CN112273709B - Preparation method of Shiyao angelica extract for perfuming tobacco - Google Patents

Abstract

The invention discloses a preparation method of a Shiyao angelica extract for flavoring tobacco, which comprises the following steps: s1, taking a mixture of Chinese angelica and cistanche salsa in a stone kiln, crushing and sieving; s2, leaching the sieved mixture with 100% ethanol, filtering to obtain filter residue and first filtrate, and distilling the first filtrate at normal pressure to obtain distillate; s3, leaching the filter residue with a solanic acid solution, filtering to obtain a second filtrate, and concentrating the second filtrate under reduced pressure to obtain a concentrated solution; and S4, mixing the distillate and the concentrated solution, and storing in an inert gas environment to obtain the lithospermum angelica extract, wherein the lithospermum angelica extract has high extraction rate and the extracted ligustilide has strong stability.

Description

A kind of preparation method of stone kiln angelica extract used for tobacco flavoring

technical field

The invention relates to the technical field of tobacco flavors, in particular to a preparation method of a stone kiln angelica extract used for flavoring tobacco.

Background technique

Flavor and fragrance are the soul of cigarette products and play a key role in the quality of cigarette products. With the decline in tar content in cigarettes and the growing controversy over smoking and health issues, one of the challenges facing the tobacco industry is to reduce tar while maintaining sufficient flavor in cigarettes. At present, many cigarette factories use various flavoring agents to make up for the lack of cigarette flavor while carefully preparing cigarette formulations.

In recent years, the use of Chinese herbal extracts as additives in cigarette flavoring has become one of the focuses and hot spots in the development of the tobacco industry. Chinese herbal medicine is a product with Chinese characteristics. The combination of tobacco and Chinese herbal medicine is one of the most distinctive styles of "Chinese cigarettes". my country is the hometown of Chinese herbal medicine, and the application of Chinese herbal medicine additives in Chinese cigarettes is a unique advantage of the Chinese tobacco industry. There are abundant Chinese herbal medicine resources in my country. Many varieties are similar to tobacco in chemical composition, but have different properties. They can make up for the deficiencies of tobacco in some aspects.

Stone kiln angelica is a traditional Chinese medicinal material. It has been an essential medicine for nourishing blood and activating blood since ancient times. It is a Umbelliferae plant. The chemical components of the extract are mainly divided into two parts: volatile oil and water-soluble components. The volatile oil of Angelica sinensis is mainly composed of ligustilide, and the water-soluble components include ferulic acid, coniferous ferulic acid, succinic acid, etc. The volatile oil is The important components of Angelica sinensis, the main components in the volatile oil are ligustilide, n-butenylphthalide, butylphthalide, new cnidolide, 6,7-epoxy ligustilide, 6,7- Phthalide compounds such as trans-dihydroxy ligustilide, 6,7-trans-dihydroxy ligustilide, angelic acid (Z)-ligustilide-11-ol ester, among which ligustilide Accounting for more than 60% of the total amount of such compounds, ligustilide has preventive and therapeutic effects on atherosclerosis, vasculitis and cerebral thrombosis, and has strong antispasmodic, antiasthmatic and sedative pharmacological effects. It can reduce the harmfulness of smoking cigarettes.

The prior art has the combination of angelica extract and tobacco preparation to reduce the harmfulness of tobacco. Chinese patent CN201410855364.8 discloses an atomized liquid containing angelica components and a preparation method thereof. The angelica extract obtained by extraction is used in the preparation of the atomized liquid, but the ligustilide prepared by this method is unstable, and the ligustilide contains unsaturated phthalide, and the 3-position is composed of an active butenyl group, which is easy to occur. Due to various isomerization reactions, the aerosol agent added with Angelica sinensis extract cannot achieve the expected medicinal effect.

SUMMARY OF THE INVENTION

In order to solve the above problems, the present invention provides a method for preparing a stone kiln angelica extract for tobacco flavoring.

