阅读说明：本技术 复合香料提取方法及应用 (Method for extracting compound spice and application thereof ) 是由 夏玲 周斌 黄青连 李东升 文超 郭昊东 于 2021-09-02 设计创作，主要内容包括：本发明涉及烟草添加剂技术领域,公开了复合香料提取方法及应用。本发明提取方法包含以下步骤：将柿子破碎为柿子浆液；将柿子浆液与烟末、水混合在恒温下浸泡；将浸泡后的混合液进行酶解,得到酶解液；将酶解液过滤离心得到上清液；以及将上清液减压浓缩得到复合香料。本发明将烟末与柿子共同酶解,经过絮凝沉淀,能够除去部分烟碱和鞣酸两种物质。在提取中,不需要额外增加提取提纯步骤和添加其他化学原料或者萃取剂来改善原料问题,生产工艺更简单,能够节约大量的能源,同时也更环保和安全。(The invention relates to the technical field of tobacco additives, and discloses a method for extracting a compound spice and application thereof. The extraction method comprises the following steps: crushing persimmon to obtain persimmon pulp; mixing persimmon pulp with tobacco powder and water, and soaking at constant temperature; carrying out enzymolysis on the soaked mixed solution to obtain an enzymolysis solution; filtering and centrifuging the enzymolysis liquid to obtain supernatant; and concentrating the supernatant under reduced pressure to obtain the compound perfume. The invention carries out enzymolysis on the tobacco powder and the persimmon together, and can remove part of two substances of nicotine and tannic acid through flocculation and precipitation. In the extraction, the problems of raw materials are improved without additionally adding an extraction and purification step and adding other chemical raw materials or an extracting agent, the production process is simpler, a large amount of energy can be saved, and the method is more environment-friendly and safer.)

1. The method for extracting the compound spice is characterized by comprising the following steps of:

crushing persimmon to obtain persimmon pulp;

mixing persimmon pulp with tobacco powder and water, and soaking at constant temperature;

carrying out enzymolysis on the soaked mixed solution to obtain an enzymolysis solution;

filtering and centrifuging the enzymolysis liquid to obtain supernatant; and

and (4) carrying out falling film reduced pressure concentration on the supernatant to obtain the compound spice.

2. The method for extracting complex spice according to claim 1, wherein the mass ratio of the tobacco powder to the persimmon pulp is 1: 8-20 parts of; the mass of the water is 5-10 times of that of the tobacco powder.

3. The method for extracting complex flavor according to claim 1, wherein the soaking is carried out at 40-55 ℃ for 2 hours.

4. The method for extracting the compound spice according to claim 1, wherein the specific method for enzymolysis is as follows: adjusting pH of the soaked enzymolysis solution to 4-5, adding cellulase and pectinase, and stirring at 40-55 deg.C for enzymolysis for 3 hr;

wherein the addition amount of the cellulase is 0.02-0.04% and the addition amount of the pectinase is 0.02-0.04% based on the total weight of the persimmon pulp and the tobacco powder.

5. The method for extracting complex flavor according to claim 1, wherein the specific method of filtration and centrifugation comprises:

adding edible ethanol with the same mass as the water into the enzymolysis liquid, heating to 80 ℃, and stirring for 1 hour;

cooling and filtering the stirred solution, and keeping a filtrate; and

the filtrate was centrifuged to obtain a supernatant.

6. The method for extracting complex perfume according to claim 5, wherein the speed of the centrifugation is 4000r/min and the time is 30 min.

7. The method for extracting complex flavor according to claim 1, wherein the method for concentrating under reduced pressure comprises: adopting falling film concentration process, wherein the vacuum degree is 0.07 Mpa-0.088MPa, the temperature is 60-80 ℃, and the concentration multiple is 5-10 times.

