阅读说明：本技术 一种烟草水提浸膏的制备方法 (Preparation method of tobacco water extract ) 是由 张强 孔宁川 陈婉 徐重军 王乃定 王浩雅 王夸平 杨培香 吴恒 高则睿 蒋卓芳 于 2021-02-09 设计创作，主要内容包括：本发明公开了一种烟草水提浸膏的制备方法,包括如下步骤：步骤(1)：将烟草提取液进行第一正渗透浓缩处理,得到烟草浓缩液,其中,烟草浓缩液的固含量为40％～60％；步骤(2)：对烟草浓缩液进行冷冻干燥处理,得到浸膏初品和冷阱冷凝液,其中,浸膏初品的固含量大于或等于72％；步骤(3)：对冷阱冷凝液进行第二正渗透浓缩处理,得到浓缩冷凝物,其中,第二正渗透浓缩处理的浓缩倍数大于或等于20倍；步骤(4)：将浓缩冷凝物回填至浸膏初品中,即得到烟草水提浸膏。本公开的烟草水提浸膏的制备方法制得到的烟草水提浸膏中的挥发性致香成分损失少,含量较减压蒸发浓缩增加30％以上,浸膏嗅香质量明显提升,且保质期长。(The invention discloses a preparation method of a tobacco water extract, which comprises the following steps: step (1): carrying out first forward osmosis concentration treatment on the tobacco extract to obtain a tobacco concentrated solution, wherein the solid content of the tobacco concentrated solution is 40-60%; step (2): freeze-drying the tobacco concentrated solution to obtain an extract primary product and cold trap condensate, wherein the solid content of the extract primary product is greater than or equal to 72%; and (3): performing second forward osmosis concentration treatment on the cold trap condensate to obtain a concentrated condensate, wherein the concentration multiple of the second forward osmosis concentration treatment is more than or equal to 20 times; and (4): backfilling the concentrated condensate into the primary extract product to obtain the tobacco water extract. The tobacco water extract prepared by the preparation method of the tobacco water extract disclosed by the invention has the advantages that the loss of volatile aroma components is less, the content is increased by more than 30% compared with that of the tobacco water extract prepared by reduced pressure evaporation and concentration, the quality of the aroma of the extract is obviously improved, and the quality guarantee period is long.)

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

step (1): carrying out first forward osmosis concentration treatment on the tobacco extract to obtain a tobacco concentrated solution, wherein the solid content of the tobacco concentrated solution is 40-60%;

step (2): freeze-drying the tobacco concentrated solution to obtain an extract primary product and cold trap condensate, wherein the solid content of the extract primary product is greater than or equal to 72%;

and (3): performing second forward osmosis concentration treatment on the cold trap condensate to obtain a concentrated condensate, wherein the concentration multiple of the second forward osmosis concentration treatment is more than or equal to 20 times;

and (4): backfilling the concentrated condensate into the primary extract product to obtain the tobacco water extract.

2. The method for preparing tobacco water extract according to claim 1, wherein the tobacco extract is filtered before the first forward osmosis concentration in step (1).

3. The method for preparing tobacco water extract according to claim 2, wherein the filtering treatment in the step (1) adopts a 200-mesh ceramic membrane to filter the tobacco extract.

4. The method for preparing tobacco water extract according to claim 1, wherein the drawing agent of the first forward osmosis concentration treatment in the step (1) is at least one of saturated sodium chloride solution, glycerin and propylene glycol.

5. The method for preparing tobacco water extract according to claim 1, wherein the first forward osmosis concentration treatment in the step (1) is a multi-stage concentration treatment.

6. The method for preparing tobacco water extract according to claim 1, wherein the freeze-drying treatment in the step (2) is as follows:

pre-freezing to-10 to-50 deg.c, controlling the vacuum degree to 2-50 Pa, and raising the temperature at 2-12 deg.c/hr.

7. The method for preparing tobacco water extract according to claim 1, wherein the drawing agent of the second forward osmosis concentration treatment in the step (3) is at least one of saturated sodium chloride solution, glycerin and propylene glycol.

8. The method for preparing the tobacco water extract according to claim 1, wherein the solid content of the tobacco water extract in the step (4) is more than or equal to 70%.

Technical Field

The invention relates to the field of tobacco extracts, in particular to a preparation method of a tobacco water extract.

Background

The tobacco water extract is prepared by taking tobacco as a raw material and water as an extraction solvent, and is commonly used for manufacturing cigarette flavoring or heating cigarette core materials.

