CN110129824A - A kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol - Google Patents

A kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol Download PDF

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Publication number
CN110129824A
CN110129824A CN201910536884.5A CN201910536884A CN110129824A CN 110129824 A CN110129824 A CN 110129824A CN 201910536884 A CN201910536884 A CN 201910536884A CN 110129824 A CN110129824 A CN 110129824A
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ergosterol
sparassis crispa
electric field
bionics techniques
field preparation
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CN110129824B (en
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陈美英
王国强
何绍东
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Fuqing Firekirin Mushrooms Technology and Development Co Ltd
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Fuqing Firekirin Mushrooms Technology and Development Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J9/00Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B3/00Electrolytic production of organic compounds
    • C25B3/20Processes
    • C25B3/25Reduction

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The method of-half bionics techniques of a kind of electric field preparation Sparassis crispa ergosterol disclosed by the invention, comprising the following steps: (1) take Sparassis crispa fructification, be ground up, sieved, obtain Sparassis crispa powder;(2) under the conditions of external electric field, using pH for 9-10 strong base solution as raw material, saponification at 90 DEG C obtains ergosterol;(3) heavy metal ion desorbed in step described in electroreduction (2) by albuminate;(4) gained mixed liquor in the step (3) is taken, centrifuge separation obtains layer deposition object, middle layer flocculate and supernatant;(5) the middle layer flocculate is taken, using the aqueous solution of ethyl alcohol as extracting solution, weak acid for adjusting pH to 3-4, water-bath is extracted, and filtering obtains filtrate;(6) merge supernatant and filtrate, adjust pH to neutrality, rotary evaporation obtains concentrate, concentrate described in vacuum freeze drying, gained powder, that is, anti-oxidant Sparassis crispa ergosterol, ergosterol recovery rate are high, removing heavy metals and silk ball mycoprotein are removed, property is stablized, through gastrointestinal tract good absorbing.

