CN104928030A - Preparation method for plum spice used for cigarette - Google Patents

Abstract

The invention provides a preparation method of plum spice for tobacco, the steps comprising: washing the plum fruit and drying it in the air; crushing the plum fruit and passing it through a 10-mesh sieve to obtain the plum powder; refluxing water to extract and then filtering to obtain the filtrate to obtain the plum fruit Crude extract; add subtilisin after cooling to room temperature, enzymatic hydrolysis to obtain plum enzymatic hydrolysis; add ethanol, stir and settle to obtain plum sedimentation liquid; filter and concentrate, then add water and n-butanol and extract to obtain n-butanol phase extraction liquid; adding propylene glycol after concentration to obtain the plum flavor for tobacco. The invention uses the plum fruit to prepare the plum flavor for tobacco, improves the utilization rate of the plum, and has a simple and environmentally friendly preparation method, and the solvent can be reused to reduce the cost. At the same time, the plum spice for tobacco prepared by the present invention has a rich and vivid aroma, which can significantly improve the aroma of cigarettes, and at the same time, has soft and delicate smoke, increases the sweetness of the mouth and improves the permeability of smoke, and has strong practicability .

Description

A kind of preparation method of plum spice for tobacco

technical field

The invention relates to a preparation method of tobacco flavor, in particular to a preparation method of tobacco plum flavor.

Background technique

Plum is the fruit of the fruit plum plant of the genus Apricot in the Rosaceae family, also known as green plum and sour plum. Plums are rich in nutrients and contain a variety of organic acids (citric acid, malic acid, etc.), vitamins, proteins and other substances necessary for the human body. At the same time, because plums have a sour and sweet fragrance, which is more harmonious with the aroma of cigarettes, plums are often used as tobacco flavors and fragrances to add to cigarettes.

However, at present, most plum flavors for tobacco use plums as raw materials, and through simple extraction, filtration, concentration and other processes, the plum extract is prepared. The plum flavor for tobacco prepared by this method not only has a low utilization rate of raw materials, but also has a low content of active ingredients in the obtained extract, and the characteristic aroma of plum is not strong, so the application effect in cigarettes is not very ideal.

Contents of the invention

The purpose of the present invention is to provide a method for preparing plum flavor for cigarettes according to the deficiencies of the prior art. The preparation method has a high utilization rate of plum, and the prepared plum flavor has a high content of active ingredients, a strong characteristic aroma, and an excellent application effect in cigarettes. good.

The present invention is achieved through the following technical solutions: a method for preparing plum flavor for tobacco, the steps comprising:

(1) After the plum fruit is washed and dried, it is dried at 80-150°C;

(2) crushing the dried plums in step (1) and passing through a 10-mesh sieve to obtain plum powder;

(3) The plum powder in the step (2) is refluxed and extracted with 4-8 times of water by weight, and the filtrate is filtered to obtain the crude plum extract;

(4) Cool the crude plum extract in step (3) to room temperature, add 0.05-0.6% of its weight of subtilisin, and enzymolyze it for 12-72 hours at 35-45°C and stirring speed 60-120r/min Obtain plum enzyme hydrolyzate;

(5) Add 0.5-2 times the weight of ethanol to the plum enzymatic hydrolysis solution in step (4), stir and settle for 24-72h to obtain the plum sedimentation liquid;

(6) concentrating after filtering the plum sedimentation liquid in step (5), adding water and n-butanol and extracting to obtain n-butanol phase extract;

(7) Concentrating the extract in step (6) and adding 5-25% by weight of propylene glycol to obtain the plum flavor for tobacco.

Preferably, the drying in the step (1) is to bake at 80-150° C. until the color is yellowish brown, stop heating after the surface is wrinkled, and then stew until the color is black.

Preferably, in the step (3), the coarse plum powder is extracted by reflux with water for 1-3 times, each time for 1-4 hours, and then the filtrates are combined to obtain a crude plum extract.

Preferably, the subtilisin activity unit in the step (4) is 1.8×10 ⁵ U.

Preferably, the ethanol in the step (5) is an aqueous ethanol solution with a mass concentration of 95%, which is first stirred for 30 minutes and then settled at room temperature for 24-72 hours.

Preferably, the plum sedimentation liquid in the step (6) is filtered with a ceramic membrane of 100nm.

