A method for improving the yield of spice preparation and its use

Abstract

The present invention discloses a method for improving the yield of spice preparation, comprising the following steps: (1) vacuum freeze-drying; (2) pulverizing and particle size screening; (3) extraction; (4) filtration and merging; (5) cold setting filtration; (6) vacuum concentration. The present invention also discloses the spice prepared by the above method and the use of the spice for enhancing the sweet and mellow feeling and reducing the irritation of the smoke. The method of the present invention can not only greatly improve the extraction yield of the fragrance raw material, but also shorten the extraction time and save energy consumption.

Description

Technical Field

[0001] The present invention belongs to the technical field of cigarettes, and particularly relates to a method and use for improving the preparation yield of tobacco flavorings. Background Art

[0002] The use of reconstituted tobacco reduces the tar content of cigarettes, resulting in a lighter smoke and a lack of aroma. To maintain the stability of the cigarette leaf blend formula, it is necessary to add flavor to the cigarettes. The flavored cigarettes can not only improve the quality and quantity of the cigarette aroma, enrich the fragrance, but also soften and delicate the smoke, alleviate the pungent and miscellaneous flavors, and inhibit the irritation, thereby improving the smoking quality of the cigarettes.

[0003] The general technology for extracting tobacco flavorings is to first pretreat (dry, crush, etc.) the tobacco flavor raw materials, and then extract their active ingredients by combining extraction, distillation, pressing, absorption, molecular distillation, supercritical extraction and other methods. However, due to the high moisture content of some tobacco flavor raw materials, the extraction yield is low, so it is necessary to dry them. Traditional drying methods such as air drying, sun drying and oven drying have low efficiency or affect the stability of heat-sensitive components in the raw materials. Vacuum freeze-drying is based on quickly freezing and sublimating the moisture in the material under high vacuum and low temperature conditions, which can reduce the moisture content to less than 5%, avoiding surface tension and the degradation of heat-sensitive components in the dried material, and making the material not easy to oxidize. It can not only keep the material with good color, fragrance and nutritional components, but also make the retention rate of components such as polyphenols, flavonoids and vitamin C reach more than 90%. It can also form a loose porous structure inside, better maintaining the original physical properties of the material, and greatly improving the nutritional characteristics and sensory quality of the material (such as fruit and vegetable chips).

[0004] Patent CN2022108533032 discloses a method for preparing flavorings from fresh sour papayas, including steps such as pulp juicing, vacuum freeze-drying, negative-pressure thermal reflux alcohol extraction, forward osmosis concentration, vacuum concentration and flavor blending. Patent CN2022106405805 discloses a method for extracting flavorings from Schisandra chinensis twigs, including vacuum freeze-drying and crushing, extracting the powder with water combined with microwave, concentrating to obtain an extract, dissolving it and performing molecular distillation to obtain Schisandra chinensis twig flavorings. In the former of the above preparation processes, the flavor raw materials are pulped, recombined and dried, which destroys the fiber and cell structure therein and is not conducive to the construction of pore structure; while the latter uses microwave combined with water extraction, but the field strength distribution of microwave is uneven, which easily leads to uneven heating and carbonization of the material, and will cause the collapse of the pore structure and the reduction of pore volume. Moreover, most of the microwave energy is absorbed by water, which is not conducive to the precipitation of flavor raw material components. At the same time, the common problem of both is that after the flavor is extracted, it is difficult to separate the plant flavor raw materials and the extraction solvent; generally, the larger the particles, the easier it is to separate the plant flavor raw materials, but the flavor extraction rate is not high; although the flavor extraction rate increases with smaller particles, it is difficult to separate the plant flavor raw materials and the extraction solvent.

[0005] Therefore, how to overcome the deficiencies of existing extraction technologies and improve the preparation yield of tobacco flavor raw materials is the problem to be solved by the present invention. Summary of the Invention

[0006] The present invention performs vacuum freeze-drying according to the eutectic point determination temperature of plant flavor raw materials, so that the surface of the plant flavor raw materials is not uneven and the interior is not collapsed. Combining the obtained particle size screening of the plant flavor raw materials and extracting with an extraction solvent is fast and effective. Not only is it easy to separate the plant flavor raw materials from the extraction solvent, but also the spice extraction rate is relatively high, saving energy consumption. The spice obtained by the method of the present invention is used in cigarettes, which can endow the cigarette smoke with a sweet and moist feeling and reduce irritation.