Description

A kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol
Technical field
The present invention relates to Sparassis crispa fields, and in particular to a kind of-half bionics techniques of electric field preparation Sparassis crispa ergosterol Method.
Background technique
Ergosterol is also known as ergot and stays alcohol, is a kind of feature alcohol contained in fungi, the silk ball bacterial content in edible mushroom It is big and stable, frequently as the primary raw material of calciferol production, it can promote absorption of the human body to pin, phosphorus etc., be conducive to bone shape At, prevention children rachitis, adult osteoporosis and osteomalacia, meanwhile, ergosterol is the weight of microbial cell film Component part is wanted, to the integrality for ensuring cell membrane, the activity of membrane bound enzyme, the mobility of film, cell viability and cell object Matter transport etc. plays an important role, but it meets daylight and the oxidizable yellowly of air, property are unstable.
In the prior art, to the extraction of ergosterol in mostly organic solvent extractionprocess, while extracting ergosterol Also a large amount of foreign matters are extracted, not only consume a large amount of organic solvent, and since ergosterol finally plays correlation by oral administration Health-care effect, organic solvent extractionprocess is extract obtained bad to the adaptability of human body intestinal canal, simultaneously as edible mushroom is easily enriched with Heavy metal, thus through organic solvent extract content of beary metal in resulting extract be also possible to it is exceeded.
Summary of the invention
To solve the above problems, the present invention provides a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol, Ergosterol recovery rate is high, through electric field-semi-bionic extraction method, mixes Sparassis crispa polysaccharide component, removes removing heavy metals and silk ball mycoprotein, Property stabilization is not oxidizable, through gastrointestinal tract good absorbing.
The technical scheme is that a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol is provided, The following steps are included: (1) takes Sparassis crispa fructification, it is ground up, sieved, obtains Sparassis crispa powder;It (2) is 9- with pH under the conditions of external electric field 10 strong base solution is raw material, and saponification at 90 DEG C obtains ergosterol;(3) by being denaturalized in step described in electroreduction (2) The heavy metal ion of albumen desorption;(4) take gained mixed liquor in the step (3), centrifuge separation, obtain layer deposition object, in Fleece condensate and supernatant;(5) the middle layer flocculate is taken, using the aqueous solution of ethyl alcohol as extracting solution, weak acid for adjusting pH to 3-4, water Bath is extracted, and filtering obtains filtrate;(6) merge supernatant and filtrate, adjust pH to neutrality, rotary evaporation obtains concentrate, and vacuum refrigeration is dry The dry concentrate, gained powder, that is, anti-oxidant Sparassis crispa ergosterol.
Preferably, in the step (3), the cathode of electroreduction is stainless steel electrode plate, and anode is graphite electrode plate.
Preferably, in the step (2), external electric field electric field strength is 20-40kv/cm, and pulse is 6 μ s-12 μ s, feed liquid Than for 1:20.
Preferably, the highly basic in the step (2) is one of NaOH or KOH.
Preferably, the weak acid in the step (5) is acetic acid.
Preferably, in the step (4), centrifugal speed 3000-4000r/m, centrifugation time 2-3min.
Preferably, the heavy metal ion in the step (3) is one or more of chromium, lead, arsenic.
Preferably, the volume ratio of ethyl alcohol and water is 2:8 in extracting solution in the step (5).
High-pressure pulse electric is placed in container using food liquid as electrolyte, two discharge electrodes with container edge By high-tension current, the method that electric pulse is processed is generated, the cell wall and cell membrane potential of cell processed can be made moment Disorder changes its permeability, or even can puncture cell wall and cell membrane, brings it about irreversible breaking, and group distributes in cell.
In Sparassis crispa fructification there are two types of ergosterol existences, free state and reference state, the prior art are generally first adopted It is saponified with alcohol alkali, the purpose being saponified to mycelium is the fatty acid removed in mycelium, is added in lye rudimentary It is so that grease and alkali alcoholic solution is formed homogeneous reaction system in order to increase grease solubility in saponification liquor that alcohol, which makees saponification agent, from And the reaction rate of saponification is improved, the extractions such as organic solvent such as petroleum ether, ether wherein unsaponifiable matter is recycled, but this Method not only used a large amount of organic solvent, also will use the organic solvents such as ether or petroleum ether in subsequent extraction process Extractant is made, there is very big security risk in these organic solvents, and cost is also very high in industrialized production, additionally, due to Ergosterol also is soluble in ethyl alcohol, therefore the recovery rate that can lose ergosterol is taken with alcohol alkali carries, ring of this programme in impulse electric field Under border, ergosterol is saponified using aqueous slkali, Electro-pulsing Field is in Sparassis crispa solution, so that oscillation aggravation, wheat when reaction Angle sterol is constantly dissolved out with the destruction of pulse pair cell membrane, is avoided the interface of saponification between the two phases from carrying out, is accelerated alkali Reference state ergosterol in mycelia can be become free state, avoid subsequent extraction process by liquid to the diffusion rate of grease Extractant is made using organic solvents such as ether or petroleum ethers, the safety that ergosterol extracts is improved, in addition also makes production cost Greatly reduce.