Preferably, the n-butanol phase extract in the step (6) is obtained by adding 2-5 times the water of the concentrated solution and 0.5-4 times the weight of the mixed solution after adding water, and then extracting, and then extracting The aqueous phase is repeatedly extracted 3-6 times with 0.5-4 times the weight of n-butanol, and the n-butanol phase extracts are combined.

The invention uses the plum fruit to prepare the plum flavor for tobacco, improves the utilization rate of the plum, and has a simple and environmentally friendly preparation method, and the solvent can be reused to reduce the cost. At the same time, the present invention uses enzymatic hydrolysis and sedimentation to retain the characteristic aroma of plums during the extraction process of plums, so that the prepared plum spices for tobacco have a rich and vivid aroma, which can significantly improve the aroma of cigarettes, and at the same time have soft and delicate smoke, which increases the flavor of the mouth. The effect of sweetness and improving smoke permeability is very practical.

Detailed ways

The present invention is further illustrated below by specific examples:

Example 1

(1) Wash and dry the ripe fruits, and use a rotary roasting machine to continuously stir and bake them at 120°C until they are evenly dried, the color turns yellowish brown, and the skin is wrinkled, then stop heating, and then stew until the color changes for black.

(2) crush the plums obtained in step (1) and pass through a 10-mesh sieve to obtain plum powder.

(3) Weigh the coarse plum powder obtained in step (2), add 5 times the weight of water to reflux and extract twice, each time for 2.5 hours, and combine the two filtrates to obtain a crude plum extract.

(4) Naturally cool the crude plum extract to room temperature, add 0.2% of its weight of subtilisin (activity unit: 1.8×10 ⁵ U), and continue enzymatic hydrolysis for 48 hours at 35°C with a stirring speed of 90r/min to obtain plums Enzyme solution.

(5) After the enzymatic hydrolysis, add 1.5 times the weight of 95% ethanol solution to the plum enzymatic hydrolysis liquid, stir for 30 min, settle at room temperature for 72 h to obtain the plum sedimentation liquid.

(6) Filter the plum sedimentation liquid in step (5) with a 100nm ceramic membrane, concentrate the membrane filtrate under reduced pressure until it has no ethanol taste, then add 4 times the weight of water, stir evenly, and then add 3 times the weight of the mixed solution The n-butanol is fully mixed to carry out liquid-liquid extraction, and the layers are left to stand to obtain the n-butanol phase extract. The aqueous phase was then repeatedly extracted 5 times with 3 times the weight of n-butanol. Combine the n-butanol phase extract that obtains at every turn and concentrate under reduced pressure to a semi-fluid extract (n-butanol has all been steamed out, and the n-butanol that reclaims can be reused), then add its weight 15% propylene glycol, mix Stir evenly to obtain the plum spice 1 for tobacco.

Example 2

(1) Wash and dry the ripe fruits, and use a rotary roasting machine to continuously stir and bake them at 90°C until they are evenly dried, the color turns yellowish brown, and the skin is wrinkled, then stop heating, and then stew until the color changes for black.

(2) crush the plums obtained in step (1) and pass through a 10-mesh sieve to obtain plum powder.

(3) Weigh the coarse plum powder obtained in step (2), add 4 times the weight of water to reflux and extract three times, each time for 2 hours, and combine the three filtrates to obtain a crude plum extract.

(4) Naturally cool the crude plum extract to room temperature, add 0.05% by weight of subtilisin (activity unit: 1.8×10 ⁵ U), and continue enzymatic hydrolysis for 72 hours at 45°C with a stirring speed of 120r/min to obtain plums Enzyme solution.

(5) After the enzymatic hydrolysis, add 95% ethanol solution twice its weight to the plum enzymatic hydrolysis liquid, stir for 30 min, settle at room temperature for 24 h to obtain the plum sedimentation liquid.

(6) The plum sedimentation liquid in the step (5) is filtered with a 100nm ceramic membrane, and the membrane filtrate is concentrated under reduced pressure until it has no ethanol taste, then adds 2 times the weight of water, stirs evenly, and then adds 0.5 times the weight of the mixed solution The n-butanol is fully mixed to carry out liquid-liquid extraction, and the layers are left to stand to obtain the n-butanol phase extract. The aqueous phase was then repeatedly extracted three times with 4 times the weight of n-butanol. Combine the n-butanol phase extract that obtains at every turn and concentrate under reduced pressure to a semi-flowing extract (n-butanol has all been steamed out, and the n-butanol that reclaims can be reused), then add its weight 10% propylene glycol, mix Stir evenly to obtain the plum spice 2 for tobacco.

