CN113679092B

CN113679092B - Preparation method of cigarette spice capable of reducing harmful substances in smoke

Info

Publication number: CN113679092B
Application number: CN202111048539.0A
Authority: CN
Inventors: 李星; 周红审; 祃志明; 蹇顺华; 程书锋; 齐富友
Original assignee: China Tobacco Hubei Industrial LLC
Current assignee: China Tobacco Hubei Industrial LLC
Priority date: 2021-09-08
Filing date: 2021-09-08
Publication date: 2023-04-07
Anticipated expiration: 2041-09-08
Also published as: CN113679092A

Abstract

The invention relates to the technical field of tobacco essence, in particular to a preparation method of a tobacco spice capable of reducing harmful substances in smoke. Which comprises the following steps: extracting Capsici fructus with water to obtain Capsici fructus extract and Capsici fructus residue; extracting black pepper with alkali solution to obtain black pepper extract and black pepper residue; mixing pepper residue and black pepper residue, and extracting with an organic solvent to obtain an oil-soluble extracting solution; adding a lipophilic surfactant into the oil-soluble extracting solution, then adding the hot pepper extracting solution and dispersing to obtain a mixture; and adding the mixture and a hydrophilic surfactant into the black pepper extracting solution and dispersing to obtain the spice for the cigarettes. According to the application, vitamin C, melanin and aromatic substances with spicy flavor are extracted from pepper and black pepper respectively, harmful substances in smoke are effectively reduced through the free radical scavenging effect of the vitamin C and the melanin, and meanwhile, excellent spicy flavor is brought to cigarettes.

Description

Preparation method of cigarette spice capable of reducing harmful substances in smoke

Technical Field

The invention relates to the technical field of tobacco essences, in particular to a preparation method of a tobacco spice capable of reducing harmful substances in smoke.

Background

It is known that cigarettes burn to produce a large amount of harmful substances such as fused-ring aromatic hydrocarbons, phenols, N-nitrosamines, free radicals, certain heterocyclic compounds, etc. Most of these harmful substances are carcinogenic and carcinogenic substances, which cause harm to human bodies, and among them, gas-phase free radicals are the most harmful substances. The radicals in the gas phase of the flue gas are, among others, mainly alkoxy (RO) and alkane (r.) radicals. The nitrogenous substance is oxidized to generate a large amount of NO when the cigarette is burnt, the free radical NO has a plurality of important biological functions, is endothelial cell relaxation factor (EDRF), participates in nerve conduction, immunity prevention and cell poisoning effects, generates a NO2 free radical with stronger reactivity when meeting oxygen, can react with an alkene substance generated when the cigarette is burnt to generate an alkane free radical R.,r, can be and O ₂ The reaction can generate an alkyl peroxy radical ROO, which can also react with NO to generate an alkyl peroxy radical RO. It is these free radicals that attack the cell membrane, causing lipid peroxidation, further stimulating the release of oxygen radicals from macrophages. These free radicals can cause damage to cell components alone, and can also poison cells together with free radicals generated by smoking, causing occurrence of lung cancer and heart disease. These free radicals can also attack and inactivate lung alpha-1 antiproteases without inhibiting elastase, resulting in lung injury. The harm of free radicals in the gas phase of cigarette smoke is very large, and a common filter tip cannot effectively remove the free radicals, so that how to effectively remove the free radicals in the gas phase of the smoke is a big problem troubling the tobacco industry, which is the problem to be solved by the invention.

The vitamin C is used as an antioxidant, and can reduce the harm of harmful substances and free radicals in the smoke to the human body to a certain extent. When smoke enters the body of a smoker, the body consumes a large amount of vitamin C in order to fight against harmful substances in the smoke. Scientific research finds that the vitamin C consumed by one cigarette is up to 25mg. Assuming that one cigarette is smoked per day, the theoretical vitamin C loss amount can reach 500mg, which is far more than the normal vitamin C intake of one person during the diet. Therefore, people who smoke inevitably have initial deficiency symptoms of vitamin C, such as frequent headache, gingival bleeding, cold and the like, and various diseases can be followed after a long time. Smokers were statistically 30% -50% less vitamin C and vitamin E in the blood than non-smokers.

