阅读说明：本技术 一种桑葚提取物及其制备方法和应用 (Mulberry extract and preparation method and application thereof ) 是由 赵瑞峰 伍锦鸣 吴启贤 任胜超 饶国华 曾健 王�华 黎玉茗 于 2021-08-05 设计创作，主要内容包括：本发明提供一种桑葚提取物及其制备方法和应用。本发明通过对桑葚选用特定浓度的乙醇进行提取,不仅实现了在较低温度下对桑葚提取,而且提取得到的桑葚提取物具有浓郁的香气,同时还可以简化提取工艺,降低了对设备的要求,有利于大规模生产。制备得到的桑葚提取物香味更加丰富浓郁,将其用于卷烟中,可以进一步增加卷烟的香气丰富度以及抽吸舒适度。(The invention provides a mulberry extract and a preparation method and application thereof. According to the invention, the mulberries are extracted by ethanol with a specific concentration, so that the mulberries are extracted at a lower temperature, the extracted mulberry extract has strong fragrance, the extraction process can be simplified, the requirement on equipment is reduced, and the mass production is facilitated. The prepared mulberry extract has richer and stronger fragrance, and can further increase the fragrance richness and smoking comfort of cigarettes when being used in the cigarettes.)

1. A preparation method of a mulberry extract is characterized by comprising the following steps:

s1, mixing mulberries with water and then homogenizing;

s2, adding ethanol into the product obtained by homogenizing in the S1, uniformly mixing to enable the mass ratio of the ethanol to the water in the system to be 55-85: 100, extracting at 40-50 ℃, filtering, collecting filtrate to obtain a mulberry crude extract, and concentrating the mulberry crude extract at a temperature not higher than 50 ℃ to obtain the mulberry extract.

2. The preparation method of the mulberry extract according to claim 1, wherein in the step S2, the mass ratio of ethanol to water in the system is 60-80: 100.

3. The preparation method of the mulberry extract according to claim 1, wherein in step S2, the mass ratio of ethanol to water in the system is 60: 100.

4. The preparation method of the mulberry extract according to claim 1, wherein in the step S1, the mass ratio of the mulberry to the water is 1: 3-5.

5. The preparation method of the mulberry extract according to claim 1, wherein the temperature of the homogenization in the step S1 is 20-30 ℃.

6. The preparation method of the mulberry extract according to claim 1, wherein the homogenization time in the step S1 is 10-15 min.

7. The preparation method of the mulberry extract according to claim 1, wherein the extraction time in the step S2 is 3-4 hours.

8. The preparation method of the mulberry extract according to claim 1, wherein the concentration in step S2. is performed until the soluble solid content is 15-20 wt%.

9. A mulberry extract, which is prepared by the preparation method according to any one of claims 1 to 8.

10. Use of a mulberry extract according to claim 9 as a cigarette flavour.

Technical Field

The invention belongs to the technical field of cigarettes, and particularly relates to a mulberry extract and a preparation method and application thereof.

Background

Mulberries (Morus alba Linn.) are mature fruits of mulberry trees, have a long cultivation history in China, are distributed in the south and north, have strong adaptability, are sour and sweet and palatable, are preferably large, thick in meat, purplish red and rich in sugar, have a fruit period of 4-6 months, contain rich amino acids, carotene, morin, volatile components, sugar, protein and the like, and have extremely high nutritional value. The mulberry can be used as a medicine, has sweet and cold taste, promotes gastrointestinal digestion, has the functions of nourishing yin and blood, and can resist oxidation, reduce blood sugar and delay senility.

The mulberry can be eaten fresh, can be processed into fruit juice, fruit wine and fruit vinegar, and can also be dried in the sun to prepare dried mulberries which are durable to store. However, the flavor of the mulberry is brought by a plurality of components, and the flavor is greatly changed after processing, so that the original taste is difficult to keep, and thus, the processing method of the mulberry is relatively limited.

In the field of cigarettes, there are also reports of processing a small amount of mulberry into essence or extract. The main method mostly adopts a hot reflux method (such as Chinese patent CN104593150A) for extraction, although the extract prepared by the method can increase the smoking quality of cigarettes and refine smoke, the type and the content of compounds of the extract prepared by a heating method have certain influence on the aroma quality, and the aroma quality needs to be further improved.

