CN113773908A

CN113773908A - Preparation method and application of jasmine extract with antioxidant activity

Info

Publication number: CN113773908A
Application number: CN202111112819.3A
Authority: CN
Inventors: 刘劲芸; 常健; 张虹娟; 吴恒; 杜超; 王浩雅; 王厚娴; 李朝华; 曹正东; 李宏坤; 陈婉
Original assignee: Yunnan China Tobacco New Material Technology Co ltd
Current assignee: Yunnan China Tobacco New Material Technology Co ltd
Priority date: 2021-09-23
Filing date: 2021-09-23
Publication date: 2021-12-10

Abstract

The invention discloses a preparation method and application of a jasmine flower extract with antioxidant activity. The method can fully break cell walls by pretreating and performing enzymolysis on the jasmine flowers, so that effective components in the cell walls are diffused as much as possible, and the later-stage extraction and separation are facilitated. The extract prepared by the method has good antioxidant activity and can be used as a natural antioxidant substance. The extract is safe and nontoxic, can be used as a spice to improve the aroma quality of cigarettes, can prevent the decay and deterioration of the cigarette spice and prolong the shelf life of the cigarette spice.

Description

Preparation method and application of jasmine extract with antioxidant activity

Technical Field

The invention relates to the technical field of production of tobacco flavor and fragrance, and particularly relates to a preparation method and application of a jasmine extract with antioxidant activity.

Background

A heating cigarette (Heat-not-Burn) is also called a low-temperature cigarette, and is a novel tobacco product which is heated by a special Heat source (below 500 ℃ or even lower), and the flavor substances are volatilized to generate smoke gas to meet the requirements of consumers during heating. Compared with the traditional cigarette, the reduction of most harmful components in the smoke of the heated cigarette is more than 90%. However, the heating temperature of the heated cigarette is low, and part of aroma components can not be released during smoking, so that the heated cigarette is weak in characteristic aroma. In order to enrich the aroma characteristics of the heated cigarette and improve the smoking feeling of consumers, a large amount of essence and spice with characteristic aroma needs to be additionally added into cigarette raw materials to compensate the smoke aroma, and the sensory quality of the heated cigarette is ensured and improved by an aroma blending mode.

Many natural aroma compounds in the cigarette essence contain easily-oxidized unsaturated double bonds, and are easily oxidized in the storage process to change the aroma quality. The reasonable addition of the antioxidant can delay the oxidation of the essence and the spice of the cigarette and prolong the storage period. With the safety of cigarette additives becoming a focus of people's attention, the selection of cigarette additives tends to natural and healthy materials, and natural plants become an important source of antioxidants. The natural antioxidant ingredient is far less toxic than the synthetic antioxidant. Therefore, studies on natural antioxidants have attracted a high degree of attention from scholars.

Jasmine (Jasminum sambac (L.) Aiton) is a tropical flower of Jasminum in Oleaceae. Jasmine flower has fresh and elegant fragrance, and is a famous spice crop from ancient times. The flower, leaf and root of jasmine have medicinal value, and have antioxidant, antidepressant, antibacterial, antifungal and antiviral activities. Jasmine essential oil is known as the king of essential oil, and has high price and elegant smell. Therefore, the jasmine essential oil is widely applied to the fields of daily chemicals, foods, spices, medical treatment and the like. The jasmine essential oil is also a common spice for the traditional cigarettes, and has the effects of increasing fresh and sweet fragrance, softening smoke, reducing irritation and the like when being applied to the cigarettes.

At present, the jasmine flower is extracted by adopting solvents such as ethanol, petroleum ether and the like at home and abroad through thermal reflux or ultrasonic extraction and is applied to the traditional cigarette. However, the organic solvent can cause more loss of the antioxidant active ingredients and small molecular fragrance substances of the jasmine flowers, and influence the fragrance quality. And the use amount of the organic solvent is large, the extraction process is complex, the preparation cost is high, and adverse effects on the environment are easily caused.

For example, in patent (CN 101317692A), an additive for jasmine flower fragrance type cigarette, its preparation method and application, the main raw material is jasmine flower. The preparation method comprises heating and refluxing with petroleum ether or ethanol solution or soaking at room temperature to extract flos Jasmini sambac, filtering the extractive solution, concentrating under reduced pressure to obtain flos Jasmini sambac extract, and mixing with Mel at a certain ratio to obtain flos Jasmini sambac additive for cigarette. Dissolving the additive for the jasmine flower fragrance type cigarette in ethanol and propylene glycol with certain concentration to form a saturated solution, uniformly spraying the saturated solution on cut tobacco, cut stems or tobacco sheets of the cigarette, and rolling the cut tobacco, the cut stems or the tobacco sheets into cigarettes. The dosage of the jasmine flower additive for the cigarette is 0.01-5% of the weight of the tobacco shreds, the tobacco stems or the tobacco sheets.

The preparation method adopts solvents such as ethanol and petroleum ether, has long treatment time and complicated extraction process, and the extract is water-soluble component of flos Jasmini sambac, and has less antioxidant active component and poor antioxidant ability.

