CN1907303A - Refining ganoderam lucidum spore oil and method for preparing same - Google Patents
Refining ganoderam lucidum spore oil and method for preparing same Download PDFInfo
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Abstract
The invention discloses refined lucid ganoderma spore oil and preparing method through ultrasonic reinforced temporary flow technology, which comprises the following parts: 85-95% organic acid and fatty acid, 0.1-3% ergosterin and 0.05-1.2% triterpenes.
Description
Technical field
The present invention relates to a kind of is a kind of medicine of raw material and health product and preparation method thereof with the plant, and what be specifically related to is refining ganoderam lucidum spore oil and preparation method thereof.
Background technology
Ganoderma spore powder is the spore that the Ganoderma mature period constantly discharges down from cap, and the eighties begins, with regard to the more basic research to Ganoderma and spore powder anti-tumor aspect thereof; To the nineties, states such as the U.S., Japan are applied to Ganoderma clinical, are used for cancer and AIDS (acquired immune deficiency syndrome (AIDS)) treatment aspect, have obtained international research scholar's extensive attention.Recent study and application more are artificial culture's Ganoderma spore powder and extract thereof, and the Ganoderma spore powder main component of reported in literature comprises: fatty acid, sterols, triterpenes, vitamins, carotene, lactone, protein and amino acids, glycopeptide class, alkaloids and inorganic ions etc.According to document [Jiangsu pharmacy and clinical research, 2001,9 (2): 55] report, China scientist discovers that lipid is disease-resistant " main force " of Ganoderma spore.Sporoderm-broken Ganoderma spore is a Ganoderma spore oil with the lipide actives matter of supercritical carbon dioxide extraction.The chemical composition research of relevant Ganoderma spore oil is less, and only Tian Yifu etc. [Chinese oil, 2003,28 (9): 44] has analyzed the fatty acid composition in the Ganoderma spore oil with the GC/MS method, and claims not contain in its Ganoderma spore oil three terpene components.Application for a patent for invention number 99123952.0 titles adopt supercritical CO
2The Ganoderma spore oil that extraction obtains contains triterpene substance 200mg/g, and it adopts supercritical CO application for a patent for invention number 200410017638.2 titles
2The Ganoderma spore oil that extraction obtains contains triterpene substance 200mg/g～500mg/g, and [Acta Pharmaceutica Sinica such as Chen Ruoyun, 1991,26 (4): 267～273] in Bao Dao the national natural science fund subsidy project " Ganoderma lucidum (Leyss. Ex Fr.) Karst. spore powder triterpene chemical constitution study ", adopted the liposoluble extract of 8kg Ganoderma lucidum (Leyss. Ex Fr.) Karst. spore powder to separate the triterpene chemical constituent, the result has only obtained 5 triterpenoids, and total amount is 1.135g, and promptly the yield of triterpene is 0.014% in the liposoluble extract.
The extracting method of Ganoderma spore oil has traditional solvent extraction method, owing to have shortcomings such as extraction efficiency is low, energy consumption is high, time-consuming length, the existing supercritical CO that adopts
2The report and the patent application of extraction are more, as CN144536A, CN1094766C etc., compare with traditional method, have with short production cycle, effective ingredient is survivable, no solvent residue, advantage such as free from environmental pollution.However, supercritical CO
2Higher pressure that the extraction Ganoderma Lucidum Spores Oil Extracted needs and long extraction time, and extract yield instability, yield has bigger shortcomings such as error between criticizing and criticizing.
In addition because Ganoderma spore powder powder body too thin (breaking cellular wall spore powder fineness completely can reach more than 400 orders), at supercritical CO
2Extraction the time, under condition of high voltage, cause material spray easily, not only influence the extraction quality of spore oil, also bring potential safety hazard to production.In order to address this problem, there is report to adopt method of granulating, as patent CN1094766C, its method is that Ganoderma spore powder is added water, gelatin and starch, at room temperature extrusion modling; Patent CN1586295A selects ethanol water 5～95% for use when being granulation, reduce pressure or the hot air drying cyclic drying at 30～50 ℃ in the back of granulating.Though this method has solved the material spray problem, caused the possibility of polluting extract because of adding adjuvant and binding agent, or, directly influenced extract yield because of heating causes the destructive possibility of composition.
The place of production difference of Ganoderma spore powder, the method difference of plantation and the difference of extracting method all influence the composition and the curative effect of the extract yield and the effective ingredient of Ganoderma spore oil.