[0007] To achieve the above object, the technical solution adopted by the present invention is as follows:

[0008] The first aspect of the present invention discloses a method for improving the preparation yield of spices, comprising the following steps:

[0009] (1) Vacuum freeze-drying: Vacuum freeze-dry it according to the eutectic point determination temperature of the flavor raw material until the water content is 4-6 wt%;

[0010] (2) Crushing and particle size screening: Crush the flavor raw material after vacuum freeze-drying in step (1), and combine with the density of the extraction solvent. According to the formula: D 3 = 12ρ 溶剂 v g / π(ρ 溶剂 -ρ 颗粒 ) perform particle size screening to obtain particles with a particle size not greater than D; in the formula, ρ 颗粒 is the density of the flavor raw material particles detected by the drainage method, v g is the opening volume of the internal pores of the flavor raw material particles detected by the carbon tetrachloride coagulation method, and ρ 溶剂 is the density of the extraction solvent used; the extraction solvent is water, ethanol or a mixture of the two;

[0011] (3) Extraction: Extract the particles with a particle size of D obtained in step (2) using an extraction solvent with a water content of not less than 50 wt% to obtain an aqueous extract; extract the particles with a particle size less than D using an extraction solvent with an alcohol content of not less than 50 wt% to obtain an alcohol extract;

[0012] (4) Filtration and combination: Filter the aqueous extract and the alcohol extract respectively, and combine the filtrates of the two to obtain a total filtrate;

[0013] (5) Cold setting and filtration: Place the total filtrate obtained in step (4) in an environment of 4-8 °C for 6-12 h, and then filter again to obtain a secondary filtrate;

[0014] (6) Vacuum concentration: The secondary filtrate obtained in step (5) is subjected to vacuum evaporation and concentration, and the process is terminated after meeting the relevant indicators or requirements, thus obtaining the said spice.

[0015] Preferably, the fragrance raw material in step (1) is one or more of strawberry, apple, raspberry, blueberry, snow pear, banana, coconut meat or mango. After peeling and removing the cores, the inner and outer pulp should have the same material and structure.

[0016] Preferably, the vacuum freeze-drying step in step (1) is as follows: pre-freezing for 2 - 5 h at a vacuum degree of 20 - 25 Pa and a temperature 5 - 15 °C lower than the eutectic point of the fragrance raw material, then sublimation drying for 4 - 10 h at a vacuum degree of 10 - 40 Pa and a temperature of 30 - 45 °C, and then desorption drying for 2 - 6 h at a vacuum degree of 5 - 20 Pa and a temperature of 50 - 60 °C.

[0017] Preferably, the extraction conditions for water extraction and alcohol extraction in step (3) are: the fragrance raw material particles and the extraction solvent are mixed at a mass ratio of 1∶(8 - 16) and extracted at 55 - 70 °C for 1 - 2 h.

[0018] Preferably, the filtration in step (4) is all carried out by multi-stage filtration; among them, the water extract is first filtered through 100 - mesh and then 300 - mesh, and the alcohol extract is first filtered through 200 - mesh and then 400 - mesh.

[0019] Preferably, the secondary filtration in step (5) is carried out by multi-stage filtration, first through 300 - mesh and then 500 - mesh.

[0020] The second aspect of the present invention discloses the spice obtained by the said method.

[0021] The third aspect of the present invention discloses the use of the said spice for enhancing the sweet and mellow feeling and reducing the irritation of cigarette smoke.

[0022] The beneficial effects of the present invention are as follows:

[0023] 1. For the spice preparation method of the present invention, after determining the vacuum freezing temperature according to the eutectic point of the fragrance raw material, vacuum freeze-drying is carried out, and then through sublimation drying and desorption drying, the moisture content is reduced to 4 - 6 wt%, and at the same time, a porous structure is generated inside the fragrance raw material, which is beneficial to improving the subsequent extraction yield.

