CN114557475A

CN114557475A - Kedilao refined extract and preparation method and application thereof

Info

Publication number: CN114557475A
Application number: CN202210289045.XA
Authority: CN
Inventors: 温志勇; 赵旭
Original assignee: Xinhuozhizao Shenzhen Co ltd
Current assignee: Xinhuozhizao Shenzhen Co ltd
Priority date: 2022-03-22
Filing date: 2022-03-22
Publication date: 2022-05-31
Anticipated expiration: 2042-03-22
Also published as: CN114557475B

Abstract

The invention belongs to the technical field of spice preparation, and particularly relates to a kedilao extract and a preparation method and application thereof. The preparation method comprises the following steps: selecting raw materials of the kedilao, removing impurities, removing kernels and crushing to obtain crushed kedilao; performing subcritical extraction on the kedilao crushed aggregates to obtain kedilao extract; adding the kedilao extract into a molecular distillation device, performing molecular distillation, separation and purification to obtain a light component and a heavy component, and collecting the light component to obtain the kedilao refined extract. The kedilao extract prepared by the invention is applied to solid electronic smoke compound or liquid electronic smoke atomized liquid as a fragrant raw material, can remarkably enrich the fragrance and taste of electronic smoke, improves the sensory quality of smoke and endows the smoke kedilao with unique fragrance characteristics.

Description

Kedilao refined extract and preparation method and application thereof

Technical Field

The invention belongs to the technical field of spice preparation, and particularly relates to a kedilao extract and a preparation method and application thereof.

Background

The kedilao is a mature fruit of myrobalan which grows in dense forest of deep mountains in Yunnan province, also called yunnan green fruit, has the efficacies of moistening lung for arresting cough, promoting the production of body fluid for reducing phlegm, cooling and detoxifying, astringing for arresting diarrhea and the like, and is praised as a natural health-preserving medicine by people. The main components of the kedilao are organic acid, polyphenol, tannic acid and the like, which are reported in related documents. The kedilao is rarely applied to incense raw materials, and is extracted from one of 10 formula components including vetiver roots, kedilao, herba houttuyniae, couchgrass roots, reed roots, kudzu roots, platycodon grandiflorum, lemon peels, orange flowers and liquorice in CN113142646A and applied to cigarette essence, but the extraction mode adopts the traditional solvent extraction, and the mixture of the formula components is extracted without fine extraction, so that more impurities are generated, and solvent residues are easily caused.

With the increasing attention to the problems of smoking and health, the research and development of novel tobacco products capable of effectively reducing the release amount of harmful ingredients in tobacco has become the key point of industrial research. Among them, the most representative new tobacco products include liquid electronic cigarettes, solid electronic cigarettes (which do not burn when heated), and other atomization products.

The novel smoking article heats the solid or liquid state atomized substance through the heating source, and the heated aerosol is evaporated to meet the smoking requirement of consumers. The principle is heating evaporation, which is in a non-combustion state and does not produce tar, so that harmful ingredients generated by high-temperature combustion of the traditional cigarette are greatly reduced in the novel smoking article, and the harm to the health of consumers is obviously reduced.

The heating evaporation principle of the electronic cigarette determines the special requirements of the perfume raw materials in the application of the products, and the extract is directly applied to the formula of the electronic smog without refined extraction, so that the problems of core paste, insufficient perfume release and the like are caused.

Disclosure of Invention

In order to solve the technical problems, the invention provides a kedilao refined extract preparation method, so that kedilao extract is applied to a solid and liquid electronic smog compound formula of a novel fuming and atomizing product for the first time, and meanwhile, the preparation method also solves the problems of insufficient, elegant and pure fragrance, low sensory quality level and low product quality which are easily generated in the preparation process of a fragrance principle.

Specifically, the invention is realized by the following technical schemes:

in a first aspect, the invention provides a preparation method of kedilao extract, which comprises the following steps:

s01: providing a raw material of the kedilao, and carrying out selection, impurity removal, kernel removal and crushing treatment to obtain crushed kedilao;

s02: performing subcritical extraction on the kedilao crushed aggregates to obtain kedilao extract;

s03: adding the kedilao extract into a molecular distillation device, performing molecular distillation, separation and purification to obtain a light component and a heavy component, and collecting the light component to obtain the kedilao refined extract.