Summary of the invention
The purpose of this invention is to provide a kind of refining ganoderam lucidum spore oil that clear and definite chemical composition is arranged and preparation method thereof.
Refining ganoderam lucidum spore oil provided by the present invention, contain Ganoderma spore oil esters, fatty acid, ergosterol class, triterpenes components, the weight content of the total organic acids of forming in conjunction with organic acid and fatty acid in its Ganoderma spore oil esters is 85%～95% of a Ganoderma spore oil, and the weight content of ergosterol class is 0.1%～3% of a Ganoderma spore oil; The weight content of triterpenes is 0.05%～1.2% of a Ganoderma spore oil.
The Ganoderma spore oil esters is to be combined with glycerol by organic acid to constitute, and is the main constituent of Ganoderma spore oil, and specific examples of such components is found first for this project researcher and proposed in Ganoderma spore oil; Fatty acid is a free fatty acid in the Ganoderma spore oil, its weight content of gas chromatography determination is about 1.5%～20% of Ganoderma spore oil, in the Ganoderma spore oil esters is total organic acids in conjunction with organic acid and free fatty sum, the Ganoderma spore oil esters is by hydrolysis, the organic acid that obtains, with free fatty, adopt titration measuring, with oleic acid is the content of its total organic acids of criterion calculation, and the weight content of total organic acids is 85%～95% of a Ganoderma spore oil in the Ganoderma spore oil provided by the present invention.
Ergosterol class Determination on content: get Ganoderma spore oil and handle by the silicagel column enrichment, with the ergosterol standard control, adopt determined by ultraviolet spectrophotometry, measure wavelength 282nm, the weight content that contains the ergosterol class in the Ganoderma spore oil with method acquisition of the present invention can reach 0.1%～3.0% of Ganoderma spore oil.
Triterpenes components is the micro constitutent in the Ganoderma spore, and single triterpene is difficult to detect in Ganoderma spore oil.The triterpenes components of Ganoderma spore oil is handled by the silicagel column enrichment, with Ganodenic acid A standard control, adopt determined by ultraviolet spectrophotometry, measure wavelength 254nm, the weight content of triterpenes is that the content of Ganoderma spore oil is 0.05%～1.2% in the Ganoderma spore oil that obtains with method of the present invention.
The ergosterol class is the endemic element in the Ganoderma spore oil, does not contain specific examples of such components in other vegetable oil (except the fungi plant oil); Composition in the said ergosterol class of Ganoderma spore oil of the present invention has ergosterol (Ergosterol), Ergota steroid-7,22-diene-3 β, 5 α, 6 beta-triols, Ergota steroid-7,22-diene-3 β, 5 α, 6 α-triol, Ergota steroid-7,9,22-triolefin-3 β, 5 α, 6 α-triol, Ergota steroid-4,6,8 (14), 22-tetraene-(3)-ketone, ergosterol cetylate etc. are one of Ganoderma spore oil cancer-resisting effective ingredient.Wherein ergosterol is handled by the silicagel column enrichment, with the ergosterol standard control, adopt the HPLC method to measure, the 282nm wavelength detects, and the weight content that contains ergosterol in the Ganoderma spore oil with method acquisition of the present invention can reach 0.04%～1.0% of Ganoderma spore oil.
Triolein is represented one of composition for it in Ganoderma spore oil esters composition, with the triolein standard control, adopt the HPLC method to measure, evaporative light scattering detector detects, and the content of triolein is 20%～35% in the Ganoderma spore oil that obtains with method of the present invention.
For implementing another object of the present invention, the preparation method of the Ganoderma spore oil that is provided is to adopt the supercritical fluid equipment that has installed ultrasonic extraction device additional, promptly extract the preparation method of Ganoderma spore oil, Ganoderma spore powder is carried out extraction separation with the ultrasound-enhanced supercritical fluid technique.
Spore powder raw material with breaking cellular wall adopts one-step-granulating method to make the granule that size is 0.1～0.5cm with dry pressing earlier, places the ultrasound-enhanced supercritical extraction kettle, is 20～80kHz at ultransonic audio frequency, and power is 10～1000W, and the sound intensity is 10～1500W/cm
2Feed CO simultaneously down,
2Supercritical fluid is 40～50 ℃ in extraction temperature, and extracting pressure is 25～35MPa, CO
2Flow is 5.0～40L/h, extract 1～4 hour after, obtain Ganoderma spore oil from the exit discharging of separating still, make with extra care with the supercentrifugal process that per minute 4000～20000 changes.