The extraction of this programme also imitates the first lye that human gastrointestinal tract is absorbed and carried out and mentions again acid solution i.e. semi-bionic extraction method, alkali The pH value of liquid is functioned simultaneously as close to human body gastric acid using the lye in saponification close to human body intestinal canal, the pH value of acid solution Extractant extracts Sparassis crispa active constituent, as silk ball granulose increases its solubility ratio and examine for oral absorption Consider that degree of dissociation is more important, and silk ball granulose includes beta glucan, with antioxygenic property, and free radical can be removed, it is rear with containing The acid solution of ethyl alcohol extracts purifying to ergosterol, enhances its dissolubility, and with the extracted ergosterol of this programme, there are also big The beta glucan of amount, when external condition causes the unstable oxidation of ergosterol, beta glucan can be first oxidized, and protect etembonate Alcohol, thus keep its property more stable.
After carrying out lye and extracting the effect with impulse electric field, since saponification temperature is higher than 80 DEG C, i.e. the denaturation of protein Temperature, and the pH of lye, but also Sparassis crispa albuminous degeneration is known as flocculate precipitating, silk ball mycoprotein includes sulfoprotein, in silk ball Since there are heavy metal pollutions in growing environment during bacterium growth, and as macro fungi, Sparassis crispa is easily enriched with a huge sum of money Belong to, especially chromium, since sulfoprotein is rich in the small peptide of cysteine, has high affinity to various heavy, it is molecule matter To measure lower, cysteine residues and the high protein of tenor form metallothionein, after protein can be denaturalized, a huge sum of money Category is parsed with the denaturation of sulfoprotein, to be dissolved in solution in ionic state heavy metal, electrolytic reduction is utilized in this programme Enriching heavy metal is inserted into electrode in the sewage containing heavy metal, then passes to the direct current of some strength, heavy metal is in electric field Lower displacement is acted on, heavy metal simple substance is precipitated on the electrode or is enriched near electrode, to remove heavy metal, in cathode, Due to the difference of heavy metal ion electrode potential, heavy metal ion is reduced to heavy metal simple substance in cathode, and mixed liquor is through being centrifuged Afterwards, since heavy metal density is larger, bottommost is fallen to, and the Sparassis crispa residue containing ergosterol forms flocculate and falls to Middle part, and then carry out the separation and removal of heavy metal.
This programme has the beneficial effect that:
(1) highly basic is that the extractant for being used as semi-bionic extraction method does not influence also as the saponification agent for generating ergosterol in this programme In the case where semi-bionic extraction method process, ergosterol is extracted;
(2) electric field destroys Sparassis crispa cell membrane, so that the ergosterol in cell membrane dissolves out, improves semi-bionic extraction method rate, simultaneously Electric field acceleration lye accelerates the progress of saponification to the diffusion rate of grease, keeps its reaction more thorough;
(3) while electric field-saponification, keep silk ball mycoprotein rotten, parse the heavy metal in conjunction with sulfoprotein, recycle original Electric field environment, electroreduction is enriched with heavy metal, obtains free of contamination Sparassis crispa ergosterol extract;
(4) due to utilizing semi-bionic extraction method, the loss of effective component is reduced, not only with respect to the activity of mixture in extraction process Ingredient, also controls the monomer component to be extracted, and in Sparassis crispa ergosterol obtained, granulose containing silk ball can prevent wheat Angle sterol aoxidizes, and enhances the stability of ergosterol.
Detailed description of the invention
Fig. 1 is Determination of ergosterol testing result;
Fig. 2 is ergosterol Detection of Stability result;
Fig. 3 is content of beary metal testing result.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
Sparassis crispa fructification 100g is taken, is ground, 200 meshes are crossed, obtained Sparassis crispa powder is packed into high-pressure pulse device, NaOH solution 2L is added, adjustment solution ph is heating stirring 1h at 9,90 DEG C, the condition of micro-electrolysis reactor is adjusted, so that outside Electric field intensity is 20kv/cm, and pulse is that 6 μ s occur simultaneously so that discharge electrode acts on Sparassis crispa cell membrane Saponification;
The mixed liquor is poured into micro-electrolysis reactor, adjusts the electrode, so that cathode is stainless steel electrode plate, anode is stone Electrode ink plate carries out electroreduction, voltage 1.8V to the resulting mixed liquor of above-mentioned steps, and reaction temperature is 25 DEG C, when reaction Between be that 120min is centrifuged resulting mixed liquor, centrifugal speed 3000r/m after slowly removing cathode electrode, when centrifugation Between be 2min, leave and take supernatant and the i.e. middle layer flocculate of first layer precipitating;