Alternatively, in the above preparation method, in step S01, the particle size of the kedilao particles is 10 to 200 mesh.

Alternatively, in the above preparation method, in step S02, the temperature of the subcritical extraction is 0 to 60 ℃, the extraction time is 0.5 to 3 hours, after the subcritical extraction is finished, the pressure of the equipment is adjusted, gas-liquid separation is performed, and the liquid fraction is collected to obtain the crude kedilao extract.

Alternatively, in the above preparation method, in step S02, the subcritical extraction is performed by co-treating a subcritical fluid and an entrainer, the subcritical fluid is one or more of propane, butane and dimethyl ether, the entrainer is one or more of ethanol, propylene glycol and glycerol, and the amount of the entrainer is 1% to 10% of the total weight of the kedilao particles.

Alternatively, in the above preparation method, in step S03, the molecular distillation apparatus has a distillation temperature of 10-100 ℃, a condensation temperature of 0-20 ℃, a pressure of 1-100Pa, and a rotation speed of 200-300 r/min.

In a second aspect, the invention provides a kedilao extract, which is prepared by the preparation method of the first aspect.

As an optional mode, in the kedilao refined extract, the main components of the kedilao refined extract are organic acid and volatile fragrant micromolecules, the aroma is pleasant, elegant and pure, the extract has a remarkable fragrant aroma, and the extract is transparent in color and easily soluble in common essence and spice solvents.

In a third aspect, the invention provides the use of the kedilao extract in the second aspect in preparing flavoring essence, essence for cigarette or essence for electronic cigarette.

As an alternative, in the above application, the kedilao extract is used in a formula of a liquid electronic aerosol or a solid electronic aerosol.

As an optional mode, in the above application, the liquid electronic cigarette aerosol formula comprises, by weight: 0-5% of nicotine salt, 20-50% of glycerol, 20-50% of propylene glycol, 0.01-50% of kedilao refined extract, 31-5% of cooling agent ws and 0.001-0.1% of neotame; or, the solid electronic smog compound formula comprises: 0-5% of nicotine salt, 20-50% of glycerol, 20-50% of propylene glycol, 0.01-50% of kedilao refined extract, 31-5% of cooling agent ws and 0.001-0.1% of neotame, wherein the solid electronic smoke compound formula is mixed with solid electronic smoke particles, the mixture is uniformly stirred for 1-2 hours in a rolling way, and the mixture is bagged and balanced for 24 hours to obtain the solid electronic smoke compound.

Preferably, the usage amount of the kedilao extract in the liquid electronic cigarette atomized liquid is 1-50% by weight percentage.

Preferably, the amount of the kedilao refined extract in the solid electronic smog compound is 1-60% by weight.

Compared with the prior art, the invention has the following beneficial effects:

the preparation method of the kedilao refined extract combines the subcritical extraction technology and the molecular distillation technology, and toxic and bad breath chemical reagents are not introduced in the extraction process, so that the preparation method has no residues of the toxic and bad breath chemical reagents, is pollution-free, accords with the green and environment-friendly concept, is easy for industrial production, and has better market application prospect.

In addition, the fludilac refined substance prepared by the preparation method disclosed by the invention is high in volatile micromolecule content, can be better applied to liquid electronic cigarettes and solid electronic cigarette incense raw material formulas, enriches the fragrance and the taste, and endows the cigarette with unique fludilac fragrance characteristics. Meanwhile, the problem of core pasting caused by application of the extract obtained by the traditional extraction method in the electronic cigarette is avoided.

Detailed Description

In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

The embodiment of the invention provides a preparation method of kedilao refined extract, which comprises the following steps:

s01: providing a raw material kedilao, and carrying out selection, impurity removal and crushing treatment to obtain crushed kedilao;

s03: adding the crude essential oil of the kedilao extract into molecular distillation equipment, adjusting the distillation temperature of the molecular distillation equipment to be 10-100 ℃, the condensation temperature to be 0-20 ℃, the pressure to be 1-100Pa and the rotating speed to be 200-300r/min, carrying out molecular distillation separation and purification to obtain a light component and a heavy component, and collecting the light component to obtain the kedilao refined extract.