8. A complex flavor obtained by extraction according to any one of claims 1 to 7.

9. The use of the compounded flavor of claim 8 in cigarettes, wherein the compounded flavor is sprayed into cut filler.

10. The use of the compound flavor in cigarettes according to claim 8, wherein the compound flavor is prepared into cigarette water beads, and the cigarette water beads are added into cigarette filter rods.

Technical Field

The invention relates to the technical field of tobacco additives, in particular to an extraction method and application of a compound spice.

Background

The essence and the spice are essential additives for cigarette modulation, and are used for improving the smoking taste of the cigarette, stabilizing the irritation, enriching the cigarette fragrance, determining the style of the cigarette and other functions.

Tobacco extract is a commonly used tobacco additive. The tobacco extract is prepared from tobacco leaf, and has effects of supplementing tobacco characteristic fragrance and transmitting smoke. A large amount of waste tobacco leaves are generated in the tobacco harvesting and production process every year in China, and huge waste is caused. By different process means, the specificity can be directionally adjusted

The qualitative tobacco leaf components are enriched, so that the tobacco leaves of a certain grade, a certain quality or a certain style are supplemented and replaced, and the method plays an important role in relieving the contradiction of high-quality raw material requirements and improving the product quality.

The tobacco extract contains a large amount of nicotine as well as various tobacco aroma components. With the low tar and low nicotine cigarette becoming the mainstream of the market, the tobacco blending process has the advantages that the general cigarette leaf formula already contains enough nicotine ingredients, and when the flavors and fragrances are selected, the flavors and fragrances are not expected to additionally contain a large amount of nicotine. However, in order to make up for the insufficient aroma of some cigarettes or increase the special tobacco aroma characteristics, tobacco extracts are often required to be added. It would be desirable to provide a tobacco extract with reduced nicotine content for use as a tobacco additive material.

Persimmon contains a large amount of saccharides and a plurality of active substances, including carotenoids, flavonoids, fatty acids, phenols, a plurality of amino acids and trace elements, and can be widely used in the fields of medicines, health care, cosmetics and the like.

However, because the tannin extract contains a large amount of tannic acid, the tannin extract is directly extracted and applied to cigarettes, and has heavy astringent taste and heavy flavor, so that the application of the tannin extract in the field of cigarette additives is limited.

Disclosure of Invention

In order to solve the problems in the background art, the invention provides a method for extracting a compound spice and application thereof.

In order to achieve the above purpose, the first technical scheme adopted by the invention is as follows:

the compound spice extraction method comprises the following steps:

crushing persimmon to obtain persimmon pulp;

mixing persimmon pulp with tobacco powder and water, and soaking at constant temperature;

carrying out enzymolysis on the soaked mixed solution to obtain an enzymolysis solution;

filtering and centrifuging the enzymolysis liquid to obtain supernatant; and

concentrating the supernatant under reduced pressure to obtain the compound perfume.

Further, the mass ratio of the tobacco powder to the persimmon pulp is 1: 8-20 parts of; the mass of the water is 5-10 times of that of the tobacco powder.

Further, the soaking method is to soak for 2 hours at the temperature of 40-55 ℃.

Further, the specific method of enzymolysis is as follows: adjusting pH of the soaked enzymolysis solution to 4-5, adding cellulase and pectinase, and stirring at 40-55 deg.C for enzymolysis for 3 hr;

wherein the addition amount of the cellulase is 0.02-0.04% and the addition amount of the pectinase is 0.02-0.04% based on the total weight of the persimmon pulp and the tobacco powder.

Further, the specific method of filtration and centrifugation comprises the following steps:

adding edible ethanol with the same mass as the water into the enzymolysis liquid, heating to 80 ℃, and stirring for 1 hour;

cooling and filtering the stirred solution, and keeping a filtrate; and

the filtrate was centrifuged to obtain a supernatant.

Further, the speed of the centrifugation is 4000r/min, and the time is 30 min.

Further, the method for concentrating under reduced pressure comprises the following steps: adopting falling film concentration process, wherein the vacuum degree is 0.07 Mpa-0.088MPa, the temperature is 60-80 ℃, and the concentration multiple is 5-10 times.