CN110982624A reports that a relatively mild supercritical carbon dioxide extraction method is adopted, and a mulberry essence is obtained by performing supercritical carbon dioxide extraction on mulberry fruit powder prepared by spray drying of mulberry fruit juice. Water, ethanol, propylene glycol or glycerol are also added as entrainer in the process of supercritical carbon dioxide. However, it still undergoes a high temperature treatment of 100 ℃ or more during the spray drying process, and some volatile components, especially flavor substances, in the mulberry have been destroyed.

Therefore, it is required to provide a mulberry extract having a simple preparation process, a richer fragrance, and a strong fragrance.

Disclosure of Invention

The invention aims to solve the problem that the aroma quality of a mulberry extract in the prior art still needs to be improved, and provides a preparation method of the mulberry extract, which is simple in preparation process, richer in aroma and strong in aroma.

Another object of the present invention is to provide the mulberry extract prepared by the preparation method.

The invention also aims to provide application of the mulberry extract as cigarette essence.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of a mulberry extract comprises the following steps:

s1, mixing mulberries with water and then homogenizing;

s2, adding ethanol into the product obtained by homogenizing in the S1, uniformly mixing to enable the mass ratio of the ethanol to the water in the system to be 55-85: 100, extracting at 40-50 ℃, filtering, collecting filtrate to obtain a mulberry crude extract, and concentrating the mulberry crude extract at a temperature not higher than 50 ℃ to obtain the mulberry extract.

The existing mulberry extract mostly adopts a heating reflux method, chemical components with fragrance are separated from the mulberry, the extraction method needs heating, has high requirements on equipment, and can decompose part of compounds with fragrance function at high temperature, and the fragrance is not rich enough.

The inventor discovers through a large number of experimental researches that the mulberry is extracted by ethanol with a certain concentration, so that the mulberry is extracted at a lower temperature, the extracted mulberry extract has strong fragrance, the extraction process can be simplified, the requirement on equipment is lowered, and the mass production is facilitated. The inventor further researches on the product of the mulberry extract and finds that the concentration of ethanol has certain influence on the types and the content of compounds of the mulberry extract, and further influences the aroma texture of the mulberry extract: if the concentration of the ethanol is too low, the concentration of the effective aroma components of the extracted compound is low, and the aroma is not strong; if the concentration of ethanol is too high, components having pungent odor are easily extracted, and the aroma has irritation, which affects the smoking quality. The mulberry extract with richer fragrance can be obtained by extracting with ethanol with specific concentration, and the mulberry extract can further increase the fragrance richness and smoking comfort of cigarettes when being used in the cigarettes.

The homogenization according to the present invention is performed under a sealed condition.

Preferably, in the step S2, the mass ratio of the ethanol to the water in the system is 60-80: 100.

Most preferably, step s2. the mass ratio of ethanol to water in the system is 60: 100.

In step s2. of the present invention, the amount of ethanol in the mass ratio of ethanol to water is calculated based on the amount of absolute ethanol, that is, the mass ratio of ethanol to water is the mass ratio of absolute ethanol to water.

The ethanol used in the invention can be conventional commercially available ethanol, and when the mass ratio of the ethanol to the water is calculated, the amount of the ethanol is converted into anhydrous ethanol according to the content of the commercially available ethanol.

The mulberry of the invention is fresh mulberry or dried mulberry. The fresh mulberry fruits are not easy to store and deteriorate, so that the method is not beneficial to industrialization; compared with fresh mulberries, the dried mulberries have the advantages of convenience in storage, no influence from seasons and the like, so that the dried mulberries are preferably used in the invention.

Preferably, in the step S1, the mulberries are washed by clean water.

Preferably, in the step S1, the mass ratio of the mulberry to the water is 1: 3-5.

Preferably, the temperature of the homogenization in the step S1 is 20-30 ℃.

Preferably, the extraction time in the step S1 is 10-15 min.

Preferably, the extraction time in the step S2 is 3-4 h.

Conventional concentration means can be used in the present invention as long as the temperature during concentration is not higher than 50 ℃. The purpose of controlling this temperature is to prevent significant losses of volatile substances during the concentration process.

The concentration is preferably rotary evaporation.

Preferably, the rotating speed of the rotary evaporation is 60-120 rpm.

Preferably, the temperature of the rotary evaporation is 40-50 ℃.

The rotary evaporation is usually carried out under a near vacuum, preferably at a pressure of around 100 mbar.

Preferably, the concentration is finished until the soluble solid content is 15-20 wt%.