Specifically, in step S01, the kedilao may be purchased from the market or may be prepared and obtained by itself. Specifically, the selection and impurity removal treatment is carried out to remove non-kedilao substances or rotten kedilao so as to reduce the impurity content in the obtained kedilao refined extract and improve the purity of the subsequently obtained kedilao refined extract. The kedilao after the selection, the impurity removal and the kernel removal is crushed so as to improve the efficiency of the subsequent subcritical extraction and the molecular distillation separation and purification as much as possible. Preferably, the particle size of the kedilao particles is 10-200 meshes.

In the step S02, the kedilao particles are placed in a subcritical extraction device for subcritical extraction. Preferably, the temperature of the subcritical extraction is 0-60 ℃, and the extraction time is 0.5-3 hours. The kedilao refined extract meeting the requirements of target components can be obtained at a proper subcritical extraction temperature. If the subcritical extraction temperature is too low or the extraction time is too short, fat-soluble components, particularly aroma components, in the kedilao crushed aggregates cannot be sufficiently and effectively extracted; if the subcritical extraction temperature is too high or the extraction time is too long, the aroma components in the kedilao crushed aggregates are easily cracked or decomposed mainly by volatile small molecular substances, and the extracted substances are changed, so that the key components of the kedilao refined extract cannot be obtained. In addition, the pressure of the subcritical extraction in the embodiment of the present invention is the saturated vapor pressure corresponding to the corresponding temperature.

Preferably, the subcritical fluid used for subcritical extraction is at least one of propane, butane and dimethyl ether. The preferable subcritical fluid is beneficial to fully extracting fragrance components such as small polar components linalool and linalyl acetate, and the obtained kedilao refined extract has better sensory quality. In addition, the preferable subcritical fluid is gaseous at normal temperature, liquid during extraction, sufficiently infiltrates with the raw material, and after the components are dissolved out, the pressure and temperature of the equipment are adjusted, and the subcritical fluid becomes gaseous, so that the solid-liquid separation of the product and the solvent is easily realized during the operation process, the reflux phenomenon is not generated, and the solvent can be completely removed. The method solves the problems of high temperature and incomplete removal in conventional solvent extraction and solvent recovery.

Further preferably, the subcritical extraction is realized by co-processing of subcritical fluid and entrainer, and the addition of the entrainer together with the subcritical fluid is beneficial to fully extracting essential oil components in the kedilao. Further, the entrainer is preferably at least one of ethanol, propylene glycol and glycerol. The optimized specific entrainer can prevent a large amount of non-essential oil components (impurity components) in the kedilao from dissolving out on the premise of ensuring that the essential oil components in the kedilao are fully extracted, so that the non-essential oil components (impurity components) in the obtained kedilao extract are not too high, subsequent molecular distillation separation and purification are facilitated, and the high-purity and high-quality kedilao refined extract is obtained. When the entrainer is more than two of ethanol, propylene glycol and glycerin, the volume ratio of each substance can be adjusted at will. Still more preferably, the materials of the entrainer are 1-10% of the total mass of the kedilao crushed aggregates. If the amount of the entrainer is not sufficient, the above effect is difficult to achieve; if the dosage of the entrainer is too much, the content of the subcritical fluid is not enough, and other impurities can be introduced by the too much entrainer, so that the subsequent operation difficulty is improved, and the high-quality kedilao extract is not favorably obtained. And after the subcritical extraction is finished, adjusting the pressure of equipment, carrying out gas-liquid separation, and collecting the liquid part to obtain the kedilao crude extract.

