CN1634532A - Ultrasonic extraction method for glossy ganoderma spore oil - Google Patents

Ultrasonic extraction method for glossy ganoderma spore oil Download PDF

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Publication number
CN1634532A
CN1634532A CN 200410052195 CN200410052195A CN1634532A CN 1634532 A CN1634532 A CN 1634532A CN 200410052195 CN200410052195 CN 200410052195 CN 200410052195 A CN200410052195 A CN 200410052195A CN 1634532 A CN1634532 A CN 1634532A
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ganoderma spore
extraction
spore oil
solvent
supersound extraction
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CN 200410052195
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CN1270729C (en
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李金华
葛发欢
周锦珂
宁德山
黄海
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Guangzhou Hanfang Pharmaceutical Co., Ltd.
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Hanfang Modem Chinese Traditional Medicine Research Development Co Ltd Guang
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Abstract

Disclosed is an ultrasonic extraction method for glossy ganoderma spore oil which comprises, using wall-broken glossy ganoderma spore powder as raw material, immersing 0-6 hours in organic solvent, loading into supersonic extraction still, extracting for 1/6-6 hours, centrifuging or filtering the extract, reclaiming the solvent.

Description

The preparation method of Ganoderma spore oil supersound extraction
Technical field
The spore that the present invention relates to Ganderma lucidum is a raw material, extracts a kind of method of active component, specifically relates to the method that a kind of ultrasonic technique is extracted Ganoderma spore oil.
Background technology
Ganoderma (Ganoderma lucidum) is a kind ofly in China edible historical rare Chinese medicine to be arranged for many years, classifies as top gradely at Shennong's Herbal, and the effect of " invigorating the spleen and replenishing QI, strengthening the body resistance " is arranged.The Ganoderma spore sexual cell that to be Ganoderma constantly eject under the cap at mature period, its main functional component can be divided into triterpenes, polysaccharide, nucleoside, enzyme, aminoacid, organic germanium, sterol, alkaloid and multivitamin etc.Ganoderma spore oil is the enrich body of Ganoderma spore lipid material, contains various active compositions such as multiple unsaturated fatty acid (especially containing unique odd-carbon fatty acid), triterpenes, has the body immunocompetence, improves physiological functions such as fatigue.
The traditional extraction process of Ganoderma spore oil is to adopt solvent extraction, has shortcomings such as low, the consuming time length of extraction efficiency, energy consumption height.The now existing supercritical CO that adopts 2Extract report and patent such as CN1445346A, CN1094766C and the CN1114446C of the preparation method of spore oil, but its major defect is a supercritical CO 2Equipment is a kind of high pressure equipment, and the equipment one-time investment is big, and in addition, in order to guarantee safety in production, the plant maintenance expense has high input, and has increased production cost.In order to overcome the shortcoming of said extracted method, be necessary to grope a kind of new Ganoderma spore oil and extract preparation method.
Summary of the invention
The purpose of this invention is to provide a kind of novel preparation method that utilizes ultrasonic technique to extract Ganoderma spore oil.
Ultrasound wave is a kind of elastic mechanical vibration wave, and the extraction that it is applied to pharmaceutical analysis and chemical constituent as a kind of extractive technique has had the research history of two more than ten years.Ultrasound assisted extraction technique is to utilize multiple primary and secondary level effects such as ultrasonic cavitation effect, mechanical vibration, heat effect, in fluid, produce the High Temperature High Pressure field of moment, the surface of solids in the convection cell produces powerful shearing force, quicken the stripping of active skull cap components and strengthen mass transport process, so also claim ultrasound-enhanced extraction.