The technical scheme solved by the present invention is, a preparation method of the stone kiln angelica extract used for tobacco flavoring, comprising the following steps:

S1. Take the mixture of Shiyao Angelica sinensis and Cistanche and crush and sieve;

S2. the mixture after sieving is filtered with 100% ethanol leaching to obtain filter residue and the first filtrate, and the first filtrate is distilled at atmospheric pressure to obtain distillate;

S3. the filter residue is leached with solanic acid solution and then filtered to obtain the second filtrate, and the second filtrate is concentrated under reduced pressure to obtain a concentrated solution;

S4. Mix the distillate and the concentrate, and store in an inert gas environment to obtain the stone kiln angelica extract.

Preferably, the mass ratio of Shiyao Angelica sinensis to Cistanche deserticola is 4-6:1.

Preferably, the water content of the concentrate is 3%-5%.

Preferably, in the step S2, the leaching temperature is 50°C-70°C, and the leaching time is 1-3h.

Preferably, the leaching temperature in the step S3 is 80°C-95°C, and the leaching time is 6-8h.

Preferably, the inert gas is one or more of nitrogen gas and fluorocarbon gas.

Preferably, the concentration of the solanaceous acid solution is 0.1-0.2‰.

In this scheme, ligustilide contains unsaturated phthalide, and the 3-position is composed of an active butenyl group, which is prone to various isomerization reactions or degradation reactions, while Cistanche deserticola contains carotene, 8-epistrychnic acid , Lilifaside and 7 phenylpropanosides, such as episteroside, 2'-acetylergosteroside, sea urchin glycoside and Cistanche glycosides A, B, C, H and other glycosides, the glycosides are more unstable , it is easier to be oxidized at high temperature such as tobacco smoking, so it can act as a protective agent for ligustilide, and the molecular structure of glycosides still has glycosyl units after high-temperature oxidation damage, and these glycosyl units can still Make its olfactory aroma "sweet", which can enhance aroma;

At the same time, in this scheme, 100% ethanol is used to extract the volatile oil with ligustilide as the main substance. Due to the solvation effect, the total energy of ligustilide in the solvent is reduced, the polarity of the solvent is large, and the solvation effect is strong. Make ligustilide more stable, and compared with non-anhydrous ethanol, the solubility of ligustilide is higher and the extraction rate is higher, and the water-soluble ferulic acid and ferulic acid coniferous cypress are extracted with solanic acid solution at the same time. Esters, succinic acid and other components can make full use of the contents in the stone kiln angelica, and solanic acid itself is degraded from cyperene substances, which has the basic aroma of tobacco, and the above-mentioned ligustilide and cistanche produce The aroma synergy makes the tobacco aroma more mellow;

The beneficial effects of the present invention are:

1. The natural aroma contained in the extract obtained by the present invention is coordinated with tobacco, and after being added to the tobacco leaf group formula, it has a better modification effect on the shape of the smoke, and simultaneously makes the aroma more abundant, and the smoke is soft and delicate. Tobacco aroma, improve the aroma and thick feeling, and have a good effect on improving the quality of tobacco;

2. The stone kiln angelica extract prepared by the present invention has good antibacterial activity;

3. The source of raw materials used in the present invention is easy to obtain, the preparation process is simple, and the cost is low, which is beneficial to production transformation;

4. The extract of Cistanche deserticola can act as a protective agent for ligustilide. After adding to tobacco, it can prevent the high temperature generated by tobacco burning from destroying the ligustilide, and protect the medicinal effect of Angelica sinensis. On the other hand, the extract can be used in the application When used in tobacco, its olfactory aroma has "sweetness", which can enhance the aroma;

5. The volatile oil and water-soluble components are extracted in steps, which improves the extraction rate of Angelica sinensis. At the same time, the extraction liquid solanaceous acid has the basic aroma of tobacco, which is synergistic with the aroma produced by ligustilide and cistanche, making the tobacco aroma more delicious. mellow.

Description of drawings

Accompanying drawing 1 is the extraction rate result of the active ingredient of the stone kiln angelica extract of embodiment 1-3 and comparative example 1-5;

Accompanying drawing 2 is the results of ligustilide extraction rate after the stone kiln angelica extracts of Examples 1-3 and Comparative Examples 1-5 are placed at 80°C for different times;

Accompanying drawing 3 is the antibacterial experiment result of the stone kiln angelica extract of Examples 1-3 and Comparative Examples 1-5.