In the step S03, the distillation temperature of the molecular distillation equipment is adjusted to 10-100 ℃, the condensation temperature is adjusted to 0-20 ℃, the pressure is 1-100Pa, and the rotation speed is 200-300r/min, so as to form the conditions for molecular distillation separation and purification. In particular, the distillation temperature, the condensation temperature, the pressure, the rotation speed are within this range, which is adjusted according to variations of other factors, such as when the pressure is larger, the distillation temperature and/or the condensation temperature may be relatively lower. But the distillation temperature, condensation temperature, pressure, rotation speed cannot exceed the above ranges. When the distillation temperature is too low, active substances (low-polarity components) of the kedilao refined extract cannot be separated out; when the distillation temperature is too high, impurities, particularly large-polarity impurities, in the kedilao crude extract essential oil are also separated, so that the purpose of separation and purification cannot be achieved. When the condensation temperature is too high, the condensation effect cannot be realized, and the active ingredients of the kedilao refined extract cannot be enriched; which condensation temperature is difficult to achieve and increases the energy consumption. In the ranges of the distillation temperature (10-100 ℃) and the condensation temperature (0-20 ℃), the corresponding range of the pressure is 1-100Pa, and the rotating speed is 200-300 r/min.

Under the conditions, volatile small molecules and organic acid are enriched to light components through molecular distillation separation and purification, and long-chain fatty acid, squalene, triterpenoid and other high-boiling-point macromolecules are remained in heavy components, so that the purposes of separation and purification are achieved. The kedilao refined extract obtained by molecular distillation has pleasant fragrance, elegant and pure flavor and obvious faint scent and aroma; transparent color, beautiful appearance, and easy dissolution in common essence and perfume solvents such as alcohol, propylene glycol, glycerol, etc. The Kedilao refined extract obtained by the embodiment of the invention mainly comprises organic acid and volatile aroma molecules, and has wide application prospects in the fields of blending edible essence, tobacco essence, electronic cigarette essence and the like.

The light component obtained in the step S03 is the kedilao extract of the present invention, and can be applied to a liquid electronic cigarette atomized liquid formula, and the formula comprises, by weight: 0-5% of nicotine salt, 20-50% of glycerol, 20-50% of propylene glycol, 0.01-50% of kedilao refined extract, 1-5% of ws-3 (cooling agent) and 0.001-0.1% of neotame.

The light component obtained in the step S03 is the kedilao extract of the present invention, and can be applied to a solid electronic aerosol formulation, and the formulation comprises, by weight: 0-5% of nicotine salt, 20-50% of glycerol, 20-50% of propylene glycol, 0.01-50% of kedilao refined extract, 1-5% of ws-3 (cooling agent) and 0.001-0.1% of neotame. And (3) mixing the solid electronic smog substance with the solid electronic cigarette fuming particles, uniformly rolling and stirring for 1-2 hours, bagging and balancing for 24 hours to obtain the solid electronic smog substance. The solid electronic smog substance accounts for 1-50% of the mass ratio of the fuming particles.

Preparation examples:

example 1:

the kedilao refined extract is prepared by the following steps:

s01: providing a raw material of the kedilao, and carrying out selection, impurity removal, kernel removal and crushing treatment to obtain crushed kedilao, wherein the particle size of the crushed kedilao is 100 meshes;

s02: performing subcritical extraction on the Kedilao crushed aggregates, wherein the temperature of the subcritical extraction is 40 ℃, the extraction time is 1.5 hours, after the subcritical extraction is finished, adjusting the pressure of equipment, performing gas-liquid separation, and collecting the liquid part to obtain a Kedilao crude extract, wherein the subcritical extraction is realized by co-processing a subcritical fluid and a entrainer, the subcritical fluid is a mixture of propane, butane and dimethyl ether, and the proportion of the three gases is 2: 2: 1, the entrainer is a mixture of ethanol and propylene glycol, and the weight ratio of the two entrainers is 2: 1, the dosage of the entrainer accounts for 10 percent of the total weight of the kedilao crushed aggregates;

s03: adding the kedilao extract into a molecular distillation device, performing molecular distillation separation and purification, wherein the distillation temperature of the molecular distillation device is 60 ℃, the condensation temperature is 10 ℃, the pressure is 60Pa, and the rotating speed is 250r/min, so as to obtain a light component and a heavy component, and collecting the light component, so as to obtain the kedilao refined extract.