The technical scheme of Cai Yonging is to achieve the object of the present invention: it is raw material that the Ganoderma spore powder of breaking cellular wall is adopted in the preparation of Ganoderma spore oil, soaks 0~6 hour with organic solvent, places the supersound extraction still, at supersonic frequency 20~800kHz, and ultrasound intensity 0.3~15W/cm 2, the w/v of Ganoderma spore powder and solvent is 1: 2~20, extracts under the condition of 10~80 ℃ of temperature, extracts 1/6~6 hour,, gets supernatant liquid and reclaims solvent through centrifugal or sucking filtration through the extracting solution after the supersound extraction, obtains Ganoderma spore oil.
The selection of used organic solvent should be had stronger dissolving power to carrying oils and fats to extract medium, and stronger volatility and certain chemical stability are arranged, and nontoxic, boiling spread is suitable, cheap easily supply etc.Therefore, it is close with the oils and fats dielectric constant that this patent emphasis is chosen, and is preferably petroleum ether, chloroform, ethanol, acetone or ether, and the best is petroleum ether and chloroform.
Condition during preferred supersound extraction: supersonic frequency is 20~50kHz, ultrasound intensity 0.3~10W/cm 2, the w/v of Ganoderma spore powder and solvent is 1: 5~10, extracts 30~40 ℃ of temperature, 1~2 hour extraction time.
Supernatant liquid reclaims solvent method and is preferably concentrating under reduced pressure or thin film concentration after the said supersound extraction, makes that to obtain the Ganoderma spore oil quality good.
Beneficial effect of the present invention:
Hyperacoustic multiple-effect during 1, owing to supersound extraction is as cavitation, stirring, the diffusion of reinforcement mass transfer etc., the motion of accelerated solvent, impel solvent in cell, to permeate, help Ganoderma spore oil and from spore coat, shift, and fully mix, promote the extraction of effective ingredient with solvent to solvent.The extraction efficiency height.
2, compare with the solvent extraction method method of routine, improved extraction efficiency, shortened extraction time, reduced the energy consumption of unit material, the solvent consumption is less relatively, the product yield height.
3 and supercritical CO 2Extraction method is compared height, does not need high pressure equipment, and the disposable input expense of equipment is low.
4, technological process is simple, and convenient being difficult for of slagging tap stops up, and production operation is controlled easily, and the safety of equipment is good, is fit to commercial production.
5, ultrasound assisted extraction technique is a kind of low-temperature physics leaching process, so the biological activity of extract is intact.
Following structure specific embodiment is set forth technical scheme of the present invention
The specific embodiment
Embodiment 1
Get 2kg the Ganoderma spore powder of breaking cellular wall in the supersound extraction still, added 10 liters of soaked in absolute ethyl alcohol 2 hours.The frequency of supersound extraction is 20kHz, ultrasound intensity 0.5W/cm 2, extract 30 ℃ of temperature, 2.5 hours extraction time.Collect extracting solution after extraction is finished, clear liquor is got in the 5000rpm centrifugalize, and concentrating under reduced pressure gets faint yellow spore oil with spore powder special odor, yield 22.98%, total triterpene contents 22.88% (with respect to the ursolic acid meter), acid value 15.8.
Embodiment 2
Get 2kg the Ganoderma spore powder of breaking cellular wall in the supersound extraction still, added 10 liter of 95% soak with ethanol 3 hours.The frequency of supersound extraction is 20kHz, ultrasound intensity 5W/cm 2, extract 30 ℃ of temperature, 2 hours extraction time.Collect extracting solution after extraction is finished, the 5000rpm centrifugalize is got the clear liquor concentrating under reduced pressure and is got faint yellow spore oil with spore powder special odor, yield 24.08%, total triterpene contents 23.01% (with respect to the ursolic acid meter), acid value 16.8.
Embodiment 3
