CN110511815A - A kind of Lignum Aquilariae Resinatum extract and the preparation method and application thereof - Google Patents
A kind of Lignum Aquilariae Resinatum extract and the preparation method and application thereof Download PDFInfo
- Publication number
- CN110511815A CN110511815A CN201910804981.8A CN201910804981A CN110511815A CN 110511815 A CN110511815 A CN 110511815A CN 201910804981 A CN201910804981 A CN 201910804981A CN 110511815 A CN110511815 A CN 110511815A
- Authority
- CN
- China
- Prior art keywords
- lignum aquilariae
- aquilariae resinatum
- resinatum extract
- extract
- added
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000284 extract Substances 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 241000271309 Aquilaria crassna Species 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 43
- 108090000790 Enzymes Proteins 0.000 claims abstract description 38
- 102000004190 Enzymes Human genes 0.000 claims abstract description 38
- 229940088598 enzyme Drugs 0.000 claims abstract description 38
- 239000003054 catalyst Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 26
- 108010059892 Cellulase Proteins 0.000 claims abstract description 22
- 229940106157 cellulase Drugs 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 239000007853 buffer solution Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000007791 liquid phase Substances 0.000 claims abstract description 13
- 238000005360 mashing Methods 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000001976 enzyme digestion Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 239000003094 microcapsule Substances 0.000 claims description 13
- 230000000694 effects Effects 0.000 claims description 12
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- 229920000642 polymer Polymers 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000007832 Na2SO4 Substances 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 6
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- 235000020679 tap water Nutrition 0.000 claims description 4
- 241000934790 Daphne mezereum Species 0.000 claims description 3
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- 238000006047 enzymatic hydrolysis reaction Methods 0.000 abstract description 3
- 230000006378 damage Effects 0.000 abstract description 2
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 239000011701 zinc Substances 0.000 description 11
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 10
- 229910052725 zinc Inorganic materials 0.000 description 10
- 229910052742 iron Inorganic materials 0.000 description 9
- 238000011084 recovery Methods 0.000 description 9
- 239000003863 metallic catalyst Substances 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
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- UCIZEPSSPDXSJA-UHFFFAOYSA-N [Na].C(C)(=O)O.C(C)(=O)[O-].[NH4+] Chemical compound [Na].C(C)(=O)O.C(C)(=O)[O-].[NH4+] UCIZEPSSPDXSJA-UHFFFAOYSA-N 0.000 description 6
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 150000004777 chromones Chemical class 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
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- 239000000126 substance Substances 0.000 description 5
- 150000001491 aromatic compounds Chemical class 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 241000208125 Nicotiana Species 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 3
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 3
- 229960000583 acetic acid Drugs 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- WPADUSLPIFNQSF-UHFFFAOYSA-M [NH4+].[Na+].CC([O-])=O.CC([O-])=O Chemical compound [NH4+].[Na+].CC([O-])=O.CC([O-])=O WPADUSLPIFNQSF-UHFFFAOYSA-M 0.000 description 2
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- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
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- 238000005303 weighing Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- BDKZHNJTLHOSDW-UHFFFAOYSA-N [Na].CC(O)=O Chemical compound [Na].CC(O)=O BDKZHNJTLHOSDW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- ISPYRSDWRDQNSW-UHFFFAOYSA-L manganese(II) sulfate monohydrate Chemical compound O.[Mn+2].[O-]S([O-])(=O)=O ISPYRSDWRDQNSW-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
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- A01N25/28—Microcapsules or nanocapsules
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
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- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
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- A61K36/83—Thymelaeaceae (Mezereum family), e.g. leatherwood or false ohelo
- A61K36/835—Aquilaria
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- A61K8/9783—Angiosperms [Magnoliophyta]
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- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
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Abstract
The invention discloses a kind of Lignum Aquilariae Resinatum extracts and the preparation method and application thereof.Method includes the following steps: (1) mixes eaglewood powder with buffer solution agglomerating to that can hold with a firm grip, microwave treatment is then carried out；(2) in the eaglewood powder after cellulase, pectase and mashing enzyme catalyst to be added to microwave treatment, then it is 1:8~24 that buffer solution to solid-to-liquid ratio, which is added, then enzyme digestion reaction is carried out in water bath with thermostatic control, it is inactivated to high-temperature-hot-water after reaction, it is separated by solid-liquid separation, it takes liquid phase to be extracted, and extract liquor is dry, filtering, concentration, obtains Lignum Aquilariae Resinatum extract.The method of the present invention is using microwave-assisted enzymatic hydrolysis and adds enzyme catalyst, its extraction process is simple, the destruction that can be saved extraction time, improve yield, reduce effective component, after its further microencapsulation, its volatilization can be prevented, decomposes and goes bad, and then expands its use scope.