The invention also provides the mulberry extract prepared by the preparation method.

The application of the mulberry extract as cigarette essence is also within the protection scope of the invention.

When the mulberry extract is used as cigarette essence, the mulberry extract can be directly added into cigarette tobacco shreds. The specific method comprises the following steps: diluting the mulberry extract by 2-5 per mill of the weight of the cigarette tobacco shreds, and then uniformly spraying the mulberry extract on the tobacco shreds.

Compared with the prior art, the invention has the following beneficial effects:

according to the invention, the mulberry is extracted by using ethanol with a specific concentration, so that the obtained mulberry extract has strong fragrance, the extraction process is simplified, the requirement on equipment is reduced, and the mass production is facilitated. The prepared mulberry extract has richer and stronger fragrance, and can further increase the fragrance richness and smoking comfort of cigarettes when being used in the cigarettes.

Drawings

Fig. 1 is a spectrum of a compound component of a mulberry extract prepared in example 1;

fig. 2 is a spectrum of the compound components of the mulberry extract prepared in example 2;

fig. 3 is a spectrum of a compound component of the mulberry extract prepared in comparative example 1;

fig. 4 is a spectrum of the compound components of the mulberry extract prepared in comparative example 3.

Detailed Description

The present invention will be further described with reference to the following specific examples and drawings, which are not intended to limit the invention in any manner. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated. Unless otherwise indicated, reagents and materials used in the present invention are commercially available.

In the examples, the ethanol used was absolute ethanol.

Example 1

The embodiment provides a mulberry extract, and a preparation method thereof comprises the following steps:

s1, cleaning and drying dried mulberries with water, uniformly mixing 10g of cleaned dried mulberries with 50g of water, and homogenizing at 25 ℃ for 10min under a sealed condition;

s2, adding 30g of ethanol into the product obtained in the S1 homogenizing step, uniformly mixing (namely, the concentration of the ethanol in an extractant solution consisting of the ethanol and the water is 60 wt%), keeping the sealing condition, extracting at 50 ℃ for 3 hours, carrying out suction filtration to obtain a filtrate, namely a mulberry crude extract, and carrying out rotary evaporation on the mulberry crude extract at the rotating speed of 40 ℃, 100mbar and 60rpm until the soluble solid content is 15 wt% to obtain the mulberry extract.

Example 2

This example provides a mulberry extract, which was prepared by a method different from that of example 1 in that the amount of ethanol added in step s2 was replaced with 32g (i.e., the concentration of ethanol in an extractant solution composed of ethanol and water was 80 wt%).

Example 3

This example provides a mulberry extract, which was prepared by a method different from that of example 1 in that the temperature for homogenization in step s1 was replaced with 30 ℃.

Example 4

This example provides a mulberry extract, which was prepared by the method different from example 1 in that the time for homogenization in step s1 was replaced with 15 min.

Example 5

This example provides a mulberry extract, which was prepared by the method different from example 1 in that the temperature of extraction in step s2. was replaced with 40 ℃.

Example 6

This example provides a mulberry extract, which was prepared by the method different from example 1 in that the extraction time in step s2. was replaced with 5 hours.

Comparative example 1

This comparative example provides a mulberry extract, which is different from example 1 in that the amount of ethanol added in step s2. is 45g (i.e., the concentration of ethanol in an extractant solution composed of ethanol and water is 90 wt%).

Comparative example 2

This comparative example provides a mulberry extract, which is different from example 1 in that the amount of ethanol added in step s2. is 25g (i.e., the concentration of ethanol in an extractant solution composed of ethanol and water is 50 wt%).

Comparative example 3

The comparison example provides a mulberry extract, which is obtained by extracting according to a conventional hot reflux method, and comprises the following preparation steps:

s1, cleaning dried mulberries for later use;

s2, uniformly mixing 10g of S1. cleaned dried mulberry and 50g of water, and homogenizing at 28 ℃ for 10min under a sealed condition to obtain mulberry pulp;

s3, adding 30g of ethanol into the mulberry fruit pulp obtained in the S2, heating to 95 ℃, refluxing for 3h at 95 ℃, and filtering to obtain a filtrate;

s4, rotatably evaporating the filtrate obtained in the step S3 at 40 ℃ and 60rpm until the soluble solid content is 15 wt% to obtain the mulberry extract.