Example 2:

the preparation method of the kedilao refined extract comprises the following steps:

s01: providing raw materials of the kedilao, and carrying out selection, impurity removal, kernel removal and crushing treatment to obtain crushed kedilao, wherein the particle size of the crushed kedilao is 100 meshes;

s02: performing subcritical extraction on the Kedilao crushed aggregates, wherein the temperature of the subcritical extraction is 30 ℃, the extraction time is 2 hours, after the subcritical extraction is finished, adjusting the pressure of equipment, performing gas-liquid separation, and collecting the liquid part to obtain a Kedilao crude extract, wherein the subcritical extraction is realized by co-processing a subcritical fluid and a entrainer, the subcritical fluid is a mixture of propane, butane and dimethyl ether, and the proportion of the three gases is 2: 2: 1, the entrainer is a mixture of ethanol, propylene glycol and glycerol, and the weight ratio of the three entrainers is 1: 1: 1, the using amount of the entrainer accounts for 8% of the total weight of the kedilao particles;

s03: adding the kedilao extract into a molecular distillation device, performing molecular distillation separation and purification, wherein the distillation temperature of the molecular distillation device is 60 ℃, the condensation temperature is 10 ℃, the pressure is 80Pa, and the rotating speed is 250r/min, so as to obtain a light component and a heavy component, and collecting the light component, so as to obtain the kedilao refined extract.

Example 3:

the kedilao refined extract is prepared by the following steps:

s02: performing subcritical extraction on the Kedilao crushed aggregates, wherein the temperature of the subcritical extraction is 50 ℃, the extraction time is 1 hour, after the subcritical extraction is finished, adjusting the pressure of equipment, performing gas-liquid separation, and collecting the liquid part to obtain a Kedilao crude extract, wherein the subcritical extraction is realized by co-treating a subcritical fluid and a entrainer, the subcritical fluid is a mixture of propane, butane and dimethyl ether, and the proportion of the three gases is 1: 1: 1, the entrainer is a mixture of ethanol and glycerol, and the weight ratio of the two entrainers is 2: 1, the dosage of the entrainer accounts for 10 percent of the total weight of the kedilao crushed aggregates;

s03: adding the kedilao extract into a molecular distillation device, performing molecular distillation separation and purification, wherein the distillation temperature of the molecular distillation device is 60 ℃, the condensation temperature is 10 ℃, the pressure is 70Pa, and the rotating speed is 250r/min, so as to obtain a light component and a heavy component, and collecting the light component, so as to obtain the kedilao refined extract.

Effect embodiment: sensory quality evaluation

(1) Preparation of test samples:

electronic cigarette products prepared from the kedilao refined extract prepared in the embodiments 1, 2 and 3 of the invention are selected as samples.

An electronic cigarette smoking product prepared by an essence formula without adding kedilao refined extract components is used as a comparative example 1, and an electronic cigarette product prepared by the sweet flavor type vetiver root composite extract prepared by the preparation method of example 1 in CN113142646A is used as a comparative example 2.

The amount of the kedilao extract in examples 1-3 and the amount of the sweet and fragrant type vetiver root composite extract in the electronic cigarette product in comparative example 2 are the same.

(2) Sensory quality evaluation criteria:

integrally setting 6 evaluation items, including: fragrant quality, fragrant amount, sweet and greasy feeling, irritation, miscellaneous gas, and aftertaste. The maximum scale of each evaluation item is 9 points, each evaluation item is divided into scoring units by 1, and specific evaluation criteria are shown in table 1.

Table 1: evaluation standard of sensory quality of electronic cigarette

Score value

Quality of fragrance

Amount of fragrance

Sweet and greasy feeling

Irritation property

Miscellaneous qi

Aftertaste

9

Is very good

Sufficient (sufficient)

Is very light

Very small

Is very light

Is very good

8

Good taste

Foot

Bland taste

Small

Light and lightweight

Good taste

7

Is preferably used

Relatively big foot

Is relatively light

Is smaller

Is lighter

Is preferably used

6

Slightly better

Little foot

Slightly bland

Is a little bit smaller

Is slightly light

Slightly better

5

In

4

A little bit worse

Is slightly provided with

Slightly concentrated

Slightly larger

Is a little heavier

A little bit worse

3

Poor quality

Is relatively light

Is thicker

Is larger than

Heavy weight

Poor quality

2

Difference (D)

Bland taste

Concentrated

Big (a)

Heavy load

Difference (D)

1

Is very poor

Is very light

Is very dense

Is very big

Is very heavy

Is very poor

(3) The evaluation method comprises the following steps: providing a sample and a sensory quality evaluation standard table for an expert in the smoking technique, and smoking each index according to the requirements of the table.