Description
Technical field
The present invention relates to plant extraction technical field, in particular to a kind of Lignum Aquilariae Resinatum extract and the preparation method and application thereof.
Background technique
Lignum Aquilariae Resinatum extract is the substances such as oil, rouge, alcohol, wax, terpenes made of being refined after extraction as precious agalloch eaglewood,
It is the essence place of agalloch eaglewood.Lignum Aquilariae Resinatum extract has multi-efficiency to human body: sesquiterpenoids is living for agalloch eaglewood main pharmacological
Property one of ingredient, there is CNS inhibition tranquilizing soporific and digestion promoting function；Chromone compounds have higher specificity, are agalloch eaglewood
The important indicator ingredient of quality evaluation；Aromatic compound is the main source of agalloch eaglewood special aroma.The extract of agalloch eaglewood can
To be the important source material of the fragrant paper of manufacture hair, perfume, cosmetics, medical treatment and tobacco business etc..Because agalloch eaglewood is expensive, from agalloch eaglewood
Middle extraction Lignum Aquilariae Resinatum extract becomes the necessary ways for making full use of agalloch eaglewood.
Application No. is 201510177749.8 Chinese patents to disclose a kind of preparation method of agilawood essential oil.It is by agalloch eaglewood
Wood powder is added in solvent, is obtained mixture and is carried out microwave irradiation, heating extraction obtains agilawood essential oil.The technique need to be with largely having
Solvent seriously pollutes environment.Application No. is 201910072417.1 Chinese patents to disclose a kind of the efficient of agilawood essential oil
Extracting method.After agalloch eaglewood is carried out microwave reaction by it, enzyme digestion reaction first is carried out with cellulase, uses filter residue after separation of solid and liquid
Pectase extracts, and is extracted again after separation of solid and liquid with alkali protease.Although the extraction process increases essential oil yield, but
Time-consuming, cumbersome, drug expends big, unsuitable production implementation.
Lignum Aquilariae Resinatum extract is mainly used in the fragrant product of production, perfume, formula Chinese medicine and other products.Good Lignum Aquilariae Resinatum extract can
Up to 30000~50000 dollars/liter.Agalloch eaglewood has antibacterial, calmness, the pharmacological actions such as spasmolysis, ease pain, relieving asthma, being depressured, fragrance
It can make one to feel that whole body is happy, passages through which vital energy circulates is submissive, and mechanism of qi reconciles.Lignum Aquilariae Resinatum extract extracts not only operating procedure complexity, consumption at present
Duration, and recovery rate is extremely low, seriously hinders Lignum Aquilariae Resinatum extract and extracts industrialization and its scale application.Therefore, it is necessary to
Develop a kind of efficient, quick Lignum Aquilariae Resinatum extract extraction process.
Summary of the invention
The primary purpose of the present invention is that the shortcomings that overcoming the prior art and deficiency, provide a kind of preparation of Lignum Aquilariae Resinatum extract
Method.
Another object of the present invention is to provide the Lignum Aquilariae Resinatum extracts that the method is prepared.
A further object of the present invention is to provide the applications of the Lignum Aquilariae Resinatum extract.
The purpose of the invention is achieved by the following technical solution: a kind of preparation method of Lignum Aquilariae Resinatum extract, including following step
It is rapid:
(1) eaglewood powder is mixed agglomerating to that can hold with a firm grip with buffer solution, then carries out microwave treatment；
(2) cellulase, pectase and mashing enzyme catalyst are added in the eaglewood powder after microwave treatment, then plus
Entering buffer solution to solid-to-liquid ratio is 1:8~24 (g:ml), then enzyme digestion reaction is carried out in water bath with thermostatic control, to high temperature after reaction
Hot water inactivation, is separated by solid-liquid separation, liquid phase is taken to be extracted, and extract liquor is dry, filtering, concentration, obtains Lignum Aquilariae Resinatum extract.
Buffer solution described in step (1) and (2) is acetic acid-sodium acetate solution of pH 4.0~5.5；Preferably pH
4.0~4.5 acetic acid-sodium acetate solution；More preferably acetic acid-sodium acetate solution of pH 4.0.
Acetic acid-sodium acetate solution configuration method of the pH 4.0 is as follows: by 54.4g sodium acetate (CH3COONa.3H2O)
It is soluble in water, 92ml glacial acetic acid is added, water is added to complement to 1000ml.
Eaglewood powder described in step (1) is the eaglewood powder of 20~80 mesh；Preferably agalloch eaglewood wood chip is cleaned, is dried in the air
20~80 mesh eaglewood powders that dry, crushing obtains.