The existing tobacco water extract is prepared by adopting a mode of concentrating a tobacco extract by reduced pressure evaporation. In the process of reduced pressure evaporation concentration, the tobacco volatile aroma components in the extracting solution enter the condensate of steam along with the evaporation of water to cause loss, and the heat-sensitive substances in the extracting solution are easy to generate reactions such as polymerization, decomposition and the like to denature, so that the tobacco aroma components of the tobacco water extract prepared in the reduced pressure evaporation concentration mode have lower content and poorer quality of smell.

Therefore, how to provide a preparation method of a water extract capable of effectively reducing the loss of the tobacco aroma components becomes a technical problem to be solved urgently in the field.

Disclosure of Invention

The invention aims to provide a novel technical scheme of a preparation method of a tobacco water extract capable of effectively reducing the loss of tobacco aroma components.

According to the first aspect of the invention, a preparation method of a tobacco water extract is provided.

The preparation method of the tobacco water extract comprises the following steps:

step (1): carrying out first forward osmosis concentration treatment on the tobacco extract to obtain a tobacco concentrated solution, wherein the solid content of the tobacco concentrated solution is 40-60%;

step (2): freeze-drying the tobacco concentrated solution to obtain an extract primary product and cold trap condensate, wherein the solid content of the extract primary product is greater than or equal to 72%;

and (3): performing second forward osmosis concentration treatment on the cold trap condensate to obtain a concentrated condensate, wherein the concentration multiple of the second forward osmosis concentration treatment is more than or equal to 20 times;

and (4): backfilling the concentrated condensate into the primary extract product to obtain the tobacco water extract.

Optionally, in the step (1), the tobacco extract is filtered before the first forward osmosis concentration treatment.

Optionally, the filtration treatment in the step (1) adopts a 200-mesh ceramic membrane to filter the tobacco extract.

Optionally, the draw solution of the first forward osmosis concentration treatment in step (1) is at least one of saturated sodium chloride solution, glycerol and propylene glycol.

Optionally, the first forward osmosis concentration treatment in step (1) is a multi-stage concentration treatment.

Optionally, the freeze-drying treatment in the step (2) is specifically as follows:

pre-freezing to-10 to-50 deg.c, controlling the vacuum degree to 2-50 Pa, and raising the temperature at 2-12 deg.c/hr.

Optionally, the drawing agent of the second forward osmosis concentration treatment in step (3) is at least one of saturated sodium chloride solution, glycerol and propylene glycol.

Optionally, the solid content of the tobacco water extract in the step (4) is greater than or equal to 70%.

The tobacco water extract prepared by the preparation method of the tobacco water extract disclosed by the invention has the advantages that the loss of volatile aroma components is less, the content is increased by more than 30% compared with that of the tobacco water extract prepared by reduced pressure evaporation and concentration, the quality of the aroma of the extract is obviously improved, and the quality guarantee period is long.

Detailed Description

Various exemplary embodiments of the present invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise.

The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.

Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate.

In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.

The preparation method of the tobacco water extract comprises the following steps:

step (1): and carrying out first forward osmosis concentration treatment on the tobacco extract to obtain a tobacco concentrated solution, wherein the solid content of the tobacco concentrated solution is 40-60%.

Forward Osmosis (FO) concentration is a utilization mode of Forward Osmosis technology, water migration from a low-Osmosis pressure area to a high-Osmosis pressure area is spontaneously realized by taking osmotic pressure difference of solutions on two sides of a selective Osmosis membrane as a driving force, and the Forward Osmosis membrane has the advantages of low operation pressure, low energy consumption, high material rejection rate, low membrane pollution and the like in the operation process. The forward osmosis concentration treatment of the tobacco extract is beneficial to efficiently retaining the tobacco volatile aroma components in the tobacco extract.

In order to ensure the purity of the tobacco extract, the tobacco extract is filtered in step (1) before the first forward osmosis concentration treatment to remove suspended impurities in the tobacco extract.

Further, the tobacco extract is filtered by a 200-mesh ceramic membrane in the filtering treatment.

In one embodiment of the preparation method of the tobacco water extract, the drawing agent of the first forward osmosis concentration treatment in step (1) is at least one of saturated sodium chloride solution, glycerin and propylene glycol. The skilled person can select a suitable draw agent according to the actual need.

In one embodiment of the method for preparing a tobacco water extract according to the present disclosure, the first forward osmosis concentration treatment in step (1) is a multi-stage concentration treatment.

Step (2): and (3) carrying out freeze drying treatment on the tobacco concentrated solution to obtain an extract primary product and cold trap condensate, wherein the solid content of the extract primary product is greater than or equal to 72%. The extract primary product refers to the product remained on the material tray of the freeze drying machine. Cold trap condensate refers to the product formed by the gases pumped away during the freeze-drying process.