This method combines ultrasound assisted extraction technique with supercritical Fluid Extraction Technology, use two kinds of technology simultaneously and extract Ganoderma spore oil, reaches and improves oil yield, reduction extraction temperature and pressure, shortens the purpose of extraction time.When adopting the one-step-granulating method dry pressing to granulate, preferred granulator principal pressure is 2～8MPa, and lateral pressure is 0.1～1Mpa.During ultrasound-enhanced supercritical extraction simultaneously, can use flash trapping stage, also can use the multiple stage separation method, feed CO
2Also can add ethanol in the time of supercritical fluid or methanol is made entrainer, to reach the purpose that improves yield, the technology of supercritical fluid extraction also can adopt the disclosed preparation method of CN144536A, CN1094766C.
Beneficial effect of the present invention:
1, the chemical composition of Ganoderma spore oil provided by the present invention is clear, the quality of product easy to control, product purity height.
2, preparation method provided by the present invention combines supersound extraction and supercritical liquid extraction technique, and the extraction ratio of Ganoderma spore oil can improve 15～30% than supercritical fluid extraction.
3, preparation method of the present invention is compared with supercritical fluid extraction, the temperature and pressure in the time of obviously reducing supercritical fluid extraction in identical extraction time; Under identical extraction temperature and pressure, extraction time can be shortened again.
4, the present invention extracts after adopting a step dry-pressing granulation that spore powder with crushed sporoderm is made granule, has solved supercritical CO
2Safety of dashing material during extraction and the incomplete problem of extraction, method of granulating is simple, need not add any adjuvant and binding agent, do not need through heating and exsiccant process yet, avoided because of add adjuvant and binding agent pollute extract or because of heating causes that composition is destructive may, simplify technology, saved production cost.
Further set forth technical scheme of the present invention below by embodiment.
The specific embodiment
Embodiment 1.
One. adopt supercritical fluid extraction
Get that MeiZhou,GuangDong produces, sporoderm-broken rate is at the Ganoderma spore powder of the Ganoderma lucidum (Leyss. Ex Fr.) Karst. 95% or more, granulate with the direct dry-pressing of dry-pressing granulator, principal pressure 2MPa, lateral pressure 0.5MPa makes the granule of 0.1～0.4cm, sieves, sieve removes the fine powder more than 60 orders, fine powder is granulated with method again.Take by weighing the 1kg granule, place the supercritical extraction reactor of 5 liters to extract, 50 ℃ of extracting pressure 30Mpa, extraction temperature, CO
2Flow is 12L/ hour, and the extraction time is 2 hours, obtains Ganoderma spore oil from separating still, separates through 10000 rev/mins high speed centrifugations, obtains refining ganoderam lucidum spore oil, yield 17.8%;
Two. ultrasound-enhanced supercritical fluid extraction method
With experiment condition substantially the same manner as Example 1, but when reaching identical temperature and pressure, open ultrasonic device, frequency of ultrasonic is 15kHz, power is 30W, the sound intensity is 30W, and extraction time is 2 hours, obtains Ganoderma spore oil from extraction-container, separate through 10000 rev/mins high speed centrifugations, obtain refining ganoderam lucidum spore oil, yield 20.5% is compared yield with embodiment 1 and has been improved 15.2%.
Two kinds of method comparative results see the following form 1:
Table 1
| The extraction process condition | The supercritical CO 2 extraction | Strengthen ultrasonic supercritical CO 2 extraction |
| The sound intensity spore oil output yield of the power ultrasonic of the hyperacoustic frequency ultrasonic wave of extraction temperature extraction pressure extraction time CO2 flow | 2 hours 12L/ hour 178g 17.8% of 50 ℃ of 30Mpa | 2 hours 12L/ hour 20kHz 10W 30W/cm of 50 ℃ of 30Mpa 2 205g 20.5％ |
Embodiment 2.