[0024] 2. The method of the present invention combines the density of the extraction solvent in a single or mixed system, according to D 3 = 12ρ 溶剂 v g / π(ρ 溶剂 -ρ 颗粒)Particle size screening can enable the extraction solvent to enter the interior of the particles more quickly and completely, prompting the particles to be fully immersed in the extraction solvent. Not only is it easy to separate the fragrance raw material from the extraction solvent, but also the extraction yield of the fragrance can be greatly improved, and the extraction time and energy consumption can be saved. Because when the particle size is relatively large, the particles will float on the surface of the extraction solvent, and it is not easy for the extraction solvent to enter the interior of the particles completely, resulting in a low extraction yield; when the particle size is relatively small, the pore structure therein is severely damaged, the open pore volume is greatly reduced, and the extraction yield of the fragrance is instead reduced, and the separation treatment is difficult, which not only wastes time but also consumes a high amount of energy.

[0025] 3. The fragrance prepared by the method of the present invention can enhance the flavor and fragrance, enrich the fragrance rhyme, emit soft and delicate smoke, reduce the roughness and irritation of the smoke, improve the sweet and moist feeling of the smoke, reduce the irritation, and enhance the smoking comfort. Detailed implementation manners

[0026] The present invention will be further described in detail below in conjunction with embodiments. Those skilled in the art will understand that the following embodiments are only used to illustrate the present invention and should not be regarded as limiting the scope of the present invention. For those not specifying specific techniques or conditions in the embodiments, the techniques or conditions described in the literature in this field or according to the product instructions are followed. For those materials or equipment without indicating the manufacturer, they are all conventional products that can be obtained by purchase. Unless otherwise specified in the present invention, the percentages are mass percentages and the ratios are mass ratios.

[0027] Embodiment 1: A method for improving the preparation yield of strawberry fragrance as a fragrance raw material, the steps are as follows:

[0028] Step (1), vacuum freeze-drying: Wash the strawberries with running water to remove surface impurities, detect that its eutectic point is -12.5 °C, remove the skin, core and fruit stalks to ensure the same material and structure of the inner and outer pulp, and then slice to 0.5 cm; Set the vacuum freeze-drying parameters as follows: pre-freezing temperature -25 °C (cold trap temperature -49 ± 1 °C), vacuum degree 20 Pa, keep for 4 h; sublimation drying temperature 40 °C, vacuum degree 25 Pa, keep for 10 h; analytical drying temperature is 55 °C, vacuum degree 10 Pa, keep for 4 h; detect the water content to be 5 wt%.

[0029] Step (2), pulverization and particle size screening: Pulverize and screen the strawberries obtained by vacuum freeze-drying in step (1). According to D 3 = 12ρ 溶剂 v g / π(ρ 溶剂 -ρ 颗粒 ) Calculate, the extraction solvent is water, ρ 水 = 1 g / ml, and it is tested that ρ 颗粒 = 0.76 g / cm 3 , v g = 0.35×10-5 cm 3 / g, it is calculated that D = 0.38 mm (about 40 mesh);

[0030] Step (3), extraction: The vacuum freeze-dried particles of 40 - 60 mesh obtained in step (2) and water are in a mass ratio of 1:14, and extracted at 70 °C in a water bath for 2 h to obtain an aqueous extract; the particles with a particle size less than 60 mesh and 95% ethanol solution are in a mass ratio of 1:16, and extracted at 60 °C in a water bath for 2 h to obtain an ethanol extract;

[0031] Step (4), filtration and combination: The aqueous extract in step (3) is first filtered through a 100-mesh and then a 300-mesh filter cloth to obtain an aqueous filtrate; the ethanol extract in step (3) is first filtered through a 200-mesh and then a 400-mesh filter cloth to obtain an ethanol filtrate; the aqueous filtrate and the subsequent ethanol filtrate are combined to obtain a total filtrate;

[0032] Step (5), cold setting and filtration: The total filtrate obtained in step (4) is placed in an environment of 4 °C for 6 h, and then successively filtered through 300-mesh and 500-mesh filter cloths for multi-stage filtration to obtain a secondary filtrate;

[0033] Step (6), reduced pressure concentration: The secondary filtrate obtained in step (5) is subjected to reduced pressure evaporation and concentration, and terminated until it meets the relevant indicators or requirements, thus obtaining the said spice; the extraction yield is 63.39%.