Example 3

(1) Wash and dry the ripe fruits, and use a rotary roasting machine to continuously stir and bake them at 80°C until they are evenly dried, the color turns yellowish brown, and the skin is wrinkled, then stop heating, and then stew until the color changes for black.

(2) crush the plums obtained in step (1) and pass through a 10-mesh sieve to obtain plum powder.

(3) Weigh the coarse plum powder obtained in step (2), add 8 times the weight of water to reflux for extraction for 1 hour, and take the filtrate to obtain a crude plum extract.

(4) Naturally cool the crude plum extract to room temperature, add 0.5% of its weight of subtilisin (activity unit: 1.8×10 ⁵ U), and continue enzymatic hydrolysis for 24 hours at 38°C with a stirring speed of 60r/min to obtain plums Enzyme solution.

(5) After the enzymatic hydrolysis, add 95% ethanol solution twice its weight to the plum enzymatic hydrolysis liquid, stir for 30 min, settle at room temperature for 24 h to obtain the plum sedimentation liquid.

(6) Filter the plum sedimentation liquid in step (5) with a 100nm ceramic membrane, concentrate the membrane filtrate under reduced pressure until it has no ethanol taste, then add 4 times its weight of water, stir evenly, and then add 2 times the weight of the mixed solution The n-butanol is fully mixed to carry out liquid-liquid extraction, and the layers are left to stand to obtain the n-butanol phase extract. The aqueous phase was then repeatedly extracted 6 times with 0.5 times the weight of n-butanol. Combine the n-butanol phase extract that obtains at every turn and concentrate under reduced pressure to a semi-flowing extract (n-butanol has all been steamed out, and the n-butanol that reclaims can be reused), then add its weight 25% propylene glycol, mix Stir evenly to obtain the plum spice 3 for tobacco.

Example 4

(1) Wash and dry the ripe fruits, and use a rotary roasting machine to continuously stir and bake them at 100°C until they are evenly dried, the color turns yellowish brown, and the skin is wrinkled, then stop heating, and then stew until the color changes for black.

(2) crush the plums obtained in step (1) and pass through a 10-mesh sieve to obtain plum powder.

(3) Weigh the coarse plum powder obtained in step (2), add 6 times the weight of water to reflux and extract twice, each time for 4 hours, and combine the two filtrates to obtain a crude plum extract.

(4) Naturally cool the crude plum extract to room temperature, add 0.15% of its weight of subtilisin (activity unit: 1.8×10 ⁵ U), and continue enzymatic hydrolysis for 48 hours at 35°C with a stirring speed of 90r/min to obtain plums Enzyme solution.

(5) After the enzymatic hydrolysis, add 95% ethanol solution of 1 times its weight to the plum enzymatic hydrolysis solution, stir for 30 minutes, and settle at room temperature for 24 hours to obtain plum sedimentation liquid.

(6) The plum sedimentation liquid in the step (5) is filtered with a 100nm ceramic membrane, and the membrane filtrate is concentrated under reduced pressure to no ethanol taste, then add 3 times the weight of water, stir evenly, and then add 1.5 times the weight of the mixed solution The n-butanol is fully mixed to carry out liquid-liquid extraction, and the layers are left to stand to obtain the n-butanol phase extract. The aqueous phase was then repeatedly extracted three times with 2 times the weight of n-butanol. Combine the n-butanol phase extract that obtains at every turn and concentrate under reduced pressure to a semi-flowing extract (n-butanol has all been steamed out, and the n-butanol that reclaims can be reused), then add its weight 10% propylene glycol, mix Stir evenly to obtain the plum spice 4 for tobacco.

Example 5

(1) Wash and dry the ripe fruits, and use a rotary roasting machine to continuously stir and bake them at 150°C until they are evenly dried, the color turns yellowish brown, and the skin is wrinkled, then stop heating, and then stew until the color changes for black.

(2) crush the plums obtained in step (1) and pass through a 10-mesh sieve to obtain plum powder.

(3) Weigh the coarse plum powder obtained in step (2), add 5 times the weight of water to reflux and extract twice, each time for 1 hour, and combine the two filtrates to obtain a crude plum extract.