The dosage of buffer solution described in step (1) is to match 1.245~1.255ml (preferably by every gram of eaglewood powder
For the calculating of 1.25ml) buffer solution.
The condition of microwave treatment described in step (1) are as follows: 250~750W microwave treatment, 0.5~5min.
The enzyme activity of cellulase described in step (2) is 400u/mg, and the dosage of the cellulase is by described in every gram
Eaglewood powder adds 1~3mg cellulase and calculates.
The enzyme activity of pectase described in step (2) is 500u/mg, and the dosage of the pectase is by agalloch eaglewood described in every gram
Wood powder adds 0.4~3mg (preferably 0.4~2mg) pectase and calculates.
Mashing enzyme catalyst described in step (2) is the mashing enzymatic purchased from Guangzhou Jia Ao Biotechnology Co., Ltd
Agent is the enzyme catalyst rich in divalent metals such as magnesium, zinc, calcium, manganese.
It is account for the eaglewood powder quality 2~12% that the dosage of enzyme catalyst is beaten described in step (2).
The condition of enzyme digestion reaction described in step (2) are as follows: 1~5h is digested at 50 DEG C.
Extraction described in step (2) is to be extracted using petroleum ether, and liquid phase and petroleum ether volume ratio are 2~10:1
(preferably 4:1).
Drying described in step (2) is using anhydrous Na2SO4It is dried.
Concentration described in step (2) be by the following method realize: under vacuum conditions with Rotary Evaporators 40 DEG C,
It is concentrated under 25r/min, being concentrated to condensation nozzle does not have liquid drippage that can stop being concentrated.
A kind of Lignum Aquilariae Resinatum extract is prepared by method described in any of the above embodiments.
Application of the Lignum Aquilariae Resinatum extract in microcapsules of the preparation containing Lignum Aquilariae Resinatum extract.
A kind of microcapsules containing Lignum Aquilariae Resinatum extract, are prepared via a method which to obtain:
(a) urea is dissolved into formalin, is reacted in 70 ± 5 DEG C of stirred in water bath, obtains performed polymer (as wall
Material)；
(b) surfactant is added in above-mentioned Lignum Aquilariae Resinatum extract, is uniformly mixed, obtained containing Lignum Aquilariae Resinatum extract
Lotion；
(c) performed polymer obtained in step (a) is added to the lotion obtained in step (b) containing Lignum Aquilariae Resinatum extract
In, pH to 1.8 ± 0.2 is adjusted, and deionized water is added, reaction is cleaned up, obtained to completion of cure under the conditions of 34 ± 1 DEG C
To the microcapsules containing Lignum Aquilariae Resinatum extract.
Formalin described in step (a) is the formalin of 37wt%；Preferably pH 8.0, the formaldehyde of 37wt% are molten
Liquid.
The temperature being stirred to react described in step (a) is preferably 70 DEG C.
The mass ratio of urea described in step (a) and formaldehyde is 1.00:2.68.
The condition of stirring described in step (a) are as follows: 500rpm stirs 1~1.5h；Preferably 500rpm stirs 1h.
Surfactant described in step (b) is surfactant EMA；Preferably concentration is mass percent 2.5%
Surfactant EMA.
The mass ratio of surfactant described in step (b) and Lignum Aquilariae Resinatum extract is preferably 0.15~0.16:10.
The speed of stirring described in step (b) is 1000rpm.
The mass ratio of performed polymer described in step (c) and the Lignum Aquilariae Resinatum extract is 0.8~2.5:1.
The mass ratio of deionized water described in step (c) and the Lignum Aquilariae Resinatum extract is 1:15~16；Preferably 1:
15.5。
Addition deionized water described in step (c) is realized preferably by following steps: first addition accounts for the agalloch eaglewood and mentions
2.5 times of amount of substance of deionized water is taken, then accounts for the Lignum Aquilariae Resinatum extract quality 1.5~5 every 15min addition at timed intervals
Deionized water again；It is more preferably achieved by the steps of: the deionization for accounting for 2.5 times of the Lignum Aquilariae Resinatum extract quality is first added
Then water sequentially adds every 15min at timed intervals in 1 hour and accounts for 1.5 times of the Lignum Aquilariae Resinatum extract quality, and 1.5 times, 5
Times, 5 times of deionized water.
PH described in step (c) is preferably 1.8.
The time of reaction described in step (c) is 3~4h；Preferably 3h.
Cleaning described in step (c) is successively to clean cleaning with the tap water of pH 3~5 and deionized water；Preferably use
The tap water of pH 3~5 is cleaned with deionized water after cleaning up and is cleaned 1~2 time.