Get 2kg the Ganoderma spore powder of breaking cellular wall in the supersound extraction still, add 20 liters of chloroforms and soaked 1 hour.The frequency of supersound extraction is 50kHz, ultrasound intensity 0.3W/cm 2, extract 40 ℃ of temperature, 2 hours extraction time.Collect extracting solution after extraction is finished, the 8000rpm centrifugalize is got the clear liquor concentrating under reduced pressure and is got faint yellow spore oil with spore powder special odor, yield 25.46%, total triterpene contents 28.12% (with respect to the ursolic acid meter), acid value 16.9.
Embodiment 4
Get 2kg the Ganoderma spore powder of breaking cellular wall in the supersound extraction still, add 6 liters of ether and soaked 2 hours.The frequency of supersound extraction is 150kHz, ultrasound intensity 8W/cm 2, extract 45 ℃ of temperature, 1 hour extraction time.Collect extracting solution after extraction is finished, the 12000rpm centrifugalize is got clear liquor and is got faint yellow spore oil with spore powder special odor, yield 24.24%, total triterpene contents 20.83% (with respect to the ursolic acid meter), acid value 18.9 through thin film concentration.
Embodiment 5
Get 2kg the Ganoderma spore powder of breaking cellular wall in the supersound extraction still, add 24 liters of acetone and soaked 4 hours.The frequency of supersound extraction is 300kHz, ultrasound intensity 0.5W/cm 2, extract 60 ℃ of temperature, 1 hour extraction time.Collect extracting solution after extraction is finished, sucking filtration is got clear liquid, gets faint yellow spore oil with spore powder special odor, yield 26.23%, total triterpene contents 23.53% (with respect to the ursolic acid meter), acid value 28.5 through thin film concentration.
Embodiment 6
Get 2kg the Ganoderma spore powder of breaking cellular wall in the supersound extraction still, add 16 liters of petroleum ether (30~60 ℃ of boiling ranges) and soaked 1 hour.The frequency of supersound extraction is 500kHz, ultrasound intensity 10W/cm 2, extract 50 ℃ of temperature, 3 hours extraction time.After finishing, extraction collects extracting solution, the 5000rpm centrifugalize, and concentrating under reduced pressure gets faint yellow spore oil with spore powder special odor, yield 25.16%, total triterpene contents 22.45% (with respect to the ursolic acid meter), acid value 21.3.
Embodiment 7
Get 2kg the Ganoderma spore powder of breaking cellular wall in the supersound extraction still, add 12 liters of petroleum ether (30~60 ℃ of boiling ranges).Directly carry out supersound extraction, supersonic frequency is 800kHz, ultrasound intensity 15W/cm 2, extract 50 ℃ of temperature, 3 hours extraction time.After finishing, extraction collects extracting solution, the 5000rpm centrifugalize, and concentrating under reduced pressure gets faint yellow spore oil with spore powder special odor, yield 25.67%, total triterpene contents 23.05% (with respect to the ursolic acid meter), acid value 22.5.
Embodiment 8
Get 2kg the Ganoderma spore powder of breaking cellular wall in the supersound extraction still, add 6 liters of petroleum ether (30~60 ℃ of boiling ranges), soaked 1 hour.The frequency of supersound extraction is 50kHz, ultrasound intensity 0.5W/cm 2, extract 30 ℃ of temperature, 2 hours extraction time.After finishing, extraction collects extracting solution, the 5000rpm centrifugalize, and concentrating under reduced pressure gets faint yellow spore oil with spore powder special odor, yield 26.96%, total triterpene contents 25.88% (with respect to the ursolic acid meter), acid value 16.7.
Embodiment 9
Get 2kg the Ganoderma spore powder of breaking cellular wall in the supersound extraction still, add 10 liters of petroleum ether (30~60 ℃ of boiling ranges), soaked 6 hours.The frequency of supersound extraction is 50kHz, ultrasound intensity 0.5W/cm 2, extract 40 ℃ of temperature, 2 hours extraction time.After finishing, extraction collects extracting solution, the 5000rpm centrifugalize, and concentrating under reduced pressure gets faint yellow spore oil with spore powder special odor, yield 28.54%, total triterpene contents 25.22% (with respect to the ursolic acid meter), acid value 17.6.