Patent document No. CN1103197C discloses a cigarette filter which can effectively remove free radicals, the filter containing proanthocyanidin; the filter tip can also contain vitamin C. The filter tow contains proanthocyanidins, and the substance has a very outstanding effect of removing gas-phase free radicals in cigarette smoke under a low-concentration state. When the proanthocyanidin and the vitamin C (Vc) are mixed for use, the proanthocyanidin and the vitamin C have a better scavenging effect on gas-phase free radicals. However, proanthocyanidins and vitamin C are all photosensitive substances, are easily oxidized and deteriorated by light, and are not beneficial to long-term storage of cigarettes.

Disclosure of Invention

The invention aims to solve the problems and provides a preparation method of a spice for cigarettes, which can reduce harmful substances in smoke.

The technical scheme for solving the problems is to provide a preparation method of the spice for the cigarettes, which can reduce harmful substances in smoke and comprises the following steps:

(1) Extracting Capsici fructus with water to obtain Capsici fructus extract and Capsici fructus residue;

(2) Extracting black pepper with alkali liquor to obtain black pepper extract and black pepper residue;

(3) Mixing the pepper residues and the black pepper residues, and extracting with an organic solvent to obtain an oil-soluble extracting solution;

(4) Adding a lipophilic surfactant into the oil-soluble extracting solution, then adding the hot pepper extracting solution and dispersing to obtain a mixture;

(5) And adding the mixture and a hydrophilic surfactant into the black pepper extracting solution together and dispersing to obtain the spice for the cigarettes.

The vitamin C content in the pepper accounts for the crowns of all vegetables, and the vitamin C content in 100g of fresh pepper reaches 13-342 mg, which is 7-15 times of the content of fruits and vegetables such as cucumbers, tomatoes, eggplants and the like. Meanwhile, the capsicum contains capsaicin, which can bring excellent spicy flavor to cigarettes, so that the capsicum is used as a main extraction raw material of the vitamin C in the application. Since vitamin C belongs to water-soluble vitamins and capsaicin is insoluble in water, the vitamin C is extracted by water extraction firstly, and then the capsaicin is extracted from water extraction residues by an organic solvent. In the extraction process, ultrasonic waves, microwaves and the like can be used as an auxiliary for improving the extraction rate, and the following extraction operation is the same.

Meanwhile, since vitamin C is a photosensitive substance, in order to prevent the vitamin C from being exposed to light, the vitamin C is coated by the action of a surfactant in the present application. The vitamin C coating mainly adopts two layers of coatings, namely a vitamin C layer, a middle layer and an outermost layer in sequence to form a water-in-oil-in-water structure.

Wherein, the outermost layer adopts alkali liquor extract of black pepper, and the black pepper has spicy flavor, which can further improve the spicy flavor of the cigarette; the black food black pepper contains melanin, which is obtained by oxidative polymerization of polyphenol and indole compounds, and has high molecular weight and red, black or brown color, and is dissolved in alkali solution. The melanin has excellent light absorption, light stability, ultraviolet resistance, oxidation reduction resistance and free radical scavenging ability, and can further improve the ability of the perfume to scavenge harmful substances such as free radicals when being mixed with vitamin C. Simultaneously in this application to melanin cladding vitamin C, avoided vitamin C photic for the cigarette that adopts the spices of this application also has good harmful substance of cleaing away ability even after long-term storage.

In this process, in order to increase the coverage of melanin, it is preferable to concentrate the black pepper extract to a solid content of 60 to 70% and then perform the step (5).