The Lignum Aquilariae Resinatum extract or the microcapsules containing Lignum Aquilariae Resinatum extract are in food industry, pesticide, medicine, coating, spinning
It knits, the application in daily cosmetics or Field of Tobacco.
The present invention has the following advantages and effects with respect to the prior art:
(1) present invention improves over existing extraction of essential oil technique, extraction process is simple, and easily operated, use is microwave-assisted
Digest and add enzyme catalyst, plant tissue can be decomposed in a mild condition, can save extraction time, improve yield, reduce have
The destruction of ingredient is imitated, the energy is saved.
(2) the Lignum Aquilariae Resinatum extract yield after extracting is high, aromatic flavour.
(3) Lignum Aquilariae Resinatum extract is a kind of with volatile liquid, essential oil of extraction is carried out microencapsulation to this, not only
It can prevent it from volatilizing and decomposing, is rotten, and expand usage, and fragrance sustained release can be made in use, make
It is greatly improved, is can be applied in medicine, food industry, pesticide, coating, weaving, daily cosmetics and tobacco business with effect.
Detailed description of the invention
Fig. 1 is mashing enzyme catalyst photo figure involved in the embodiment of the present invention 1~4；Wherein, a is mashing enzyme catalyst
Purchase inventory (delivery receipt)；B is the product information for being beaten enzyme catalyst；C is mashing enzyme catalyst.
Fig. 2 is the appearing diagram for the Lignum Aquilariae Resinatum extract that the present invention is prepared.
Fig. 3 is the microcapsules SEM figure for the natural drying that the present invention is prepared.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method and apparatus.It is following
The test method of specific experiment condition is not specified in embodiment, usually according to conventional laboratory conditions or according to proposed by manufactory
Experiment condition.Unless stated otherwise, agents useful for same and raw material of the present invention can pass through commercially available acquisition.
First agalloch eaglewood wood chip (the natural agilawood wood particle from Vietnam's Nha Trang) is cleaned in the present invention, is dried, is crushed 20
~80 mesh eaglewood powders.
The acetic acid of pH 4.0 involved in the embodiment of the present invention-sodium acetate solution configuration method is as follows: weighing 54.4g acetic acid
Sodium (CH3COONa.3H2O) soluble in water, 92ml glacial acetic acid is added, water is added to complement to 1000ml.
Cellulase involved in the embodiment of the present invention is purchased from Shanghai Yuan Ye Biotechnology Co., Ltd, and article No. is
S10042, enzyme activity 400u/mg；Pectase is purchased from Shanghai Yuan Ye Biotechnology Co., Ltd, article No. S10007, enzyme activity
For 500u/mg.
Surfactant EMA involved in the embodiment of the present invention, the entitled coconut oil diethanol amide of Chinese, sample is powder
Shape, purchased from Co., Ltd in Sigma-Aldrich (Sigma-Aldrich China)；It is configured in embodiment with deionized water
The EMA aqueous solution of 2.5wt%.
Mashing enzyme catalyst involved in the embodiment of the present invention is purchased from Guangzhou Jia Ao Biotechnology Co., Ltd, is rich in
The divalent metals such as magnesium, zinc, calcium, manganese (see Fig. 1).
Embodiment 1
(1) 20 mesh eaglewood powder of 200g is weighed, buffer solution is added, and (sodium acetate-acetic acid ammonium salt solution, pH 4.0 are added
250ml or so) mix, progress microwave treatment agglomerating to that can be held with a firm grip with hand: with 750W reaction 0.5min in micro-wave oven.
(2) 800u/g cellulase is added and (adds 800u cellulase by every gram of eaglewood powder；Press every gram of eaglewood powder
2mg cellulase is added), 400u/g pectase (add 400u pectase by every gram of eaglewood powder；Add by every gram of eaglewood powder
Enter 0.8mg pectase) and the mashing of mass fraction 9% enzyme catalyst (i.e. by 9% addition of eaglewood powder quality), then addition is slow
Solution (sodium acetate-acetic acid ammonium salt solution, pH 4.0) is rushed to solid-to-liquid ratio 1:20 progress constant temperature (50 DEG C) water-bath 2h；Water-bath terminates, and uses
95 DEG C of high-temperature-hot-waters inactivate 8min, and centrifugal solid-liquid separation takes liquid phase petroleum ether (liquid phase and petroleum ether volume ratio 4:1) extraction
3 times, extract liquor anhydrous Na2SO4Dry, filtering, uses Rotary Evaporators low speed (25r/min) at 40 DEG C under vacuum conditions
(being concentrated to condensation nozzle does not have liquid drippage that can stop being concentrated) is concentrated, to obtain Lignum Aquilariae Resinatum extract (Fig. 2), recovery rate
It is 1.32%.(percentage that recovery rate is extract weight and eaglewood powder weight used).