The invention also discloses the composite spice extracted by the method.

The second technical scheme adopted by the invention is as follows:

the application of the compound spice extracted by the method in cigarettes is realized by spraying the compound spice in the single cut tobacco.

The third technical scheme adopted by the invention is as follows:

the application of the compound spice extracted by the method in cigarettes is to prepare the compound spice into the cigarette water blasting bead and add the cigarette water blasting bead into a cigarette filter stick.

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

1. the invention carries out enzymolysis on the tobacco powder and the persimmon together, and can remove part of two substances of nicotine and tannic acid through flocculation and precipitation. In the extraction, the problems of raw materials are improved without additionally adding an extraction and purification step and adding other chemical raw materials or an extracting agent, the production process is simpler, a large amount of energy can be saved, and the method is more environment-friendly and safer.

2. The extraction process of the compound spice adopts low-temperature enzymolysis and reduced-pressure low-temperature concentration, the temperature in the whole extraction process does not exceed 80 ℃, the aroma components in the raw materials are retained, the product can reflect the freshness and natural feeling of the raw materials, and compared with the traditional high-temperature extraction, a large amount of energy can be saved.

3. The extracted compound spice is applied to cigarettes or cigarette substitute products, so that the taste of the cigarettes can be improved, the cigarette fragrance can be increased, and the natural and fresh persimmon fragrance of the cigarettes can be enriched; the extracted composite spice has lower nicotine content, so that the composite spice is used in the cigarette bead blasting and has higher safety performance.

Detailed Description

The present invention is described in detail below by way of examples, and it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The invention is susceptible to numerous insubstantial modifications and adaptations by those skilled in the art in view of the foregoing disclosure.

The invention utilizes the reaction of nicotine and tannic acid in tobacco leaves, flocculates and precipitates, and removes partial nicotine and tannic acid. The self characteristics of the two raw materials are utilized to carry out mixed extraction, so that the problems caused by the self components of the raw materials can be well overcome, and the usability of the raw materials is improved. In the extraction, the problems of raw materials are improved without additionally adding an extraction and purification step and adding other chemical raw materials or an extracting agent, the production process is simpler, a large amount of energy can be saved, and the method is more environment-friendly and safer.

In one embodiment of the present invention, there is provided a complex spice extraction method comprising the steps of: crushing persimmon to obtain persimmon pulp; mixing persimmon pulp with tobacco powder and water, and soaking at constant temperature; carrying out enzymolysis on the soaked mixed solution to obtain an enzymolysis solution; filtering and centrifuging the enzymolysis liquid to obtain supernatant; and concentrating the supernatant under reduced pressure to obtain the compound perfume.

Wherein the mass ratio of the tobacco powder to the persimmon pulp is 1: 8-20 parts of; the mass of the water is 5-10 times of that of the tobacco powder.

In one embodiment, the soaking is carried out at 40-55 deg.C for 2 hours.

In a specific embodiment, the specific method of the enzymatic hydrolysis is as follows: adjusting pH of the soaked enzymolysis solution to 4-5, adding cellulase and pectinase, and stirring at 40-55 deg.C for enzymolysis for 3 hr; wherein the addition amount of the cellulase is 0.02-0.04% and the addition amount of the pectinase is 0.02-0.04% based on the total weight of the persimmon pulp and the tobacco powder.

In one embodiment, the specific method of filtration centrifugation comprises: adding edible ethanol with the same mass as the water into the enzymolysis liquid, heating to 80 ℃, and stirring for 1 hour; cooling and filtering the stirred solution, and keeping a filtrate; and centrifuging the filtrate to obtain a supernatant.

Wherein the speed of centrifugation is 4000r/min, and the time is 30 min.

In one embodiment, the method of concentrating under reduced pressure is: adopting membrane concentration process, wherein the vacuum degree is 0.07 Mpa-0.088MPa, the temperature is 60-80 ℃, and the concentration multiple is 5-10 times.