Adopt the experiment condition identical with embodiment 1, unique different be supercritical CO
2Extracted 4 hours, and strengthened ultrasonic supercritical extraction 2 hours, result of the test sees the following form 2:
Table 2
| The extraction process condition | The supercritical CO 2 extraction | Strengthen ultrasonic supercritical CO 2 extraction |
| The sound intensity spore oil output yield of the power ultrasonic that the hyperacoustic frequency of extraction temperature extraction pressure extraction time CO2 flow is ultrasonic | 4 hours 12L/ hour 196g 19.6% of 50 ℃ of 30Mpa | 2 hours 12L/ hour 40kHz 30W 50W/cm of 50 ℃ of 30Mpa 2 219g 21.9％ |
Embodiment 3
Adopt the experiment condition identical with embodiment 1, different is that inventory is 5kg, strengthens 42 ℃ of extracting pressure 23Mpa, the extraction temperature of ultrasonic supercritical extraction, and frequency of ultrasonic is 40kHz, and power is 50W, and the sound intensity is 100W/cm
2, extraction time is 2 hours, result of the test sees the following form 3:
Table 3
| The extraction process condition | The supercritical CO 2 extraction | Strengthen ultrasonic supercritical CO 2 extraction |
| The sound intensity spore oil output yield of the power ultrasonic of the hyperacoustic frequency ultrasonic wave of extraction temperature extraction pressure extraction time CO2 flow | 4 hours 12L/ hour 890g 17.8% of 50 ℃ of 30Mpa | 2 hours 12L/ hour 40kHz 50W 110W/cm of 43 ℃ of 23Mpa 2 1150g 23.0％ |
Embodiment 4.
Ganoderma spore powder behind the 5kg breaking cellular wall directly is pressed into granule with the dry-pressing one-step-granulating method, crosses 60 mesh sieves, remove the fine powder that sifts out, fine powder is granulated with method again.Granulator principal pressure 3MPa, lateral pressure is 0.5MPa.Place the supercritical fluid extraction still that has installed ultrasonic extraction device additional to extract the Ganoderma spore powder after granulating, frequency of ultrasonic is 50kHz, and power is 100W, and the sound intensity is 200W/cm
2The supercritical extraction fluid is CO
2, extraction temperature is 45 ℃, and extracting pressure is 25MPa, and the extraction time is 2 hours, and the extraction flow is 13L/h.
Ganoderma spore powder behind the 5kg breaking cellular wall is directly added in the extraction kettle, extract with condition by above, two kinds of result of the tests see the following form 4:
Table 4
| Dry-pressing is granulated | Do not granulate | |
| Extraction temperature extracting pressure extraction time CO 2The hyperacoustic power spore oil of flow frequency of ultrasonic character spore oil output yield | 2 hours 13L/ hour faint yellow, transparent 1265g 25.3% of 60kHz 100W of 45 ℃ of 25Mpa | 2 hours 13L/ hour 60kHz 100W muddiness of 45 ℃ of 25Mpa, be mixed with spore powder 910g 18.2% |
Embodiment 5:
Identical with the operating process of embodiment 4, different is: inventory is 20kg, and the granulator principal pressure is 4kg, makes the granule of 0.2～0.3cm, supercritical CO
245 ℃ of collection pressure 25Mpa, extraction temperature, frequency of ultrasonic is 60kHz, and power is 500W, and the sound intensity is 900W/cm
2, extraction time is 2 hours, obtains the 5300g Ganoderma spore oil from extraction-container, yield 26.5%.
Embodiment 6:
Identical with the operating process of embodiment 4, different is: inventory is 100kg, and the granulator principal pressure is 5kg, makes the granule of 0.2～0.4cm, supercritical CO
250 ℃ of collection pressure 28Mpa, extraction temperature, frequency of ultrasonic is 80kHz, and power is 1000W, and the sound intensity is 1200W/cm
2, extraction time is 3 hours, obtains the 27300g Ganoderma spore oil from extraction-container, yield 27.3%.
Embodiment 7
Strengthen ultrasonic supercritical CO to using
2The sample of extraction embodiment carries out composition detection, the results are shown in following table 5:
Table 5
| Product is formed | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Total organic acids triolein ergosterol class ergosterol triterpenes | 91.2 31.5 2.94 0.96 1.18 | 85.2 25.5 1.74 0.61 0.81 | 93.3 34.6 0.58 0.23 0.79 | 94.2 31.5 0.34 0.12 0.39 | 85.2 22.5 0.44 0.16 0.24 | 93.3 32.6 0.11 0.05 0.06 |
Claims (4)
1. refining ganoderam lucidum spore oil, it is characterized in that containing Ganoderma spore oil esters, fatty acid, ergosterol class, triterpenes components, the weight content of the total organic acids of forming in conjunction with organic acid and fatty acid in its Ganoderma spore oil esters is 85%～95% of a Ganoderma spore oil, and the weight content of ergosterol class is 0.1%～3% of a Ganoderma spore oil; The weight content of triterpenes is 0.05%～1.2% of a Ganoderma spore oil.