(3) microencapsulation:
1. taking suitable 37wt% formalin, its pH to 8.00 is adjusted, with ureaformaldehyde mass ratio (the i.e. matter of urea and formaldehyde
Amount ratio) it is that 1.00:2.68 weighs urea, it is dissolved in stirring in formalin and extremely dissolves, and this solution is stirred in magneton
It is placed in the case where (500rpm) in the water-bath that preset temperature is 70 DEG C and reacts 1h, obtained performed polymer (as wall material)；
2. weighing 6.275g EMA aqueous solution (concentration 2.5wt%), it is placed in the beaker of 250ml, in the machine of 1000rpm
Under tool stirring, 10g Lignum Aquilariae Resinatum extract is added, obtains the lotion containing Lignum Aquilariae Resinatum extract；
3. performed polymer is added in above-mentioned emulsion, (mass ratio of wall material and Lignum Aquilariae Resinatum extract is 0.8:1, i.e. 10g agalloch eaglewood mentions
Take object that 8g performed polymer is added), and pH to 1.8 is adjusted, then system is heated up, when temperature reaches 34 DEG C, is added a certain amount of
Deionized water (first adds 25ml water, then add 15ml, 15ml, 50ml, 50ml every 15min in 1 hour), then allows above-mentioned
System reacts 3h (note: 3h here does not include 1 hour of above-mentioned addition deionized water) at 34 DEG C, is stirred to react to solidification
Completely, it is cleaned up with the tap water that pH is 3~5, is finally cleaned 1~2 time with deionized water, spontaneously dried and obtain the micro- glue of white
Capsule powder (Fig. 3).
Embodiment 2
(1) 80 mesh eaglewood powder of 200g is weighed, buffer solution is added, and (sodium acetate-acetic acid ammonium salt solution, pH 4.0 are added
250ml or so) mix, progress microwave treatment agglomerating to that can be held with a firm grip with hand.1min is reacted with 650W in micro-wave oven.
(2) 1000u/g cellulase (2.5mg cellulase is added in every gram of eaglewood powder) is added, 600u/g pectase (is pressed
1.2mg pectase is added in every gram of eaglewood powder) and the mashing enzyme catalyst of mass fraction 12%, then add buffer solution (acetic acid
Sodium-ammonium acetate solution, pH 4.0) to solid-to-liquid ratio 1:16 progress constant temperature (50 DEG C) water-bath 3h, water-bath terminates, with 95 DEG C high warm
Water inactivates 8min, and centrifugal solid-liquid separation takes liquid phase petroleum ether (liquid phase and petroleum ether volume ratio 4:1) extraction 3 times, extract liquor
Use anhydrous Na2SO4Dry, filtering, with Rotary Evaporators, low speed (25r/min) is concentrated at 40 DEG C under vacuum conditions, with
Obtain Lignum Aquilariae Resinatum extract, recovery rate 2.40%.
(3) microencapsulation: method with 1 step of embodiment (3), the difference is that: step 3. in wall material and agalloch eaglewood extract
The mass ratio of object is 1:1, obtains white microcapsule powder.
Embodiment 3
(1) 40 mesh eaglewood powder of 200g is weighed, buffer solution is added, and (sodium acetate-acetic acid ammonium salt solution, pH 4.0 are added
250ml or so) mix, progress microwave treatment agglomerating to that can be held with a firm grip with hand.3min is reacted with 450W in micro-wave oven.
(2) 400u/g cellulase (1mg cellulase is added in every gram of eaglewood powder), 200u/g pectase is added (by every
0.4mg pectase is added in gram eaglewood powder) and mass fraction 2% be beaten enzyme catalyst, then add buffer solution (sodium acetate-
Ammonium acetate solution, pH 4.0) to solid-to-liquid ratio 1:8 carry out constant temperature (50 DEG C) water-bath 5h.Water-bath terminates, and is gone out with 95 DEG C of high-temperature-hot-waters
8min living, centrifugal solid-liquid separation take liquid phase petroleum ether (liquid phase and petroleum ether volume ratio 4:1) extraction 3 times, extract liquor nothing
Water Na2SO4Dry, filtering, with Rotary Evaporators, low speed (25r/min) is concentrated at 40 DEG C under vacuum conditions, to obtain
Lignum Aquilariae Resinatum extract, recovery rate 0.67%.
(3) microencapsulation: method with 1 step of embodiment (3), the difference is that: step 3. in wall material and agalloch eaglewood extract
The mass ratio of object is 2:1, obtains white microcapsule powder.
Embodiment 4
(1) 60 mesh eaglewood powder of 200g is weighed, buffer solution is added, and (sodium acetate-acetic acid ammonium salt solution, pH 4.0 are added
250ml or so) mix, progress microwave treatment agglomerating to that can be held with a firm grip with hand.5min is reacted with 250W in micro-wave oven.
