阅读说明：本技术 一种沉香提取物及其制备方法与应用 (A kind of Lignum Aquilariae Resinatum extract and the preparation method and application thereof ) 是由 杨仁党 吕晓萍 朱慧霞 于 2019-08-29 设计创作，主要内容包括：本发明公开了一种沉香提取物及其制备方法与应用。该方法包括以下步骤：(1)将沉香木粉与缓冲溶液混合至可握紧成团,然后进行微波处理；(2)将纤维素酶、果胶酶和打浆酶催化剂加入到微波处理后的沉香木粉中,然后加入缓冲溶液至固液比为1：8～24,接着在恒温水浴进行酶解反应,待反应结束后高温热水灭活,固液分离,取液相进行萃取,并将萃取液干燥、过滤、浓缩,得到沉香提取物。本发明方法采用微波辅助酶解并添加酶催化剂,其提取工艺简单,可节省提取时间、提高得率、减少有效成分的破坏,将其进一步微胶囊化后,可防止其挥发、分解和变质,进而扩大其使用范围。(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.)

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.

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).