In another embodiment of the invention, the application of the compound spice in cigarettes is provided, and the compound spice is sprayed in the single cut tobacco.

In another embodiment of the invention, the application of the compound spice in cigarettes is provided, the compound spice is prepared into cigarette water blasting beads, and the cigarette water blasting beads are added into cigarette filter sticks.

In order to better understand the technical scheme provided by the invention, the following specific examples respectively illustrate the extraction method, the application method and the performance test of the compound perfume provided by the above embodiment of the invention.

Example 1

Extracting the compound spice:

cleaning fresh persimmon fruits, adding into a wall breaking machine for crushing, and collecting persimmon pulp for later use; mixing the tobacco powder and the persimmon pulp according to the mass ratio of 1:8, and putting the mixture into a fermentation tank; adding water with the weight 5 times of that of the tobacco powder, and soaking for 2 hours at the constant temperature of 42 ℃; adjusting pH to 4.3, adding 0.02% of cellulase and 0.02% of pectinase according to the mass ratio of the total weight of the tobacco powder and the persimmon pulp, and stirring at a constant temperature of 45 ℃ for enzymolysis for 3 hours; adding 95% of edible ethanol by mass, wherein the mass of the edible ethanol is the same as that of the added water; stirring at constant temperature of 80 deg.C for 1 hr, naturally cooling, and filtering to obtain filtrate and residue; centrifuging the filtrate to obtain extract clear solution, wherein the centrifugation speed is 4000r/min, and the centrifugation time is 30 min; and (3) carrying out reduced pressure concentration on the filtrate by falling film concentration equipment to obtain a composite extract, wherein in the falling film concentration process, the vacuum degree is 0.08 MPa, the temperature is kept at 65 ℃, and the concentration multiple is 5 times.

Example 2

Extracting the compound spice:

cleaning fresh persimmon fruits, adding into a wall breaking machine for crushing, and collecting persimmon pulp for later use; mixing the tobacco powder and the persimmon pulp according to the mass ratio of 1:15, and putting the mixture into a fermentation tank; adding water with the weight 8 times of that of the tobacco powder, and soaking for 2 hours at the constant temperature of 50 ℃; adjusting pH to 5, adding cellulase 0.04% and pectase 0.03% in terms of the mass ratio of the total weight of the tobacco powder and the persimmon pulp, stirring at a constant temperature of 50 deg.C for enzymolysis for 3 h; adding 95% of edible ethanol by mass, wherein the mass of the edible ethanol is the same as that of the added water; stirring at constant temperature of 80 deg.C for 1 hr, naturally cooling, and filtering to obtain filtrate and residue; centrifuging the filtrate to obtain extract clear solution, wherein the centrifugation speed is 4000r/min, and the centrifugation time is 30 min; and (3) carrying out reduced pressure concentration on the filtrate through falling film concentration equipment to obtain a composite extract, wherein in the falling film concentration process, the vacuum degree is 0.07 MPa, the temperature is kept at 70 ℃, and the concentration multiple is 7 times.

Example 3

Extracting the compound spice:

cleaning fresh persimmon fruits, adding into a wall breaking machine for crushing, and collecting persimmon pulp for later use; mixing the tobacco powder and the persimmon pulp according to the mass ratio of 1:20, and putting the mixture into a fermentation tank; adding water with the weight 10 times of that of the tobacco powder, and soaking for 2 hours at the constant temperature of 55 ℃; adjusting pH to 4.8, adding 0.03% of cellulase and 0.03% of pectinase according to the mass ratio of the total weight of the tobacco powder and the persimmon pulp, and stirring at a constant temperature of 55 ℃ for enzymolysis for 3 hours; adding 95% of edible ethanol by mass, wherein the mass of the edible ethanol is the same as that of the added water; stirring at constant temperature of 80 deg.C for 1 hr, naturally cooling, and filtering to obtain filtrate and residue; centrifuging the filtrate to obtain extract clear solution, wherein the centrifugation speed is 4000r/min, and the centrifugation time is 30 min; and (3) carrying out reduced pressure concentration on the filtrate by falling film concentration equipment to obtain a composite extract, wherein in the falling film concentration process, the vacuum degree is 0.088MPa, the temperature is kept at 80 ℃, and the concentration multiple is 10 times.