(2) 1200u/g cellulase (3mg cellulase is added in every gram of eaglewood powder) is added, 1000u/g pectase (is pressed
2mg pectase is added in every gram of eaglewood powder) and the mashing enzyme catalyst of mass fraction 6%, then add buffer solution (sodium acetate-
Ammonium acetate solution, pH 4.0) to solid-to-liquid ratio 1:24 carry out constant temperature (50 DEG C) water-bath 1h.Water-bath terminates, and is gone out with 95 DEG C of high-temperature-hot-waters
8min living, centrifugal solid-liquid separation.Take liquid phase petroleum ether (liquid phase and petroleum ether volume ratio 4:1) extraction 3 times, extract liquor nothing
Water Na2SO4Dry, filtering, with Rotary Evaporators, low speed (25r/min) is concentrated at 40 DEG C under vacuum conditions, to obtain
Lignum Aquilariae Resinatum extract, recovery rate 0.98%.
(3) microencapsulation: method with 1 step of embodiment (3), the difference is that: step 3. in wall material and agalloch eaglewood extract
The mass ratio of object is 2.5:1, obtains white microcapsule powder.
Effect example 1
Influence of the different enzyme catalysts to Lignum Aquilariae Resinatum extract recovery rate, i.e. other conditions are carried out according to the method for embodiment 2
Under same case, zinc divalent metal catalyst will be contained, iron content trivalent metal catalyst, iron content (trivalent), zinc metallic catalyst, or
Iron content (trivalent), manganese, the enzyme catalyst in zinc metallic catalyst alternative embodiment 2.Different enzyme catalysts mention Lignum Aquilariae Resinatum extract
Take rate as shown in table 1, in which:
(the Zn of divalent containing zinc2+) metallic catalyst be zinc chloride (analyze pure AR, 98%, be purchased from Mike's woods reagent, article No.:
Z820755)；Iron content trivalent (Fe3+) metallic catalyst be ferric sulfate (AR is purchased from Mike's woods reagent, article No.: F821829)；Iron content
(trivalent), zinc metallic catalyst are that ferric sulfate and zinc chloride press metal ion (Fe3+: Zn2+) molar ratio 1:1 is mixed to get；Iron content
(trivalent), manganese, zinc metallic catalyst be ferric sulfate, manganese sulfate monohydrate (analyze pure AR, 99%, be purchased from Mike's woods reagent,
Article No.: M813649) with zinc chloride press metal ion (Fe3+: Mn2+: Zn2+) molar ratio 1:1:1 is mixed to get.
Influence of the different enzyme catalysts of table 1 to Lignum Aquilariae Resinatum extract recovery rate
| Enzyme catalyst | Recovery rate |
| The catalyst of divalent metal containing zinc | 1.28% |
| Iron content trivalent metal catalyst | 0.93% |
| Iron content (trivalent), zinc metallic catalyst | 1.35% |
| Iron content (trivalent), manganese, zinc metallic catalyst | 1.84% |
| Embodiment 2 | 2.40% |
Different metal catalyst has nothing in common with each other to the extraction rate impact of Lignum Aquilariae Resinatum extract as shown in Table 1, different superposition groups
Effect caused by closing also is difficult to it is anticipated that the enzyme catalyst extraction effect in the present invention is best.
Effect example 2
1, GC-MS detection, and microencapsulation application are carried out to the Lignum Aquilariae Resinatum extract that above-described embodiment 2 is prepared.Specifically
Steps are as follows for GC-MS and microencapsulation:
GC-MS detection: chromatographic column is RTX-5MS (30m × 0.25mm × 0.25 μm), and temperature programming is 80 DEG C of holdings
2min rises to 160 DEG C with 20 DEG C/min, rises to 230 DEG C with 2 DEG C/min, then rise to 290 DEG C with 5 DEG C/min, keeps 2min, into
290 DEG C of sample temperature；Carrier gas He, flow velocity 1.0mL/min；Split ratio is 25:1；1 μ L of sample volume.Mass Spectrometry Conditions are EI ion source, electricity
Sub- energy is 70eV.
The Lignum Aquilariae Resinatum extract prepared through the invention it can be seen from 2 Lignum Aquilariae Resinatum extract GC-MS testing result of table contains again
The main plants derived essential oils such as half terpene, chromone class, aromatic are in brown color liquid, aromatic flavour.
2 this method of table prepares Lignum Aquilariae Resinatum extract characteristic component GC-MS analysis
Note: " * " represents aromatic compound in table 2；" # " represents sesquiterpenoids；" ^ " represents fatty acid
Close object；" & " represents chromone compounds, remaining substance is Lignum Aquilariae Resinatum extract, there is pharmacological action.