Detailed ways

In order to make the content of the present invention easier to understand, the technical solutions of the present invention will be further described below with reference to specific embodiments, but the present invention is not limited thereto.

Example 1

A method for preparing a stone kiln angelica extract for tobacco flavoring, comprising the following steps:

S1. Take the mixture of Shiyao Angelica and Cistanche, grind and pulverize it with a mortar, and pass through a 200-mesh sieve, wherein the mass ratio of Shiyao Angelica and Cistanche is 4:1;

S2. filter the mixture after sieving with 100% ethanol 50 ℃ of leaching 1h to obtain filter residue and the first filtrate, and the first filtrate is distilled at atmospheric pressure to obtain distillate, wherein the temperature of atmospheric distillation is 70 ℃ °C;

S3. filter the residue after leaching with 0.1‰ solanic acid solution at 80°C for 6h to obtain the second filtrate, and the second filtrate is concentrated under reduced pressure to continuously evaporate water to a moisture content of 3% to obtain a concentrated solution;

S4. mix described distillate and concentrated solution, preserve in inert gas nitrogen, fluorocarbon gas environment, promptly obtain described stone kiln angelica extract;

Example 2

A method for preparing a stone kiln angelica extract for tobacco flavoring, comprising the following steps:

S1. Take the mixture of Shiyao Angelica and Cistanche, grind and pulverize it with a mortar, and pass through a 200-mesh sieve, wherein the mass ratio of Shiyao Angelica and Cistanche is 6:1;

S2. filter the mixture after sieving with 100% ethanol at 70°C for leaching 3h to obtain filter residue and the first filtrate, and the first filtrate is distilled at atmospheric pressure to obtain distillate, wherein the temperature of atmospheric distillation is 80 ℃ °C;

S3. filter residue with 0.2‰ solanic acid solution 95 DEG C leaching for 8h to obtain the second filtrate, and the second filtrate is concentrated under reduced pressure to continue evaporating water to a moisture content of 5% to obtain a concentrated solution;

S4. mix described distillate and concentrated solution, preserve in inert gas nitrogen, fluorocarbon gas environment, promptly obtain described stone kiln angelica extract;

Example 3

A method for preparing a stone kiln angelica extract for tobacco flavoring, comprising the following steps:

S1. Take the mixture of Shiyao Angelica and Cistanche, grind and pulverize it with a mortar, and pass through a 200-mesh sieve, wherein the mass ratio of Shiyao Angelica and Cistanche is 5:1;

S2. filter the mixture after sieving with 100% ethanol 60 ℃ of leaching for 2h to obtain filter residue and the first filtrate, and the first filtrate is distilled at atmospheric pressure to obtain distillate, wherein the temperature of atmospheric distillation is 75 ℃ °C;

S3. filter the residue after leaching with 0.15‰ solanic acid solution at 90°C for 7h to obtain a second filtrate, and the second filtrate is concentrated under reduced pressure to continuously evaporate water to a moisture content of 4% to obtain a concentrated solution;

S4. mix described distillate and concentrated solution, preserve in inert gas nitrogen, fluorocarbon gas environment, promptly obtain described stone kiln angelica extract;

Comparative Example 1

A method for preparing a stone kiln angelica extract for tobacco flavoring, comprising the following steps:

S1. Take the stone kiln Angelica and use a mortar to grind and pulverize it, and pass through a 200-mesh sieve;

S2. filter the mixture after sieving with 100% ethanol 70 ℃ of leaching 2h to obtain filter residue and the first filtrate, and the first filtrate is distilled at atmospheric pressure to obtain distillate, wherein the temperature of atmospheric distillation is 75 ℃ °C;

S3. filter the residue after leaching with 0.15‰ solanic acid solution at 90°C for 7h to obtain a second filtrate, and the second filtrate is concentrated under reduced pressure to continuously evaporate water to a moisture content of 4% to obtain a concentrated solution;

S4. mix described distillate and concentrated solution, preserve in inert gas nitrogen, fluorocarbon gas environment, promptly obtain described stone kiln angelica extract;

Comparative Example 2

A method for preparing a stone kiln angelica extract for tobacco flavoring, comprising the following steps:

S1. Take the stone kiln Angelica and use a mortar to grind and pulverize it, and pass through a 200-mesh sieve;

S2. filter the mixture after sieving with 100% ethanol 60 ℃ of leaching for 2h to obtain filter residue and the first filtrate, and the first filtrate is distilled at atmospheric pressure to obtain distillate, wherein the temperature of atmospheric distillation is 75 ℃ °C;

S3. filter the residue after leaching with 0.15‰ solanic acid solution at 90°C for 7h to obtain a second filtrate, and the second filtrate is concentrated under reduced pressure to continuously evaporate water to a moisture content of 4% to obtain a concentrated solution;

S4. mix described distillate and concentrated solution, preserve in inert gas nitrogen, fluorocarbon gas environment, promptly obtain described stone kiln angelica extract;

Comparative Example 3

A method for preparing a stone kiln angelica extract for tobacco flavoring, comprising the following steps:

S1. Take the mixture of Shiyao Angelica and Cistanche, grind and pulverize it with a mortar, and pass through a 200-mesh sieve, wherein the mass ratio of Shiyao Angelica and Cistanche is 5:1;

S2. filter the mixture after sieving with 60% ethanol 60 ℃ of leaching 2h to obtain filter residue and the first filtrate, and the first filtrate is distilled at atmospheric pressure to obtain distillate, wherein the temperature of atmospheric distillation is 75 ℃ °C;

S3. filter the residue after leaching with 0.15‰ solanic acid solution at 90°C for 7h to obtain a second filtrate, and the second filtrate is concentrated under reduced pressure to continuously evaporate water to a moisture content of 4% to obtain a concentrated solution;

S4. mix described distillate and concentrated solution, preserve in inert gas nitrogen, fluorocarbon gas environment, promptly obtain described stone kiln angelica extract;

Comparative Example 4

A method for preparing a stone kiln angelica extract for tobacco flavoring, comprising the following steps:

S1. Take the mixture of Shiyao Angelica and Cistanche, grind and pulverize it with a mortar, and pass through a 200-mesh sieve, wherein the mass ratio of Shiyao Angelica and Cistanche is 5:1;

S2. filter the mixture after sieving with 40% ethanol 60 ℃ of leaching 2h, obtain filter residue and the first filtrate, the first filtrate is distilled at atmospheric pressure to obtain distillate, wherein the temperature of atmospheric distillation is 75 ℃ °C;

S3. filter the residue after leaching with 0.15‰ solanic acid solution at 90°C for 7h to obtain a second filtrate, and the second filtrate is concentrated under reduced pressure to continuously evaporate water to a moisture content of 4% to obtain a concentrated solution;

S4. mix described distillate and concentrated solution, preserve in inert gas nitrogen, fluorocarbon gas environment, promptly obtain described stone kiln angelica extract;

Comparative Example 5

A method for preparing a stone kiln angelica extract for tobacco flavoring, comprising the following steps:

S1. Take the mixture of Shiyao Angelica and Cistanche, grind and pulverize it with a mortar, and pass through a 200-mesh sieve, wherein the mass ratio of Shiyao Angelica and Cistanche is 5:1;

S2. filter the mixture after sieving with 100% ethanol 60 ℃ of leaching for 2h to obtain filter residue and the first filtrate, and the first filtrate is distilled at atmospheric pressure to obtain distillate, wherein the temperature of atmospheric distillation is 75 ℃ °C;

S3. the filter residue is filtered after leaching with 0.15‰ ethanol aqueous solution at 90°C for 7h to obtain a second filtrate, and the second filtrate is concentrated under reduced pressure and continues to evaporate water to a moisture content of 4% to obtain a concentrated solution;

S4. mix described distillate and concentrated solution, preserve in inert gas nitrogen, fluorocarbon gas environment, promptly obtain described stone kiln angelica extract;

testing method

High performance liquid chromatography was used to test the content of active components in Shiyao Angelica extract. The content of ligustilide in the volatile oil was mainly, and the content of water-soluble components was mainly ferulic acid. For the chromatographic conditions and implementation steps of high-performance liquid chromatography testing the active ingredients in Angelica sinensis, see the published document "Comparison of the contents of ferulic acid, ligustilide and total polysaccharide in Angelica of different origins", Examples 1-3 and Comparative Examples 1- The extraction rate results of the active ingredients of the stone kiln angelica extract of 5 are shown in Figure 1, and the stone kiln angelica extracts of Examples 1-3 and Comparative Examples 1-5 were placed at 80 ° C for different times and were determined by the above method. The results of the extraction rate of ligustilide are shown in Figure 2;