In the prior art, the common alkaline solution for extracting melanin is sodium hydroxide, but the sodium hydroxide is considered to be strong alkali, and the extract of the application needs to be used in cigarettes, so that, as a preferred option of the invention, in the step (2), the alkaline solution is sodium bicarbonate solution with the concentration of 5-10 g/L. However, the extraction rate of the sodium bicarbonate solution is low, therefore, as a preferred method of the invention, in the step (2), before the black pepper is extracted by the alkaline solution, the black pepper is fermented for 24-48 hours at 22-28 ℃ together with strains, wherein the strains comprise one or more of monospore bacteria, bacillus, west watt bacteria, vibrio, rhizobium and proteus, and the melanin content is increased by a fermentation method.

In addition, since black pepper also contains various other water-soluble components, such as vitamin C, vitamin B6, betaine and the like, in order to avoid damage to these active components during alkali liquor extraction, it is preferable that in step (2), before alkali liquor extraction, the black pepper is extracted with water to obtain an aqueous extract and an aqueous extraction residue, and the aqueous extraction residue is extracted with alkali liquor to obtain the black pepper extract and the black pepper residue; in the step (4), the water extract and the pepper extract are mixed and then added into the mixed solution of the oil-soluble extract and the lipophilic surfactant.

On one hand, the black pepper extract and the pepper extract have high compatibility and are inconvenient to coat; on the other hand, the pungent substances in pepper and black pepper are difficult to be extracted by water and alkali liquor, and the water-soluble extract of the two is used as the spice, so that the spice does not have obvious spicy flavor. Therefore, an intermediate layer is also designed, when the capsicum and the black pepper are extracted in the steps (1) and (2), oil-soluble substances in the capsicum and the black pepper, such as capsaicin in the capsicum, vitamin a, and the black pepper in the black pepper, are remained in the residue, and are extracted by an organic solvent to be used as the intermediate coating layer, and the organic solvent comprises ethanol in the step (3) as a preferable preference of the invention. The coating of melanin on vitamin C is realized in a water-in-oil-in-water mode, the spicy flavor of the spice is improved, and the spicy substances are coated by the melanin, so that the loss of the spicy substances is avoided.

In order to realize the water-in-oil-in-water structure, as a preferable aspect of the present invention, in the step (4), the lipophilic surfactant includes one or more of span 60, span 65, span 80, and mannitol monooleate. Preferably, in the step (5), the hydrophilic surfactant includes one or more of polyethylene glycol 264 monooleate, polyethylene glycol 400 monooleate and polyethylene glycol 600 monooleate.

In addition, because the pepper and the black pepper are both raw materials with heavier spicy taste, in order to adjust the flavor of the spice, the step (3) preferably further comprises clove; mixing the pepper residue, the black pepper residue and the clove, and extracting with an organic solvent to obtain an oil-soluble extracting solution. Further, as a preferable aspect of the present invention, the mixing mass ratio of the capsicum residue, the black pepper residue and the clove is 1: (1-2): (5-10).

The invention has the beneficial effects that:

according to the application, vitamin C, melanin and aromatic substances with spicy flavor are extracted from pepper and black pepper respectively, harmful substances in smoke are effectively reduced through the free radical scavenging effect of the vitamin C and the melanin, and meanwhile, excellent spicy flavor is brought to cigarettes. Meanwhile, the vitamin C and the fragrant substances are wrapped in the melanin through a water-in-oil-in-water structure, so that deterioration loss of the vitamin C and the fragrant substances is avoided, the storage time of cigarettes containing the essence is prolonged, release of the fragrant substances is slowly released, and the problem that the fragrance amount is insufficient in the later smoking period of the cigarettes is solved.

Detailed Description

The following are specific embodiments of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.

Example 1

A preparation method of a cigarette spice capable of reducing harmful substances in smoke comprises the following steps:

(1) Pepper and deionized water were mixed according to a 1g: mixing 5mL of the feed liquid in a brown conical flask, sealing, and placing in a constant-temperature water bath kettle at 50 ℃ for shaking extraction for 7h. And then carrying out solid-liquid separation to obtain a pepper extract and pepper residues, wherein the pepper extract is stored in dark for later use.

(2) Black pepper and sodium bicarbonate solution with concentration of 8g/L were mixed according to a ratio of 1g:5mL of the mixture is mixed and then is put under 400W ultrasonic waves and extracted for 45min at the temperature of 45 ℃. Then carrying out solid-liquid separation to obtain black pepper extract and black pepper residue.

