hot-air seasoning, ethanol is inflammable, and is dangerous.Among the patent CN1194079C, Ganoderma spore powder, granulation expanded through bulking machine, changed the raw material bulk density, can improve mass transfer effect, increase oil yield, but adopt puffing technique temperature higher (80～140 ℃), can quicken the oxidation and the process of becoming sour of lipid in the spore powder, can bring disadvantageous effect the quality of oil.Patent CN1255519C discloses the method for its Ganoderma Lucidum Spores Oil Extracted, under the CO 2 supercritical state, Ganoderma spore powder with cellular wall broken is substep step-down and change temperature in nonionogenic tenside Tween80, obtain the component of different solubilities at last by one-level resolver and secondary resolver, but tensio-active agent can be blended in the spore oil, and the ability of auxiliary extraction is also limited.

Adopt supercritical CO ₂The method of Ganoderma Lucidum Spores Oil Extracted is a lot, but perfect not enough, needs further to explore the processing condition of best suitable suitability for industrialized production.

Summary of the invention

The object of the present invention is to provide the multistage supercritical CO of a kind of many bodies ₂The method of Ganoderma Lucidum Spores Oil Extracted, this method is simple and easy, efficient, the production time short, be fit to suitability for industrialized production.

The present invention is achieved like this, and method steps is:

(1) Ganoderma spore is put into the supper micron mill broken wall, obtained Ganoderma spore powder;

(2) Ganoderma spore powder with cellular wall broken is granulated with the one-step-granulating method dry pressing, makes 10-40 purpose particle;

(3) the Ganoderma spore powder particles is put into had three grades of isolating supercritical COs ₂In the extraction kettle, with the aqueous ethanolic solution of massfraction 25%～95% as carrying agent, 25%～95% of every kilogram of dress material adding 20～250ml aqueous ethanolic solution in the extraction kettle, carry out supercritical extraction then, extracting pressure is 25～40MPa, extraction temperature is 35～60 ℃, and the extraction time is 2～4 hours;

(4) obtain the Ganoderma spore oil ingredient of different solubilities respectively from separating still I and separating still II, entrainment agent is then mainly emitted from the separating still III.

At supercritical CO ₂Install rectifier unit and many gradient temperatures pressure in the separating still device in the extraction plant additional and regulated separation system, the separating pressure of separating still I is 10～20MPa, temperature is 35～50 ℃, the separating pressure of separating still II is 7.5～10MPa, temperature is 30～45 ℃, the separating pressure of separating still III is 4～7MPa, and temperature is 30～40 ℃.

Know-why of the present invention:

1. common supercritical CO ₂In the extraction process because CO ₂Polarity a little less than, it only can extract nonpolar attitude composition and the less composition of polarity, but the extracts active ingredients poor effect relatively large to polarity.Triterpene substance in the Ganoderma spore is that chemical structure is various, and a class material of polarity a wider range needs higher extraction conditions just can extract, and it is dissolved in ethanol, further increasing of solubleness under condition of high voltage.So agent and CO are carried in the second alcohol and water conduct by certain proportioning ₂Form many bodies CO of polarity a wider range ₂Medium, many bodies CO ₂Medium can effectively extract the opposed polarity composition in the Ganoderma spore, thereby reaches triterpenes, fatty acid, sterols isoreactivity composition in the high efficiency extraction Ganoderma spore.

2. at supercritical CO ₂Install a rectifier unit and many gradient temperatures pressure regulating system in the separating still device of extraction plant additional, make it to become multistage separation temperature, pressure gradient, thereby reach stage trapping by optimization temperature, pressure parameter, under the trickleer temperature difference, pressure reduction change, make effective constituent, ethanol, water and the CO of Ganoderma spore ₂Between separate, improved quality product, changed and can not realize carrying agent and the complete isolating situation of effective constituent under the single separation temperature pressure gradient condition.

Technique effect of the present invention is: 1. owing to adopted the multistage CO of many bodies ₂The extraction mode can more effectively more extract the multiple functional component in the Ganoderma spore, so the oil yield height, and triterpenes content also increases in the Ganoderma spore oil; 2. because the multistage extraction of many bodies is more can be effectively separating of oil with carrying composition such as agent second alcohol and water and Ganoderma spore, so the quality of extract is better; 3. extract under oxygen free condition, the destroyed probability of the active ingredient of Ganoderma spore reduces.

Embodiment

Embodiment 1:

After Ganoderma spore powder with cellular wall broken 6Kg granulation, place supercritical CO ₂In the extraction kettle, extracting pressure is 25MPa, and extraction temperature is 40 ℃, carrying agent is 90% aqueous ethanolic solution, 800 ml, extracted 2 hours, the separating pressure of separating still I is 13MPa, and temperature is 45 ℃, the separating pressure of separating still II is 8.5MPa, temperature is 40 ℃, and the separating pressure of separating still III is 6MPa, and temperature is 35 ℃, from the separating still I, emit the more weak Ganoderma spore oil ingredient 1.52Kg of polarity at last, oil yield 25.3%; From the separating still II, emit the stronger Ganoderma spore oil ingredient 0.33Kg of polarity, oil yield 5.5%.

Embodiment 2:

After Ganoderma spore powder with cellular wall broken 6Kg granulation, place supercritical CO ₂In the extraction kettle, extracting pressure is 30MPa, and extraction temperature is 50 ℃, carrying agent is 85% aqueous ethanolic solution, 1000 ml, extracted 4 hours, the separating pressure of separating still I is 15MPa, and temperature is 45 ℃, the separating pressure of separating still II is 8MPa, temperature is 45 ℃, and the separating pressure of separating still III is 5MPa, and temperature is 40 ℃, from the separating still I, emit the more weak Ganoderma spore oil ingredient 1.65Kg of polarity at last, oil yield 27.5%; From the separating still II, emit the stronger Ganoderma spore oil ingredient 0.47Kg of polarity, oil yield 7.8%.

Claims

1. the multistage supercritical CO of body more than a kind ₂The method of Ganoderma Lucidum Spores Oil Extracted is characterized in that method steps is:

2. the multistage supercritical CO of a kind of many bodies according to claim 1 ₂The method of Ganoderma Lucidum Spores Oil Extracted is characterized in that at supercritical CO ₂Install rectifier unit and many gradient temperatures pressure in the separating still device in the extraction plant additional and regulated separation system, the separating pressure of separating still I is 10～20MPa, temperature is 35～50 ℃, the separating pressure of separating still II is 7.5～10MPa, temperature is 30～45 ℃, the separating pressure of separating still III is 4～7MPa, and temperature is 30～40 ℃.