The stone kiln angelica extracts of Example 1-3 and Comparative Example 1-5 were subjected to bacteriostatic experiments on three types of bacteria tested: Staphylococcus aureus, Salmonella and Listeria. After culturing for 5-7 days, the three types of bacteria were tested. The diameter of the inhibition zone of the test bacteria was used to judge the antibacterial activity of the Shiyao Angelica extract. The results are shown in Figure 3. Between -15 mm, it is moderately sensitive, that is, the extract has strong antibacterial activity against all three bacteria; and Angelica sinensis extract has the strongest antibacterial activity against Salmonella, and the diameter of the inhibition zone reaches 13.60±0.38 mm. Second is Listeria, and third is Staphylococcus aureus;

The Shiyao Angelica extracts of Examples 1-3 and Comparative Examples 1-5 were added to the tobacco as spices, and sensory evaluation was carried out. The addition amount of 0.1% is evenly sprayed on the blank cut tobacco after dissolving with ethanol, and the cut tobacco is dried to a moisture content of 14% under the condition of 65 ° C to make cigarettes, and sensory evaluation is carried out on the made cigarettes, wherein Example 1 The sensory evaluation of the subjects -3 is that the smoke is transparent, the amount of aroma is increased, the thickness of the smoke is improved, the smoke is soft and delicate, and it has an anti-asthma effect. The sensory evaluation of the subjects in the comparative example 1-2 is the smoke is transparent , increase the amount of aroma, the smoke is not thick enough, the smoke is soft and delicate, and the anti-asthma effect is not good. The sensory evaluation of the subjects in Comparative Examples 3-4 is that the smoke is weak, the aroma is insufficient, and the smoke is not thick enough. The smoke is soft and delicate, and has an anti-asthmatic effect. The sensory evaluation of the subjects in Comparative Example 5 is that the smoke smell is weak, the amount of increased aroma is insufficient, the thickness of the smoke is insufficient, the softness and fineness of the smoke is not good, and the smoke has an anti-asthmatic effect.

Specific embodiments of the present invention have been described above in detail.

It should be understood that those skilled in the art can make many modifications and changes according to the concept of the present invention without creative efforts. Therefore, all technical solutions that those skilled in the art can obtain through logical analysis, reasoning or limited experiments in the prior art with the inventive concept shall fall within the protection scope determined by the claims.

Claims (3)

1. A preparation method of Shiyao angelica extract for flavoring tobacco is characterized by comprising the following steps:

s1, taking a mixture of Chinese angelica and cistanche salsa, crushing and sieving;

s2, leaching the sieved mixture with 100% ethanol, filtering to obtain filter residue and first filtrate, and distilling the first filtrate at normal pressure to obtain distillate;

s3, leaching the filter residue with an solanic acid solution, filtering to obtain a second filtrate, and concentrating the second filtrate under reduced pressure to obtain a concentrated solution, wherein the concentration of the solanic acid solution is 0.1-0.2 per thousand;

s4, mixing the distillate and the concentrated solution, and storing in an inert gas environment to obtain the stone kiln angelica extract;

the mass ratio of the Chinese angelica to the cistanche deserticola is 4-6: 1; the temperature of the normal pressure distillation is 70-80 ℃; the leaching temperature in the step S2 is 50-70 ℃, the leaching time is 1-3h, the leaching temperature in the step S3 is 80-95 ℃, and the leaching time is 6-8 h.

2. The method for preparing the angelica shikou extract for flavoring tobacco as claimed in claim 1, wherein the water content of the concentrated solution is 3% -5%.

3. The method for preparing the angelica shikou extract for flavoring tobacco as claimed in claim 1, wherein the inert gas is one or more of nitrogen and fluorocarbon gas.

Images