(3) Mixing the pepper residues and the black pepper residues according to a mass ratio of 1: 6mL, and extracting at 45 ℃ for 60min. Then solid-liquid separation is carried out, and oil-soluble extract is taken for standby.

(4) Adding 0.5g span 60 into 30mL oil-soluble extractive solution, stirring with magnetic stirrer for 15min, adding 50mL Capsici fructus extractive solution, continuing magnetic stirring for 2min, and performing ultrasonic treatment for 4min to obtain W/O type mixture.

(5) Adding 0.3g of polyethylene glycol 264 monooleate into 30mL of black pepper extract, magnetically stirring for 5min, adding 10mL of the mixture into the mixture, continuously magnetically stirring for 5min, and performing ultrasonic treatment for 2min to obtain the W/O/W type cigarette spice.

Example 2

This embodiment is substantially the same as embodiment 1, except that:

in the step (2), the obtained black pepper extract is concentrated to 65% of solid content by an evaporation concentration mode, and then the step (5) is carried out.

Example 3

This embodiment is substantially the same as embodiment 1, except that:

in the step (2): firstly, black pepper and deionized water are mixed according to the weight ratio of 1g: mixing 5mL of the feed liquid in a brown conical flask, sealing, and placing in a constant-temperature water bath kettle at 50 ℃ to shake and extract for 7h. Then solid-liquid separation is carried out to obtain water extract and water extraction residue. Then, the water extraction residue and sodium bicarbonate solution with the concentration of 8g/L are mixed according to the proportion of 1g:5mL of the mixture is mixed and then is put under 400W ultrasonic waves and extracted for 45min at the temperature of 45 ℃. Then carrying out solid-liquid separation to obtain black pepper extract and black pepper residue.

In the step (4), all the water extract and the pepper extract are mixed to obtain a mixed extract. Then 0.5g span 60 is added into 30mL oil-soluble extract, after stirring for 15min with a magnetic stirrer, 50mL of the mixed extract is added into the mixture, and the magnetic stirring is continued for 2min, and then the ultrasonic treatment is carried out for 4min, thus obtaining the W/O type mixture.

Example 4

This embodiment is substantially the same as embodiment 1, except that:

in the step (2): firstly, fermenting black pepper and bacillus together at 25 ℃ for 36 hours; the product obtained is then extracted after mixing with a sodium bicarbonate solution.

Example 5

This embodiment is substantially the same as embodiment 1, except that:

in the step (3), clove is also included; mixing pepper residue, black pepper residue and clove according to the weight ratio of 1:2:8, adding the mixture into an ethanol solution, wherein the material-liquid ratio is 1g:6mL, and extracting at 45 ℃ for 60min. Then solid-liquid separation is carried out, and oil-soluble extract is taken for standby.

Example 6

A preparation method of a spice for tobacco capable of reducing harmful substances in smoke comprises the following steps:

(1) Pepper and deionized water were mixed according to a 1g: mixing 5mL of the feed liquid in a brown conical flask, sealing, and placing in a constant-temperature water bath kettle at 50 ℃ to shake and extract for 7h. And then carrying out solid-liquid separation to obtain a pepper extract and pepper residues, wherein the pepper extract is kept away from light for later use.

(2) First, black pepper and bacillus are fermented together at 25 ℃ for 36h.

The fermentation product and deionized water were then mixed in a 1g: mixing 5mL of the feed liquid in a brown conical flask, sealing, and placing in a constant-temperature water bath kettle at 50 ℃ to shake and extract for 7h. Then solid-liquid separation is carried out to obtain water extract and water extraction residue.

Then, the water extraction residue and sodium bicarbonate solution with the concentration of 8g/L are mixed according to the proportion of 1g: mixing 5mL of the mixture, and extracting for 45min at 45 ℃ under 400W of ultrasonic waves. Then carrying out solid-liquid separation to obtain black pepper extract and black pepper residue. Concentrating the obtained black pepper extract by evaporation concentration until the solid content is 65% for later use.