(4) Naturally cool the crude plum extract to room temperature, add 0.6% of its weight of subtilisin (activity unit: 1.8×10 ⁵ U), and continue enzymatic hydrolysis for 12 hours at 45°C with a stirring speed of 60r/min to obtain plums Enzyme solution.

(5) After the enzymatic hydrolysis, add 0.5 times the weight of 95% ethanol solution to the plum enzymatic hydrolysis liquid, stir for 30 min, settle at room temperature for 36 h to obtain the plum sedimentation liquid.

(6) The plum sedimentation liquid in the step (5) is filtered with a 100nm ceramic membrane, and the membrane filtrate is concentrated under reduced pressure until it has no ethanol taste, then 5 times the weight of water is added, stirred evenly, and then 4 times the weight of the mixed solution is added The n-butanol is fully mixed to carry out liquid-liquid extraction, and the layers are left to stand to obtain the n-butanol phase extract. The aqueous phase was then repeatedly extracted 5 times with 0.5 times the weight of n-butanol. Combine the n-butanol phase extract that obtains at every turn and concentrate under reduced pressure to a semi-flowing extract (n-butanol has all steamed out, and the n-butanol that reclaims can be reused), then add its weight 5% propylene glycol, mix Stir evenly to obtain the plum spice 5 for tobacco.

Dissolve the above-mentioned plum spices 1-5 for cigarettes in ethanol or propylene glycol at a ratio of 0.1-1‰ of the weight of shredded tobacco, flakes or tobacco stems, and spray evenly on the shredded tobacco, flakes or stems of cigarettes, and roll them into cigarette sticks . Cigarettes without the plum spice for tobacco of the present invention have a general aroma, the smoke is dry, the mouth feels astringent, and the throat is more irritated. The smoke can increase the sweetness of the mouth, improve the permeability of the smoke, and reduce the irritation of the throat.

Claims (7)

1. a preparation method of plum flavor for cigarettes, the steps comprising: (1) After the plum fruit is washed and dried, it is dried at 80-150°C; (2) crushing the dried plums in step (1) and passing through a 10-mesh sieve to obtain plum powder; (3) The plum powder in the step (2) is refluxed and extracted with 4-8 times of water by weight, and the filtrate is filtered to obtain the crude plum extract; (4) Cool the crude plum extract in step (3) to room temperature, add 0.05-0.6% of its weight of subtilisin, and enzymolyze it for 12-72 hours at 35-45°C and stirring speed 60-120r/min Obtain plum enzyme hydrolyzate; (5) Add 0.5-2 times the weight of ethanol to the plum enzymatic hydrolysis solution in step (4), stir and settle for 24-72h to obtain the plum sedimentation liquid; (6) concentrating after filtering the plum sedimentation liquid in step (5), adding water and n-butanol and extracting to obtain n-butanol phase extract; (7) Concentrating the extract in step (6) and adding 5-25% by weight of propylene glycol to obtain the plum flavor for tobacco. 2. The method for preparing plum flavor for tobacco according to claim 1, characterized in that: the drying in the step (1) is first performed at 80-150°C until the color is yellowish brown, and the surface is wrinkled. Turn off the heat and simmer until the color is black. 3. according to the preparation method of the described tobacco plum spice of claim 1, it is characterized in that: in described step (3), be to reflux extract plum powder with water 1-3 time, each 1-4h, then combine filtrate to obtain Plum crude extract. 4. The method for preparing plum flavor for tobacco according to claim 1, characterized in that: the subtilisin activity unit in the step (4) is 1.8×10 ⁵ U. 5. according to the preparation method of the described cigarette plum flavor of claim 1, it is characterized in that: the ethanol in the described step (5) is the ethanol aqueous solution of 95% mass concentration, first stirs 30min and then settles at room temperature 24-72h . 6. The preparation method of plum flavor for tobacco according to claim 1, characterized in that: the filtration of the plum sedimentation liquid in the step (6) is to filter with a 100nm ceramic membrane. 7. according to the preparation method of the described tobacco plum flavor of claim 1, it is characterized in that: the n-butanol phase extraction liquid in the described step (6) is to add the water of 2-5 times of concentrated liquid weight and the mixed liquid after adding water 0.5-4 times the weight of n-butanol, and then extract the obtained, then repeatedly extract the water phase with 0.5-4 times the weight of n-butanol for 3-6 times, and combine the n-butanol phase extracts.