[0034] Sensory evaluation by smoking: The strawberry spice obtained in step (6) is diluted with ethanol and added to cigarettes, and the blank cigarettes without added spice are used as a control, and evaluated by the personnel with the qualification of cigarette smoking evaluation according to the relevant standards. The smoking evaluation results are as follows:

[0035] The aroma richness, salivation and sweet and moist feeling are improved, the smoke is soft and delicate, the irritation is reduced, and the comfort is increased.

[0036] Comparative Example 1

[0037] Same as Example 1, the difference is: In step (2), the particle size of the crushed and screened particles is relatively large, about 20 mesh. The result shows that during the extraction process, some particles always float on the liquid surface, and the extraction yield is 43.68%. Compared with Example 1, the spice yield is significantly lower.

[0038] Comparative Example 2

[0039] Same as Example 1, the difference is: In step (2), the particle size of the crushed and screened particles is relatively small, about 120 mesh. The result shows that the spice yield of the extract is 60.56%. Compared with Example 1, the spice yield is also relatively high, but the separation is significantly difficult.

[0040] Comparative Example 3

[0041] Same as Example 1, the difference is: in step (1), strawberries are directly subjected to fresh fruit extraction without vacuum freeze-drying treatment. The results show that the water extraction yield is 29.76%, and the 95% ethanol extraction yield is 34.18%. Compared with Example 1, the spice yield is significantly lower.

[0042] Comparative Example 4

[0043] Same as Example 1, the difference is: in step (3), both or 95% ethanol is used for extraction. The results show that the extraction yield is 57.33%. The yields are all lower than those in Example 1 because the particles in the target range could not be completely immersed in the extraction solvent, and the types of aroma components extracted by a single extraction solvent are fewer than those extracted by a mixed solvent.

[0044] Example 2: A method for improving the yield of the flavor raw material blueberry spice, the steps are as follows:

[0045] Step (1), vacuum freeze-drying: Wash the blueberries with running water to remove impurities, detect its eutectic point as -32.9 °C, and use a steel needle to punch holes on the fruit surface; Set the vacuum freeze-drying parameters: the pre-freezing temperature is -45 °C (the cold trap temperature is -49 ± 1 °C), the vacuum degree is 45 Pa, and the time is 4 h; The sublimation drying temperature is 30 °C, the vacuum degree is 40 Pa, and it is maintained for 8 h; The analytical drying temperature is 45 °C, the vacuum degree is 20 Pa, and it is maintained for 7 h; Detect the water content as 4 wt%.

[0046] Step (2), crushing and particle size screening: Crush and screen the particle size of the blueberries obtained by vacuum freeze-drying in step (1). According to D 3 = 12ρ 溶剂 v g / π(ρ 溶剂 -ρ 颗粒 ) Calculate, the extraction solvent is an aqueous solution containing 20% ethanol, ρ 水 = 0.96 g / ml, test to obtain ρ 颗粒 = 0.89 g / cm 3 , v g = 0.32×10 -5 cm 3 / g, calculate to obtain D = 0.55 mm (about 30 mesh);

[0047] Step (3), extraction: Mix the vacuum freeze-dried 30 - 60 mesh particles obtained in step (2) with the extraction solvent (aqueous solution containing 20% alcohol) at a mass ratio of 1:14, and extract for 2 h at 70 °C in a water bath to obtain an aqueous extract; Mix the particles with a particle size less than 60 mesh with 95% ethanol solution at a mass ratio of 1:16, and extract for 2 h at 60 °C in a water bath to obtain an alcohol extract;

[0048] Step (4), filtration and merging: Filter the aqueous extract from step (3) through a 100-mesh and then a 300-mesh filter cloth to obtain an aqueous filtrate; filter the ethanol extract from step (3) through a 200-mesh and then a 400-mesh filter cloth to obtain an ethanol filtrate; merge the aqueous filtrate and the ethanol filtrate to obtain a total filtrate;

[0049] Step (5), cold setting and filtration: Place the total filtrate obtained in step (4) in an environment at 5°C for 10 h, and then perform multi-stage filtration through 350-mesh and 500-mesh filter cloths to obtain a secondary filtrate;

[0050] Step (6), vacuum concentration: Perform vacuum evaporation and concentration on the secondary filtrate obtained in step (5), and terminate when it meets the relevant indicators or requirements, thus obtaining the said spice; the spice yield is 69.89%.