(3) Mixing pepper residue, black pepper residue and clove according to the weight ratio of 1:2:8, adding the mixture into an ethanol solution, wherein the material-liquid ratio is 1g:6mL, and extracting at 45 ℃ for 60min. Then solid-liquid separation is carried out, and oil-soluble extract is taken for standby.

(4) Firstly, mixing all the water extracts obtained in the step (2) with the pepper extract to obtain a mixed extract. Then 0.5g span 60 is added into 30mL oil-soluble extract, after stirring for 15min with a magnetic stirrer, 50mL of the mixed extract is added into the mixture, and the magnetic stirring is continued for 2min, and then the ultrasonic treatment is carried out for 4min, thus obtaining the W/O type mixture.

(5) Adding 0.3g of polyethylene glycol 264 monooleate into 30mL of concentrated black pepper extract, magnetically stirring for 5min, adding 10mL of the mixture into the mixture, continuously magnetically stirring for 5min, and performing ultrasonic treatment for 2min to obtain W/O/W type cigarette spice.

Comparative example 1

This comparative example is essentially the same as example 1 except that:

directly mixing the pepper extract, the black pepper extract and the oil-soluble extract to obtain a comparison sample.

Comparative example 2

This comparative example is essentially the same as example 1 except that:

in the step (2), black pepper is extracted by water.

Comparative example 3

In this comparative example, microcapsules were prepared according to the method in patent document No. CN 107373744A:

the capsicum extract obtained in example 1 was freeze-dried under vacuum and pulverized to obtain a powder. 10g of PEG-400 is weighed and placed in a flask, methanol with the mass of 100g is added, and the mixture is fully dissolved and uniformly mixed in a water bath at 25 ℃ to obtain a methanol solution containing the PEG-400. Weighing 3.33g of edible paraffin, heating the paraffin to completely melt, adding 10g of the powder while the powder is hot, and uniformly stirring to obtain a mixture. The resulting mixture was added to a PEG methanol solution while hot, and stirred at 70 ℃ for 30min with heat preservation. Stopping heating and stirring, and naturally cooling to room temperature under reflux state to obtain suspension containing solids. And after the suspension is completely cooled, filtering to remove supernatant, washing the obtained solid with methanol for 3-5 times, drying under reduced pressure, freeze-drying to obtain microcapsules, and preparing the microcapsules into a solution with the concentration of 1% by using ethanol.

[ Property measurement for removing harmful substances ]

The flavors obtained in the examples and comparative examples were mixed with tobacco shreds in a ratio of 1mg:2g of the tobacco shreds are mixed to prepare cigarettes, and meanwhile, blank cigarettes without spices are prepared. Each of the cigarettes in each of examples, comparative examples and blank examples was divided into two batches, one batch was immediately tested, and the other batch was left to stand in the same light environment for 10 days and then tested.

The detection method comprises the following steps: the smoking machine is used for simulating the smoking of people, the smoke flow is 400mL/min, the smoke is sucked every 2s, and the interval is 1min. Tar was collected on two layers of Cambridge filter paper, and the smoke from smoking was then introduced into 2ml (0.1 mol/L) of PBN (N-tertbutyl-2-phenyl nitrate) (N-tetrabutyl-2-azocarbonyl benzene) spin-trapping benzene solution to trap free radicals therein. The solution was then drawn into a quartz capillary and the signal of the free radicals was measured on an ESR spectrometer. The relative concentration of free radicals is represented by signal intensity. ESR test conditions: x wave band, microwave power 20mW, modulation frequency 100KHZ, modulation amplitude 1G. The clearance E is calculated according to the following formula: e = (HO-HX)/HO × 100%. Wherein HO is the reference system peak intensity of the blank example, and HX is the peak intensity of the example or the comparative example. The results are shown in Table 1 below.

Table 1.