2. by the described Ganoderma spore oil of claim 1, the weight content that it is characterized in that triolein in the Ganoderma spore oil esters is 20%～35% of a Ganoderma spore oil; The weight content of ergosterol is 0.04%～1.0% of a Ganoderma spore oil in the ergosterol constituents.
3. the preparation method of a refining ganoderam lucidum spore oil; it is characterized in that adopting the preparation method of ultrasound-enhanced supercritical fluid extraction; spore powder raw material with breaking cellular wall adopts one-step-granulating method to make the granule that size is 0.1～0.5cm with dry pressing earlier; place the ultrasound-enhanced supercritical extraction kettle; at ultransonic audio frequency is 20～80kHz; power is 10～1000W, and the sound intensity is 0.3～1500W/cm
2Feed CO simultaneously down,
2Supercritical fluid is 40～50 ℃ in extraction temperature, and extracting pressure is 25～35MPa, CO
2Flow is 5.0～40L/h, extract 1～4 hour after, obtain Ganoderma spore oil from the exit discharging of separating still, get refining ganoderam lucidum spore oil through 4000～20000 rev/mins rotating speed centrifugalize.
4. by the preparation method of the described Ganoderma spore oil of claim 3, when it is characterized in that adopting the one-step-granulating method dry pressing to granulate, the granulator principal pressure is 2～8MPa, and lateral pressure is 0.1～1Mpa.
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| CN101967426A (en) * | 2010-10-15 | 2011-02-09 | 王朝臣 | Preparation process and system for ultrasonic reinforced supercritical CO2 extraction of tussah pupa oil |
| CN102058082A (en) * | 2010-11-22 | 2011-05-18 | 晨光生物科技集团股份有限公司 | Efficient extraction and separation technology for effective ingredients of peppers |
| CN102379906A (en) * | 2011-06-22 | 2012-03-21 | 南京中科药业有限公司 | Processing method of improving tumor resistance of ganoderma lucidum spore oil |
| CN101176548B (en) * | 2007-11-30 | 2012-05-09 | 华南理工大学 | Method for preparing low acid value ganoderma lucidum spore oil |
| CN104946383A (en) * | 2015-04-30 | 2015-09-30 | 江苏江大源生态生物科技有限公司 | Method for preparing ganoderma lucidum spores oil through supercritical CO2 composite microwave-assisted extraction |
| CN105628681A (en) * | 2016-04-11 | 2016-06-01 | 惠州市食品药品检验所 | Identification method of ganoderma lucidum spore oil |
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| CN1255519C (en) * | 2003-06-20 | 2006-05-10 | 陈列 | Glossy ganoderma spore oil extracting and refining process |
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| CN101176548B (en) * | 2007-11-30 | 2012-05-09 | 华南理工大学 | Method for preparing low acid value ganoderma lucidum spore oil |
| CN101967426A (en) * | 2010-10-15 | 2011-02-09 | 王朝臣 | Preparation process and system for ultrasonic reinforced supercritical CO2 extraction of tussah pupa oil |
| CN102058082A (en) * | 2010-11-22 | 2011-05-18 | 晨光生物科技集团股份有限公司 | Efficient extraction and separation technology for effective ingredients of peppers |
| CN102379906A (en) * | 2011-06-22 | 2012-03-21 | 南京中科药业有限公司 | Processing method of improving tumor resistance of ganoderma lucidum spore oil |
| CN104946383A (en) * | 2015-04-30 | 2015-09-30 | 江苏江大源生态生物科技有限公司 | Method for preparing ganoderma lucidum spores oil through supercritical CO2 composite microwave-assisted extraction |
| CN104946383B (en) * | 2015-04-30 | 2018-07-03 | 江苏江大源生态生物科技有限公司 | A kind of supercritical CO2The method that composite microwave auxiliary extraction prepares ganoderma lucidum spore oil |
| CN105628681A (en) * | 2016-04-11 | 2016-06-01 | 惠州市食品药品检验所 | Identification method of ganoderma lucidum spore oil |
| WO2023001161A1 (en) * | 2021-07-22 | 2023-01-26 | 广州白云山汉方现代药业有限公司 | Ganoderma spore oil and use thereof in preparation of drug counteracting cancer-related fatigue |
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