The middle layer flocculate is taken, 200ml ethyl alcohol is added, 800ml acetum adjusts pH to 3, and 1h, mistake are extracted in 40 DEG C of water-baths Filter, takes filtrate;
Merging filtrate and supernatant adjust pH to neutrality, and rotary evaporation obtains concentrate, concentrate described in vacuum freeze drying, gained Powder, that is, anti-oxidant Sparassis crispa ergosterol takes gained powder to carry out Data Detection.
Embodiment 2
Sparassis crispa fructification 100g is taken, is ground, 200 meshes are crossed, obtained Sparassis crispa powder is packed into high-pressure pulse device, KOH solution 2L is added, adjustment solution ph is heating stirring 1h at 10,90 DEG C, the condition of micro-electrolysis reactor is adjusted, so that outside Electric field intensity is 40kv/cm, and pulse is that 12 μ s occur simultaneously so that discharge electrode acts on Sparassis crispa cell membrane Saponification;
The mixed liquor is poured into micro-electrolysis reactor, adjusts the electrode, so that cathode is stainless steel electrode plate, anode is stone Electrode ink plate carries out electroreduction, voltage 1.8V to the resulting mixed liquor of above-mentioned steps, and reaction temperature is 25 DEG C, when reaction Between be that 120min is centrifuged resulting mixed liquor, centrifugal speed 4000r/m after slowly removing cathode electrode, when centrifugation Between be 3min, leave and take supernatant and the i.e. middle layer flocculate of first layer precipitating;
The middle layer flocculate is taken, 200ml ethyl alcohol is added, 800ml acetum adjusts pH to 4, and 1h, mistake are extracted in 40 DEG C of water-baths Filter, takes filtrate;
Merging filtrate and supernatant adjust pH to neutrality, and rotary evaporation obtains concentrate, concentrate described in vacuum freeze drying, gained Powder, that is, anti-oxidant Sparassis crispa ergosterol takes gained powder to carry out Data Detection.
Embodiment 3
Sparassis crispa fructification 100g is taken, is ground, 200 meshes are crossed, obtained Sparassis crispa powder is packed into high-pressure pulse device, KOH solution 2L is added, adjustment solution ph is heating stirring 1h at 10,90 DEG C, the condition of micro-electrolysis reactor is adjusted, so that outside Electric field intensity is 50kv/cm, and pulse is that 10 μ s occur simultaneously so that discharge electrode acts on Sparassis crispa cell membrane Saponification;
The mixed liquor is poured into micro-electrolysis reactor, adjusts the electrode, so that cathode is stainless steel electrode plate, anode is stone Electrode ink plate carries out electroreduction, voltage 1.8V to the resulting mixed liquor of above-mentioned steps, and reaction temperature is 25 DEG C, when reaction Between be that 120min is centrifuged resulting mixed liquor, centrifugal speed 3500r/m after slowly removing cathode electrode, when centrifugation Between be 3min, leave and take supernatant and the i.e. middle layer flocculate of first layer precipitating;
The middle layer flocculate is taken, 200ml ethyl alcohol is added, 800ml acetum adjusts pH to 3.5, and 1h is extracted in 40 DEG C of water-baths, Filtering, takes filtrate;
Merging filtrate and supernatant adjust pH to neutrality, and rotary evaporation obtains concentrate, concentrate described in vacuum freeze drying, gained Powder, that is, anti-oxidant Sparassis crispa ergosterol takes gained powder to carry out Data Detection.
Embodiment 4
Sparassis crispa fructification 100g is taken, is ground, 200 meshes are crossed, KOH solution 2L is added, adjustment solution ph is 10,90 DEG C Lower heating stirring 1h, is centrifuged resulting mixed liquor, centrifugal speed 3500r/m, and centrifugation time 3min takes supernatant 200ml ethyl alcohol is added in above-mentioned precipitating in liquid, and 800ml acetum adjusts pH to 3.5, and 40 DEG C of water-baths are extracted 1h, filtered, Take filtrate;
Merging filtrate and supernatant adjust pH to neutrality, and rotary evaporation obtains concentrate, concentrate described in vacuum freeze drying, gained Powder, that is, anti-oxidant Sparassis crispa ergosterol takes gained powder to carry out Data Detection.
Embodiment 5
Sparassis crispa fructification 100g is taken, is ground, 200 meshes are crossed, KOH solution 2L is added in obtained Sparassis crispa powder, is adjusted Whole solution ph is heating stirring 1h at 10,90 DEG C, and with petroleum ether extraction, rotary evaporation obtains concentrate, vacuum freeze drying institute Concentrate is stated, gained powder, that is, anti-oxidant Sparassis crispa ergosterol takes gained powder to carry out Data Detection.
Embodiment 6
Data Detection is carried out according to known method to powder obtained by above-described embodiment 1-5, above-mentioned powder is dissolved in 1L solution It is detected, Determination of ergosterol testing result such as Fig. 1, the measurement ergosterol of the powder obtained by illumination and oxidizer treatment is stablized Property testing result such as Fig. 2, content of beary metal testing result such as Fig. 3, it is known that the resulting ergosterol recovery rate of this programme is high, content High and property is stablized, heavy metal free residual.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, is all covered by the present invention.