Comparative example 1

Compared with the embodiment 2, the difference is that the addition of the tobacco powder is eliminated, and the rest components and the process are the same as the embodiment 2.

Comparative example 2

The persimmon essence prepared by the method of example 3 in Chinese patent CN108219939A is adopted.

Comparative example 3

Compared with the example 2, the difference is that the addition of the persimmon is eliminated, and the rest components and the process are the same as the example 2.

Examples of the experiments

The content of nicotine and tannic acid of the samples obtained in the comparative examples 1-3 of the grades 1-3 of the examples is detected by the following specific detection method:

1. the nicotine detection adopts YC/T246-2008 tobacco and tobacco product nicotine determination gas chromatography. The detection instrument is gas chromatography.

2. The tannin is detected by a spectrophotometric method for determining the tannin content in NY/T1600-2008 fruits, vegetables and products thereof.

The results are shown in Table 1.

TABLE 1 (content per 100 g sample, unit g)

。

As can be seen from table 1, when the composite extract of tobacco leaves was added to the persimmon syrup, the tannin content was significantly reduced, while the nicotine content was significantly reduced.

Application example 1

The samples obtained in the above examples and comparative examples are applied to cigarettes, and the effect after application is detected, and the specific method is as follows:

taking a plurality of single cut tobaccos, placing the cut tobaccos in a constant temperature and humidity box with the temperature of 22 +/-2 ℃ and the relative humidity of 60 +/-5 percent for balancing for 48 hours, and then averagely dividing the cut tobaccos into 20 parts and 50g of each part;

0.1g of each of the samples of examples 1 to 3 and comparative examples 1 to 3 was taken, and each sample was diluted with 2 mL of water; each diluted sample is sprayed into each 100 g of cut tobacco according to 0.1% of the mass of each cut tobacco (the balance water is 12% +/-1%), and 2 mL of water is directly sprayed into the cut tobacco in a blank control sample. The balanced tobacco shreds were rolled into a cigarette tube according to the standard of total weight (0.80 + -0.01) g of each cigarette, 8 cigarette evaluation experts in the technical center of the organization company were compared and scored according to the standard of blank sample, and the results are shown in Table 2.

TABLE 2

。

As can be seen from Table 2, the effect of applying the extracted compound spice to cigarettes is obvious. Has the effects of improving the taste of the cigarette, increasing the cigarette fragrance, enriching the natural persimmon aroma of the cigarette and reducing the pungency of the cigarette.

Application example 2

The samples obtained in the above examples and comparative examples are prepared into cigarette water blasting beads to be applied to cigarettes, and the effect after application is detected. And directly preparing the cigarette water blasting bead with water as a blank control sample. The preparation of the water blasting beads is carried out according to the method of the embodiment 2 in the Chinese patent CN 201811372831.6. And placing the prepared water blasting beads in a cigarette filter stick or an external cigarette holder, and performing pinching blasting in the cigarette smoking process to act on the cigarette for cigarette smoking evaluation. 8 cigarette evaluation experts of the technical center of the organization company compare and evaluate the blank samples by taking the blank samples as a standard, and the results are shown in Table 3.

TABLE 3

。

As can be seen from the data in Table 3, the water exploded beads prepared by the composite extract have obvious effect when applied to cigarettes. The persimmon fruit-containing cigarette has the effects of improving the taste of cigarettes, increasing the fragrance of the cigarettes, increasing the moist feeling of the cigarettes, enriching the natural persimmon fruit fragrance of the cigarettes and reducing the pungent taste of the cigarettes.

Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.