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As can be seen from Table 1, the cigarette spice prepared by the method can effectively remove free radicals in smoke, and after the cigarette is stored for a long time, the loss rate of active ingredients for removing the free radicals in the spice is extremely low. In comparative example 1, although better radical scavenging rate can be obtained by directly mixing the capsicum extract, the black pepper extract and the oil-soluble extract, the vitamin C is still exposed and can be contacted with the external environment because the vitamin C and the melanin are simply mixed, so that the loss rate of the active ingredients is high after the cigarette is stored for a long time, and the radical scavenging performance is reduced. In comparative example 2, melanin was not extracted, resulting in a decrease in the clearance of its free radicals and an increase in the loss rate of active ingredients. In comparative example 3, although the active ingredient is microencapsulated to prevent the loss of the active ingredient to some extent, the paraffin is white and the vitamin C encapsulated therein is deteriorated by light, resulting in the decrease of its radical scavenging property.

The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.

Claims

1. A preparation method of a spice for tobacco capable of reducing harmful substances in smoke is characterized by comprising the following steps: the method comprises the following steps:

(1) Extracting Capsici fructus with water to obtain Capsici fructus extract and Capsici fructus residue; the capsicum extract contains vitamin C;

(2) Extracting black pepper with alkali solution to obtain black pepper extract and black pepper residue; the black pepper extract contains melanin;

(5) And adding the mixture and a hydrophilic surfactant into the black pepper extracting solution together, and dispersing to form a melanin-coated vitamin C water-in-oil-in-water structure, thereby obtaining the spice for the cigarettes.

2. The method for preparing the cigarette spice capable of reducing harmful substances in smoke according to claim 1, wherein the method comprises the following steps: and (5) concentrating the black pepper extract until the solid content is 60-70%.

3. The method for preparing the spice for cigarette capable of reducing harmful substances in smoke according to claim 1, wherein the method comprises the following steps: in the step (2), before the black pepper is extracted by the alkaline solution, water is firstly extracted to obtain water extract and water extraction residues; extracting the water extraction residues with an alkali solution to obtain black pepper extract and black pepper residues; in the step (4), the water extract and the pepper extract are mixed and then added into the mixed solution of the oil-soluble extract and the lipophilic surfactant.

4. The method for preparing the spice for cigarette capable of reducing harmful substances in smoke according to claim 1, wherein the method comprises the following steps: in the step (2), the alkali liquor is sodium bicarbonate solution with the concentration of 5-10 g/L.

5. The method for preparing the spice for cigarette capable of reducing harmful substances in smoke according to claim 1, wherein the method comprises the following steps: in the step (2), before the black pepper is extracted by the alkaline solution, the black pepper and bacterial strains are fermented together at the temperature of 22-28 ℃ for 24-48h, wherein the bacterial strains comprise one or more of monospore bacteria, bacillus, west watt bacteria, vibrio, rhizobium and proteus.

6. The method for preparing the spice for cigarette capable of reducing harmful substances in smoke according to claim 1, wherein the method comprises the following steps: in the step (3), the organic solvent includes ethanol.

7. The method for preparing the spice for cigarette capable of reducing harmful substances in smoke according to claim 1, wherein the method comprises the following steps: in the step (4), the lipophilic surfactant comprises one or more of span 60, span 65, span 80 and mannitol monooleate.

8. The method for preparing the spice for cigarette capable of reducing harmful substances in smoke according to claim 1, wherein the method comprises the following steps: in the step (5), the hydrophilic surfactant comprises one or more of polyethylene glycol 264 monooleate, polyethylene glycol 400 monooleate and polyethylene glycol 600 monooleate.

9. The method for preparing the spice for cigarette capable of reducing harmful substances in smoke according to claim 1, wherein the method comprises the following steps: in the step (3), clove is also included; mixing the pepper residue, the black pepper residue and the clove, and extracting with an organic solvent to obtain the oil-soluble extracting solution.

10. The method for preparing the cigarette spice capable of reducing harmful substances in smoke according to claim 9, wherein the method comprises the following steps: the mixing mass ratio of the pepper residues, the black pepper residues and the clove is 1: (1-2): (5-10).