Claims (8)

1. a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol, which comprises the following steps:
(1) Sparassis crispa fructification is taken, is ground up, sieved, Sparassis crispa powder is obtained;
(2) under the conditions of external electric field, using pH for 9-10 strong base solution as raw material, saponification at 90 DEG C obtains free state ergot Sterol;
(3) heavy metal ion desorbed in step described in electroreduction (2) by albuminate;
(4) gained mixed liquor in the step (3) is taken, centrifuge separation obtains layer deposition object, middle layer flocculate and supernatant;
(5) the middle layer flocculate is taken, using the aqueous solution of ethyl alcohol as extracting solution, weak acid for adjusting pH to 3-4, water-bath is extracted, filtering, Obtain filtrate;
(6) merge supernatant and filtrate, adjust pH to neutrality, rotary evaporation obtains concentrate, concentrate described in vacuum freeze drying, institute Obtain powder, that is, anti-oxidant Sparassis crispa ergosterol.
2. a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol according to claim 1, feature exist In in the step (3), the cathode of electroreduction is stainless steel electrode plate, and anode is graphite electrode plate.
3. a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol according to claim 1, feature exist In in the step (2), external electric field electric field strength is 20-40kv/cm, and pulse is 6 μ s-12 μ s, solid-liquid ratio 1:20.
4. a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol according to claim 1, feature exist In the highly basic in the step (2) is one of NaOH or KOH.
5. a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol according to claim 1, feature exist In the weak acid in the step (5) is acetic acid.
6. a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol according to claim 1, feature exist In, in the step (4), centrifugal speed 3000-4000r/m, centrifugation time 2-3min.
7. a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol according to claim 1, feature exist In the heavy metal ion in the step (3) is one or more of chromium, lead, arsenic.
8. a kind of method of-half bionics techniques of electric field preparation Sparassis crispa ergosterol according to claim 1, feature exist In the volume ratio of ethyl alcohol and water is 2:8 in extracting solution in the step (5).
CN201910536884.5A 2019-06-20 2019-06-20 Method for preparing Sparassis crispa ergosterol by electric field-semi-bionic technology Expired - Fee Related CN110129824B (en)

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CN110835149A (en) * 2019-11-26 2020-02-25 上海天汉环境资源有限公司 Method and device for removing heavy metal settlement through tubular column type electric flocculation
CN112679402A (en) * 2021-01-25 2021-04-20 福建万菇生物科技有限公司 Low-pollution sparassis crispa vitamin D2Preparation method of extract

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Publication number Priority date Publication date Assignee Title
CN110835149A (en) * 2019-11-26 2020-02-25 上海天汉环境资源有限公司 Method and device for removing heavy metal settlement through tubular column type electric flocculation
CN112679402A (en) * 2021-01-25 2021-04-20 福建万菇生物科技有限公司 Low-pollution sparassis crispa vitamin D2Preparation method of extract

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