2, (fiber is only added according to the enzyme digestion reaction that the method for embodiment 2 contain only cellulase and pectase
Plain enzyme and pectase are added without enzyme catalyst and without microwave treatment), and the reaction of the microwave-assisted enzymatic hydrolysis without enzyme catalyst
(i.e. addition cellulase and pectase and progress microwave treatment, but be added without enzyme catalyst).Its Lignum Aquilariae Resinatum extract obtained
In each substance relative amount (being detected by above-mentioned GC-MS) it is as shown in the table respectively.
The constituent content and yield of 3 Lignum Aquilariae Resinatum extract of table
| Method | Chromone compounds | Sesquiterpenoids | Aromatic compound | Lignum Aquilariae Resinatum extract total yield |
| Enzyme digestion reaction | 18.02% | 9.78% | 18.59% | 0.70% |
| Microwave-assisted enzymatic hydrolysis reaction | 20.80% | 11.03% | 17.12% | 1.23% |
| Embodiment 2 | 21.69% | 12.95% | 18.25% | 2.40% |
The main component and content of three kinds of extracting method Lignum Aquilariae Resinatum extracts obtained change there is no larger as shown in Table 3
Become, illustrates that the addition of enzyme catalyst can't destroy the quality of Lignum Aquilariae Resinatum extract.And Lignum Aquilariae Resinatum extract mentions after adding enzyme catalyst
It takes rate to significantly improve and reaches 2.40%, illustrate the extraction that enzyme catalyst facilitates enzyme preparation to Lignum Aquilariae Resinatum extract, i.e., in same item
Under part, the agalloch eaglewood of equivalent is extracted, chromone compounds, sesquiterpenoids chemical combination in the extract that the method for the present invention obtains
The content of object and aromatic compound is higher.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of Lignum Aquilariae Resinatum extract, which comprises the following steps:
(1) eaglewood powder is mixed agglomerating to that can hold with a firm grip with buffer solution, then carries out microwave treatment；
(2) it in the eaglewood powder after cellulase, pectase and mashing enzyme catalyst to be added to microwave treatment, is then added slow
Rushing solution to solid-to-liquid ratio is 1:8~24, then carries out enzyme digestion reaction in water bath with thermostatic control, inactivates to high-temperature-hot-water after reaction,
It is separated by solid-liquid separation, liquid phase is taken to be extracted, and extract liquor is dry, filtering, concentration, obtain Lignum Aquilariae Resinatum extract.
2. the preparation method of Lignum Aquilariae Resinatum extract according to claim 1, it is characterised in that:
Buffer solution described in step (1) and (2) is acetic acid-sodium acetate solution of pH 4.0~5.5；
The enzyme activity of cellulase described in step (2) is 400u/mg, and the dosage of the cellulase is by agalloch eaglewood described in every gram
Wood powder adds 1~3mg cellulase and calculates；
The enzyme activity of pectase described in step (2) is 500u/mg, and the dosage of the pectase is by eaglewood powder described in every gram
0.4~3mg pectase is added to calculate；
It is account for the eaglewood powder quality 2~12% that the dosage of enzyme catalyst is beaten described in step (2).
3. the preparation method of Lignum Aquilariae Resinatum extract according to claim 2, it is characterised in that:
Buffer solution described in step (1) and (2) is acetic acid-sodium acetate solution of pH 4.0~4.5；
The dosage of pectase described in step (2) is to add 0.4~2mg pectase by eaglewood powder described in every gram to calculate.
4. the preparation method of Lignum Aquilariae Resinatum extract according to claim 1, it is characterised in that:
The condition of microwave treatment described in step (1) are as follows: 250~750W microwave treatment, 0.5~5min；
The dosage of buffer solution described in step (1) is based on every gram of eaglewood powder proportion 1.245~1.255ml buffer solution
It calculates.
5. the preparation method of Lignum Aquilariae Resinatum extract according to claim 1, it is characterised in that:
Eaglewood powder described in step (1) is the eaglewood powder of 20~80 mesh；
The condition of enzyme digestion reaction described in step (2) are as follows: 1~5h is digested at 50 DEG C；
Extraction described in step (2) is to be extracted using petroleum ether, and liquid phase and petroleum ether volume ratio are 2~10:1；
Drying described in step (2) is using anhydrous Na2SO4It is dried.
6. a kind of Lignum Aquilariae Resinatum extract, it is characterised in that: be prepared by the described in any item methods of Claims 1 to 5.
7. application of the Lignum Aquilariae Resinatum extract as claimed in claim 6 in microcapsules of the preparation containing Lignum Aquilariae Resinatum extract.