Claims (5)

1, a kind of preparation method of Ganoderma spore oil is characterized in that the Ganoderma spore powder with breaking cellular wall is a raw material, soaks 0~6 hour with organic solvent, places the supersound extraction still, is 20~800kHz in supersonic frequency, ultrasound intensity 0.3~15W/cm 2, the w/v of Ganoderma spore powder and solvent is 1: 2~20, extracts under the condition of 10~80 ℃ of temperature, extracts 1/6~6 hour,, gets supernatant liquid and reclaims solvent through centrifugal or sucking filtration through the extracting solution after the supersound extraction, obtains Ganoderma spore oil.
2,, it is characterized in that used organic solvent is petroleum ether, chloroform, ethanol, acetone or ether according to claim 1 described Ganoderma spore oil preparation method.
3, Ganoderma spore oil preparation method according to claim 1 is characterized in that after the said supersound extraction that it is the method that adopts concentrating under reduced pressure or thin film concentration that supernatant liquid reclaims solvent.
4,, it is characterized in that used organic solvent is petroleum ether or chloroform according to claim 1 described Ganoderma spore oil preparation method.
5, the preparation method of Ganoderma spore oil according to claim 1, the condition when it is characterized in that supersound extraction: supersonic frequency is 20~50kHz, ultrasound intensity 0.5~10W/cm 2, the w/v of Ganoderma spore powder and solvent is 1: 5~10, extracts 30~40 ℃ of temperature, 1~2 hour extraction time.
CN 200410052195 2004-11-16 2004-11-16 Ultrasonic extraction method for glossy ganoderma spore oil Active CN1270729C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007068143A1 (en) * 2005-12-13 2007-06-21 Lanqin Yang Preparation of plant oil, crude protein and fiber by water extraction
CN100376660C (en) * 2005-12-30 2008-03-26 北京工商大学 Complex frequency ultrasonic leaching method for spice oleoresin
CN102876447A (en) * 2012-10-17 2013-01-16 青岛农业大学 Goose fat liver oil extracting method
CN103710264A (en) * 2013-12-13 2014-04-09 广西科技大学 Auxiliary additive for wall breaking of Mythic Fungus spores
CN105175238A (en) * 2015-10-28 2015-12-23 中山大学 New component in ganoderma spores and extracting and separating method of new component
CN112138031A (en) * 2020-09-08 2020-12-29 广东都市菜族农业科技有限公司 Preparation method and application of ganoderma lucidum spore powder extract containing ganoderma lucidum triterpene and ganoderma lucidum polysaccharide

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007068143A1 (en) * 2005-12-13 2007-06-21 Lanqin Yang Preparation of plant oil, crude protein and fiber by water extraction
CN100376660C (en) * 2005-12-30 2008-03-26 北京工商大学 Complex frequency ultrasonic leaching method for spice oleoresin
CN102876447A (en) * 2012-10-17 2013-01-16 青岛农业大学 Goose fat liver oil extracting method
CN103710264A (en) * 2013-12-13 2014-04-09 广西科技大学 Auxiliary additive for wall breaking of Mythic Fungus spores
CN103710264B (en) * 2013-12-13 2015-11-04 广西科技大学 A kind of broken wall supplementary additive of Ganoderma spore
CN105175238A (en) * 2015-10-28 2015-12-23 中山大学 New component in ganoderma spores and extracting and separating method of new component
CN105175238B (en) * 2015-10-28 2017-07-18 中山大学 New component and its extraction separation method in a kind of Reishi sporule
CN112138031A (en) * 2020-09-08 2020-12-29 广东都市菜族农业科技有限公司 Preparation method and application of ganoderma lucidum spore powder extract containing ganoderma lucidum triterpene and ganoderma lucidum polysaccharide

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Owner name: GUANGZHOU HANFANG PHARMACEUTICAL CO., LTD.

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Address after: 510240 Haizhuqu District Jiangnan Road, Guangdong, No. 134, No.

Patentee after: Guangzhou Hanfang Pharmaceutical Co., Ltd.

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Patentee before: Hanfang Modem Chinese Traditional Medicine Research Development Co., Ltd., Guang