Comparative example 4

The comparative example provides a mulberry extract, which is obtained by extracting according to a supercritical carbon dioxide extraction method in patent CN110982624A, namely: extracting mulberry fruit powder prepared by spray drying mulberry fruit juice with supercritical carbon dioxide, taking 60 wt% ethanol water solution as an entrainer, wherein the weight ratio of the entrainer to the supercritical carbon dioxide is 1:4, and collecting the mulberry extract in a separation kettle.

Performance testing

1. Analyzing the components of the compounds in the mulberry extract: the mulberry extracts prepared in the above examples and comparative examples are detected by using an SPME-GC-MS method, and the specific detection conditions are as follows:

GC-MS analysis conditions used DB-WAX capillary chromatography column (30 m.times.0.25 μm);

inlet temperature: 250 ℃;

temperature rising procedure: 70 ℃, 1min → 70-190 ℃ (the heating rate is 5 ℃/min) → 190-250 ℃ (the heating rate is 20 ℃/min) → 250 ℃, 20 min;

carrier gas: helium (99.99%);

flow rate: 1.2 mL/min; sample introduction amount: 1 mu L of the solution;

the split ratio is as follows: 200: 1;

an ionization mode: EI; ionization energy: 70 eV;

ion source temperature: 230 ℃;

mass scan range: 30 to 350 amu.

And using a Wiley spectrum library to determine the character with the similarity higher than 85%. The results of the tests are shown in FIGS. 1 to 4 and Table 1.

2. Evaluation of application effect of the mulberry extract as a fragrant raw material in cigarettes:

the mulberry extracts prepared in the above examples and comparative examples are respectively and uniformly injected into single blank trial-produced cigarettes, the addition amount of the mulberry extract is 2 per mill of the weight of tobacco shreds, the obtained cigarettes are stood in a constant temperature and humidity cabinet for 48 hours to obtain cigarette samples, then 7 sensory evaluation experts perform smoking evaluation on the cigarette samples, the aroma richness, the smoke concentration and the smoking strength of the cigarette samples are subjected to scoring evaluation according to 1-10 points, and the scoring and the averaging are performed, wherein the higher the score is, the better the effect is. The evaluation results are shown in Table 2.

TABLE 1 Mulberry extract composition and content

TABLE 2 cigarette evaluation results

As can be seen from fig. 1 to 4 and table 1, the types of compounds, especially terpene compounds, are significantly increased when the extraction method (examples 1 to 6) of the present invention is selected compared with the types of mulberry extracts obtained by the conventional reflux method (comparative example 3), and when the terpene compounds are added to cigarettes as flavor raw materials, the aroma richness, smoke concentration and smoking strength are significantly improved, and the flavor is strong, fine and soft, and the taste is fragrant and sweet; the compounds prepared by the conventional reflux method are few in types, so that the aroma richness is poor, the aroma richness, the soft feeling and the like are poor, and the fragrance has certain irritation and light taste; the mulberry extract prepared by the supercritical carbon dioxide method (comparative example 4) is used in cigarettes, and the smoking feeling evaluation result is similar to that of the backflow method.

The increase of terpene compounds is beneficial to improving the richness and the taste of aroma, and the increase of the richness of the aroma is beneficial to covering the irritation brought by other compound components and improving the overall smoking feeling of the cigarette.

From the results of example 1 and comparative example 1 (ethanol concentration is too high, 90 wt%) and comparative example 2 (ethanol concentration is too low, 50 wt%): the comparison example 1 selects ethanol with higher concentration for extraction, so that the obtained mulberry extract is richer in terpene compounds, but when the mulberry extract is applied to cigarettes, certain irritation appears, and the result shows that only the terpene compounds of a specific kind extracted under specific extraction conditions have a certain effect on the increase of the richness of the fragrance; the comparison example 2 selects ethanol with lower concentration for extraction, the concentration of the effective fragrance components in the obtained mulberry extract is obviously reduced, and when the mulberry extract is applied to cigarettes, the fragrance is not strong and the taste is slightly light.

In addition, as can be seen from comparison of examples 1 and 3 to 6 (the compositions of the products of examples 3 to 6 are similar to those of example 1, and the details are shown in table 1), the homogenization temperature and time have no influence on the types of compounds in the mulberry extract, and only have a slight influence on the extraction content of each compound composition, while the concentration of ethanol has a slight influence on the types and content of the compounds in the prepared mulberry extract.

The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.