[0051] Sensory smoking evaluation: Dilute the blueberry spice obtained in step (6) with ethanol and add it to cigarettes, and use the blank cigarettes without added spice as a control. Evaluate by personnel with the qualification of cigarette smoking evaluation according to relevant standards. The smoking evaluation results are as follows:

[0052] The richness of aroma, salivation and sweet and mellow feeling are significantly improved, the smoke is soft and delicate, the irritation is greatly reduced, and the comfort is significantly increased.

[0053] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. What is described in the above embodiments and the specification only illustrates the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements fall within the scope of the present invention claimed. The scope of protection claimed by the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for improving the yield of spice preparation, characterized in that, It includes the following steps: (1) Vacuum freeze-drying: According to the eutectic point of the fragrance raw material, determine the temperature and conduct vacuum freeze-drying until the water content is 4 - 6 wt%; (2) Crushing and particle size screening: Crush the fragrance raw materials after vacuum freeze-drying in step (1), and combine with the density of the extraction solvent. According to the formula: D 3 = 12ρ 溶剂 v g / π(ρ 溶剂 - ρ 颗粒 ) for particle size screening to obtain particles with a particle size not greater than D; where ρ 颗粒 is the density of the fragrance raw material particles detected by the drainage method, v g is the opening volume of the internal pores of the fragrance raw material particles detected by the carbon tetrachloride coagulation method; ρ 溶剂 is the density of the extraction solvent with a water content of not less than 50 wt% used for particles with a particle size of D; (3) Extraction: Use an extraction solvent with a water content of not less than 50 wt% to extract the particles with a particle size of D obtained in step (2) to obtain an aqueous extract; use an extraction solvent with an alcohol content of not less than 50 wt% to extract the particles with a particle size less than D to obtain an alcohol extract; (4) Filtration and combination: Filter the aqueous extract and the alcohol extract respectively, and combine the filtrates of the two to obtain a total filtrate; (5) Cold setting and filtration: Place the total filtrate obtained in step (4) in an environment of 4 - 8 °C for 6 - 12 h, and then filter again to obtain a secondary filtrate; (6) Vacuum concentration: Conduct vacuum evaporation and concentration on the secondary filtrate obtained in step (5), and terminate until it meets the relevant indicators or requirements, that is, the fragrance is obtained; The vacuum freeze-drying step in step (1) is: pre-freeze for 2 - 5 h at a vacuum degree of 20 - 25 Pa and a temperature 5 - 15 °C lower than the eutectic point of the fragrance raw material, then conduct sublimation drying for 4 - 10 h at a vacuum degree of 10 - 40 Pa and a temperature of 30 - 45 °C, and then conduct desorption drying for 2 - 6 h at a vacuum degree of 5 - 20 Pa and a temperature of 50 - 60 °C.

2. The method according to claim 1, wherein The fragrance raw material in step (1) is one or several of strawberry, apple, raspberry, blueberry, snow pear, banana, coconut meat or mango, and the skin and core are removed to ensure the same material and structure of the inner and outer pulp.

3. The method according to claim 1, wherein The extraction conditions for aqueous extraction and alcohol extraction in step (3) are: mix the fragrance raw material particles and the extraction solvent at a mass ratio of 1∶(8 - 16) and extract at 55 - 70 °C for 1 - 2 h.

4. The method according to claim 1, wherein The filtration in step (4) adopts multi-stage filtration; among them, the aqueous extract is filtered first through 100 mesh and then through 300 mesh, and the alcohol extract is filtered first through 200 mesh and then through 400 mesh.

5. The method according to claim 1, characterized in that, The secondary filtration in step (5) adopts multi-stage filtration, first through 300 mesh and then through 500 mesh.

6. The fragrance obtained by the method according to any one of claims 1 - 5.

7. Use of the fragrance according to claim 6 for enhancing the sweet and mellow feeling and reducing the irritation of cigarette smoke.