8. a kind of microcapsules containing Lignum Aquilariae Resinatum extract, which is characterized in that be prepared via a method which to obtain:
(a) urea is dissolved into formalin, is reacted in 70 ± 5 DEG C of stirred in water bath, obtains performed polymer；
(b) surfactant is added in Lignum Aquilariae Resinatum extract as claimed in claim 6, is uniformly mixed, obtained containing heavy
The lotion of fragrant extract；
(c) performed polymer obtained in step (a) is added in the lotion obtained in step (b) containing Lignum Aquilariae Resinatum extract, is adjusted
PH to 1.8 ± 0.2 is saved, and deionized water is added, reaction cleans up, contained to completion of cure under the conditions of 34 ± 1 DEG C
The microcapsules of Lignum Aquilariae Resinatum extract.
9. the microcapsules according to claim 8 containing Lignum Aquilariae Resinatum extract, it is characterised in that:
Formalin described in step (a) is the formalin of pH 8.0,37wt%；
The mass ratio of urea described in step (a) and formaldehyde is 1.00:2.68；
The condition of stirring described in step (a) are as follows: 500rpm stirs 1~1.5h；
Surfactant described in step (b) is surfactant EMA；
The mass ratio of surfactant described in step (b) and Lignum Aquilariae Resinatum extract is 0.15~0.16:10；
The mass ratio of performed polymer described in step (c) and the Lignum Aquilariae Resinatum extract is 0.8~2.5:1；
The mass ratio of deionized water described in step (c) and the Lignum Aquilariae Resinatum extract is 1:15~16；
The time of reaction described in step (c) is 3~4h；
Cleaning described in step (c) is successively to clean cleaning with the tap water of pH 3~5 and deionized water.
10. microcapsules of any one of Lignum Aquilariae Resinatum extract as claimed in claim 6 or the claim 8~9 containing Lignum Aquilariae Resinatum extract exist
Application in food industry, pesticide, medicine, coating, weaving, daily cosmetics or Field of Tobacco.
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| CN111321589A (en) * | 2020-03-03 | 2020-06-23 | 刘志强 | Cloth processing technology containing Kyara lignum aquilariae resinatum component |
| CN113046883A (en) * | 2021-03-05 | 2021-06-29 | 李庆生 | Color yarn containing agarol and preparation method thereof |
| CN114732931A (en) * | 2022-05-06 | 2022-07-12 | 广州阜耀生物科技有限公司 | Preparation method of agilawood microcapsule sustained-release granules |
| CN115387129A (en) * | 2022-08-02 | 2022-11-25 | 厦门旭纶成纺织科技有限公司 | Agilawood cloth preparation method |
| CN116459192A (en) * | 2023-05-19 | 2023-07-21 | 广东兆禧健康产业投资有限公司 | Preparation method of aquilaria sinensis extract and toothpaste |
| CN116556098A (en) * | 2023-05-09 | 2023-08-08 | 华南理工大学 | Method for extracting wikstroma flower paper medicine by deep sea compound enzyme and application |
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| CN111321589A (en) * | 2020-03-03 | 2020-06-23 | 刘志强 | Cloth processing technology containing Kyara lignum aquilariae resinatum component |
| CN113046883A (en) * | 2021-03-05 | 2021-06-29 | 李庆生 | Color yarn containing agarol and preparation method thereof |
| CN114732931A (en) * | 2022-05-06 | 2022-07-12 | 广州阜耀生物科技有限公司 | Preparation method of agilawood microcapsule sustained-release granules |
| CN115387129A (en) * | 2022-08-02 | 2022-11-25 | 厦门旭纶成纺织科技有限公司 | Agilawood cloth preparation method |
| CN116556098A (en) * | 2023-05-09 | 2023-08-08 | 华南理工大学 | Method for extracting wikstroma flower paper medicine by deep sea compound enzyme and application |
| CN116459192A (en) * | 2023-05-19 | 2023-07-21 | 广东兆禧健康产业投资有限公司 | Preparation method of aquilaria sinensis extract and toothpaste |
| CN116459192B (en) * | 2023-05-19 | 2023-09-22 | 广东兆禧健康产业投资有限公司 | Preparation method of aquilaria sinensis extract and toothpaste |
| CN118374316A (en) * | 2024-06-26 | 2024-07-23 | 中国林业科学研究院木材工业研究所 | Method for extracting heavy essential oil and agilawood oil through grading pretreatment |
| CN118374316B (en) * | 2024-06-26 | 2024-08-23 | 中国林业科学研究院木材工业研究所 | Method for extracting heavy essential oil and agilawood oil through grading pretreatment |
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