The solid content of the primary extract is controlled to be at least 72%, so that the shelf life of the extract can be prolonged to more than one year under the condition of not adding a preservative.

In order to ensure the freeze-drying effect, the freeze-drying treatment in the step (2) is specifically as follows:

pre-freezing to-10 to-50 deg.c, controlling the vacuum degree to 2-50 Pa, and raising the temperature at 2-12 deg.c/hr.

And (3): and carrying out second forward osmosis concentration treatment on the cold trap condensate to obtain a concentrated condensate, wherein the concentration multiple of the second forward osmosis concentration treatment is greater than or equal to 20 times.

In one embodiment of the preparation method of the tobacco water extract, the drawing agent of the second forward osmosis concentration treatment in step (3) is at least one of saturated sodium chloride solution, glycerin and propylene glycol. The skilled person can select a suitable draw agent according to the actual need.

In particular, the draw agent of the first forward osmosis concentration treatment and the draw agent of the second forward osmosis concentration treatment may be the same or different.

And (4): backfilling the concentrated condensate into the primary extract product to obtain the tobacco water extract.

In one embodiment of the preparation method of the tobacco water extract, in order to more effectively prolong the shelf life of the extract, the solid content of the tobacco water extract in the step (4) is greater than or equal to 70%.

The experimental procedures used in the examples below are conventional unless otherwise specified, the materials and reagents used therein are commercially available, and the equipment used in the experiments are well known to those skilled in the art without otherwise specified.

Example 1

100kg of redried tobacco fragment extracting solution which is filtered by a ceramic membrane of 200 meshes to remove suspended impurities and has the solid content of 4.0 percent is placed in a concentration chamber of a forward osmosis device, three-stage concentration is carried out at room temperature by taking a aquaporin hollow fiber forward osmosis membrane as a separation membrane and a saturated sodium chloride solution as a drawing agent, and the flow rates of the tobacco extracting solution and the drawing agent are both controlled to be 0.9L/min. The first-stage concentration uses 20.0L of saturated sodium chloride solution as an absorbent to concentrate until the solid content is 20 percent; the second concentration uses 8L saturated sodium chloride solution as the drawing agent to concentrate until the solid content is 35 percent; the third concentration uses 3L of saturated sodium chloride solution as the drawing agent to concentrate until the solid content is 40 percent, and 9.9Kg of tobacco concentrated solution is obtained.

Loading 1.225Kg of tobacco concentrated solution into tray, pre-freezing to-50 deg.C in freeze-drying machine at slow speed, controlling vacuum degree at 2-40Pa, heating at 2 deg.C/hr until solid content reaches 72%, to obtain 5.5Kg of extract primary product and 4.2Kg of cold trap condensate.

4.2Kg of cold trap condensate is placed in a concentration chamber of a forward osmosis device, 40 times of concentration is carried out at room temperature by taking an aquaporin hollow fiber forward osmosis membrane as a separation membrane and 1.0Kg of glycerin as an extracting agent, and the flow rates of the cold trap condensate and the extracting agent are both controlled to be 0.8L/min, so as to obtain 100g of concentrated condensate.

And backfilling 100g of the concentrated condensate into 5.5Kg of an extract primary product to obtain 5.6Kg of tobacco water extract S1 with the solid content of 70.5 percent.

Example 2

100kg of K326 tobacco leaf extract which is filtered by a ceramic membrane of 200 meshes to remove suspended impurities and has a solid content of 7.5 percent is placed in a concentration chamber of a forward osmosis device, multi-stage concentration is carried out at room temperature by taking a aquaporin hollow fiber forward osmosis membrane as a separation membrane and taking glycerin as a drawing agent, and the flow rates of the extract and the drawing agent are both controlled to be 0.8L/min. The first-stage concentration uses 5L of glycerin as an extracting agent, when the extracting agent loses the extracting capacity, the same amount of glycerin as the first-stage concentration is replaced as the extracting agent, and the multi-stage concentration is carried out until the solid content is 50 percent, so as to obtain 14.8Kg of tobacco concentrated solution.

Loading 1.24Kg of tobacco concentrated solution into trays per material, pre-freezing to-40 deg.C in a freeze-drying machine at slow speed, controlling vacuum degree at 10-30Pa, and heating at 12 deg.C/hr until solid content reaches 75% to obtain 9.8Kg of primary extract and 4.9Kg of cold trap condensate.