(4) And (4) counting results: the result of the smoking of all technical experts is effective, the arithmetic mean value of the single smoking result of each smoking expert is calculated, the result is reserved to 1 decimal, the arithmetic mean values of the single items are added, the total score is obtained, and the result is shown in table 2.

Table 2: sensory quality evaluation results

Score value	Quality of fragrance	Amount of fragrance	Sweet and greasy feeling	Irritation property	Miscellaneous qi	Aftertaste	Total score
								Example 1	7.5	7.1	7.5	7.4	7.2	7.3	44.0
Example 2	7.6	7.4	7.2	7.4	7.4	7.4	44.4
								Example 3	7.3	7.5	7.2	7.4	7.3	7.3	44.0
Comparative example 1	5.5	5.5	6.0	6.5	6.0	6.0	35.5
								Comparative example 2	6.5	6.5	6.0	7.0	7.2	7.0	40.2

As can be seen from table 3, compared with the electronic cigarette smoking article without the kedilao extract and the electronic cigarette smoking article including the known kedilao-containing composite extract in the prior art, the kedilao extract electronic cigarette smoking article provided in embodiments 1 to 3 of the present invention has a consumer experience of more comfortable taste, more pleasant aroma quality, less irritation, and better smoking quality.

It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims

1. A preparation method of Kedilao refined extract is characterized by comprising the following steps: the method comprises the following steps:

s02: performing subcritical extraction on the kedilao crushed aggregates to obtain a kedilao extract;

2. The method of claim 1, wherein: in step S01, the particle size of the kedilao particles is 10-200 mesh.

3. The production method according to claim 1 or claim 2, characterized in that: in step S02, the temperature of the subcritical extraction is 0 to 60 ℃, the extraction time is 0.5 to 3 hours, after the subcritical extraction is finished, the pressure of the equipment is adjusted, gas-liquid separation is performed, and the liquid part is collected to obtain the crude extract of kedilao.

4. The production method according to any one of claims 1 to 3, characterized in that: in step S02, the subcritical extraction is implemented by co-processing a subcritical fluid and an entrainer, the subcritical fluid is one or more of propane, butane and dimethyl ether, the entrainer is one or more of ethanol, propylene glycol and glycerol, and the amount of the entrainer is 1% to 10% of the total weight of the kedilao particles.

5. The production method according to any one of claims 1 to 4, characterized in that: in step S03, the molecular distillation equipment has a distillation temperature of 10-100 ℃, a condensation temperature of 0-20 ℃, a pressure of 1-100Pa, and a rotation speed of 200-300 r/min.

6. A kedilao refined extract is characterized in that: the kedilao refined extract is prepared by the preparation method of any one of claims 1 to 5.

7. The kedilao refined extract according to claim 6, characterized in that: the Kedilao refined extract mainly comprises organic acid and volatile fragrant micromolecules, is pleasant in fragrance, elegant, pure, transparent in color and easy to dissolve in common essence and spice solvents.

8. Use of the kedilao raisin according to claim 6 or claim 7 in the formulation of flavourings, flavours for cigarettes or flavours for electronic cigarettes.

9. Use according to claim 8, characterized in that: the kedilao refined extract is used in the formula of liquid electronic smoke atomized liquid or solid electronic smoke atomized compound.

10. Use according to claim 9, characterized in that: the liquid electronic cigarette atomized liquid comprises the following components in percentage by weight: 0-5% of nicotine salt, 20-50% of glycerol, 20-50% of propylene glycol, 0.01-50% of kedilao refined extract, 31-5% of cooling agent ws and 0.001-0.1% of neotame; or, the solid electronic smog compound formula comprises: 0-5% of nicotine salt, 20-50% of glycerol, 20-50% of propylene glycol, 0.01-50% of kedilao refined extract, 31-5% of cooling agent ws and 0.001-0.1% of neotame, wherein the solid electronic smoke compound formula is mixed with solid electronic smoke particles, the mixture is uniformly stirred for 1-2 hours in a rolling way, and the mixture is bagged and balanced for 24 hours to obtain the solid electronic smoke compound.