4.9Kg of cold trap condensate is placed in a concentration chamber of a forward osmosis device, and concentrated by 30 times at room temperature by taking an aquaporin hollow fiber forward osmosis membrane as a separation membrane and 1.0Kg of glycerol as a drawing agent to obtain 140g of concentrated condensate.

140g of the concentrated condensate was backfilled into 9.8Kg of the primary extract to obtain 9.9Kg of tobacco water extract S2 with a solid content of 73.5%.

Example 3

100kg of the extract of the Hongda tobacco leaves which is filtered by a ceramic membrane with 200 meshes and has suspended impurities and solid content of 6.2 percent is placed in a concentration chamber of a forward osmosis device, a aquaporin hollow fiber forward osmosis membrane is a separation membrane, a mixed solution (volume ratio is 1:1) of glycerol and propylene glycol is used as a drawing agent, three-stage concentration is carried out at room temperature, and the flow rates of the tobacco extract and the drawing agent are both controlled to be 0.8L/min. In the first-stage concentration, 20L of mixed liquor is used as an extracting agent to be concentrated until the solid content is 25%, in the second-stage concentration, 10L of mixed liquor is used as an extracting agent to be concentrated until the solid content is 50%, and in the third-stage concentration, 5L of mixed liquor is used as an extracting agent to be concentrated until the solid content is 60%, so that 10.2Kg of tobacco concentrated solution is obtained.

Loading 1.28Kg of tobacco concentrated solution into trays per material, pre-freezing to-10 deg.C in a freeze-drying machine at slow speed, controlling vacuum degree at 5-50Pa, and heating at 8 deg.C/hr until solid content of the material reaches 90%, to obtain 6.8Kg of primary extract and 3.3Kg of cold trap condensate.

3.3Kg of cold trap condensate is placed in a concentration chamber of a forward osmosis device, a aquaporin hollow fiber forward osmosis membrane is taken as a separation membrane, 0.4Kg of mixed solution (volume ratio is 1:1) of glycerol and propylene glycol is taken as a drawing agent, and the concentration is carried out at room temperature by 20 times to obtain 130g of concentrated condensate.

130g of the condensed condensate is backfilled into 6.8Kg of the primary extract product to obtain 6.9Kg of tobacco water extract S3 with the solid content of 88.0 percent.

Comparative example 1

100kg of redried tobacco leaf fragment extract (the raw materials are the same as in example 1) which is filtered by a ceramic membrane with 200 meshes to remove suspended impurities and has the solid content of 4.0 percent is subjected to reduced pressure evaporation concentration under the conditions of 50-100mbar and water bath at 60-70 ℃ until the solid content is 71.0 percent, and the tobacco water extract D1 is obtained.

Comparative example 2

100kg of K326 tobacco leaf extract (the raw materials are the same as the example 2) which is filtered by a ceramic membrane with 200 meshes and has suspended impurities and solid content of 7.5 percent is subjected to reduced pressure evaporation concentration under the conditions of 30-90mbar and water bath at 50-70 ℃ until the solid content is 74.0 percent, and the tobacco water extract D2 is obtained.

Comparative example 3

100kg of the extract of the Hongda tobacco leaves (the raw materials are the same as the example 3) which is filtered by a ceramic membrane with 200 meshes and has suspended impurities and solid content of 6.2 percent is subjected to reduced pressure evaporation concentration under 70 to 150mbar and water bath at 70 to 80 ℃ until the solid content is 88.0 percent, and the tobacco water extract D3 is obtained.

Sensory evaluation and detection are respectively carried out on the smelly components and the aroma components of the tobacco water extracts S1-S3 and D1-D3, and the results are shown in the following table 1.

TABLE 1 content of the smelling and tobacco aroma components of the aqueous tobacco extract

As can be seen from Table 1, the tobacco water extract S1-S3 has higher content of aroma components compared with the tobacco water extract D1-D3 prepared by traditional reduced pressure evaporation and concentration, the content of benzyl alcohol and phenethyl alcohol in the tobacco water extract is far higher than that in the tobacco water extract D1-D3 prepared by traditional reduced pressure evaporation and concentration, the important aroma components of tobaccos such as damascenone, dihydroactinidiolide and megastigmatrienone are also obviously improved, and the aroma components are obviously improved. Moreover, compared with the traditional tobacco water extract D1-D3 prepared by reduced pressure evaporation and concentration, the tobacco water extract S1-S3 has stronger natural tobacco flavor, is positively correlated with the content of aroma components, and is also obviously improved in the aspect of smell and fragrance components.

Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustrative purposes only and are not intended to limit the scope of the present invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.