Disclosure of Invention

In order to solve the problems, the invention provides a preparation method and application of a jasmine flower extract with antioxidant activity. The extract is safe and nontoxic, can be added into tobacco shreds as a spice to improve the aroma quality of cigarettes, prevent the cigarette spice from going bad, and prolong the shelf life of the cigarette spice.

In order to achieve the above objects, the present invention provides a method for preparing a jasmine extract having antioxidant activity, which comprises the following steps:

s1, removing impurities from the jasmine, pretreating, filtering and washing to obtain pretreated jasmine;

preferably, the pretreatment process in S1 is as follows: placing jasmine in 0.5-1% diluted hydrochloric acid, and treating at 20-40 deg.C for 5-10 min.

The jasmine flower is pretreated, and aims to destroy the original structure of jasmine flower cell walls, separate or remove part of lignin, reduce the crystallinity of cellulose and increase the porosity of a jasmine flower substrate, so that the mass transfer coefficient of jasmine flower fluid in a material and the accessibility of the substrate are improved. The mass transfer coefficient is improved, so that the transfer rate of a subsequent biocatalyst such as a chemical reagent, a microorganism or a hydrolase in a substrate can be increased, the reaction rate is improved, the diffusion rate of substances in cell walls of the jasmine flowers can be improved, the contact area of the jasmine flowers and a solvent is increased, the inhibition effect of diffusion is reduced, and the reaction is promoted to be carried out towards the positive reaction; the accessibility of the substrate is improved, and the target components in the jasmine flowers are mainly selectively separated, so that the target functional groups are fully exposed.

Therefore, the jasmine flower is pretreated by dilute acid, so that a large amount of hemicellulose in cell walls can be hydrolyzed, a small amount of lignin can be removed, and the acid bond connection between the cinnamic acid and the lignin can be broken, so that the accessibility of cellulose and other target components can be increased.

S2, adding the pretreated jasmine obtained in the step S1 into deionized water with the mass being 20 times that of the jasmine, leaching for 10-20min, adding 1% of combined enzyme by mass, adjusting the pH value to 4.0-5.0, hydrolyzing in a magnetic stirring oil bath kettle at the temperature of 20-50 ℃ at the rotating speed of 200r/min for 15-20min, centrifuging the hydrolyzed sample for 15-20min at 3200r/min, and then passing through a fiber ultrafiltration membrane to obtain clear liquid and filter residue;

the invention also selectively enzymolyzes the cellulose and hemicellulose components of the plant cell wall by adding the combined enzyme, thereby enabling other components in the plant cell to be extracted more easily.

S3, placing the filter residue obtained in the step S2 in a supercritical extraction kettle, adding ethanol, performing supercritical extraction to obtain an extract, freezing the extract at 4 ℃ for 6-24h, and filtering to obtain a jasmine flower extract;

s4, performing primary molecular distillation on the jasmine flower extract obtained in the step S3 to obtain a primary distillate, performing secondary molecular distillation on the primary distillate, and collecting the obtained light component extract, namely the jasmine flower extract.

The molecular distillation is a separation process which takes gas phase molecules escaping from a liquid phase as a main body by means of gas diffusion, realizes substance separation by utilizing the property that the average free path of the liquid molecules is different after the liquid molecules are heated, and has a special mass and heat transfer mechanism. The liquid mixture is heated and molecules with enough energy escape from the liquid surface at the temperature lower than the boiling point, the average free path of light molecules is larger than that of heavy molecules, the light molecules are evaporated at a high speed, if the catcher is arranged above the liquid surface and is smaller than the average free path of the light molecules and larger than the average free path of the heavy molecules, the light molecules are continuously condensed and caught, the dynamic balance of the light molecules is broken, the light molecules in the mixture continuously escape, and the heavy molecules tend to be dynamically balanced quickly because the heavy molecules cannot reach the catcher, and do not escape from the mixed liquid, so that the separation of the light molecules and the heavy molecules is realized.

Therefore, the invention adopts supercritical CO₂The extraction method and the molecular distillation purification method are combined, extraction is carried out at a lower temperature, so that the active ingredients can be prevented from being damaged by heating, and the antioxidant activity and the aroma quality of the product are improved. And by molecular distillationPurifying the extract, and separating heat-sensitive substances from flos Jasmini sambac under high vacuum condition, wherein the method has the operation temperature lower than the boiling temperature of antioxidant substances under normal pressure, short heating time and high separation degree, and can not damage antioxidant active substances and aroma components of flos Jasmini sambac, and improve the purity of antioxidant substances.

Preferably, the combined enzyme in the S2 is a mixture of cellulase, hemicellulase, beta-glucanase and pectinase, and the mass ratio of the cellulase, the hemicellulase, the beta-glucanase and the pectinase is 1:1:1: 1.

Preferably, the supercritical extraction conditions in S3 are as follows: the extraction temperature of the carbon dioxide fluid is 30-55 ℃, the pressure is 15-40MPa, and the flow of the carbon dioxide is 3-30L/h; the pressure of the separation kettle is 5.0-10.0MPa, and the separation temperature is 25-40 ℃; the extraction time is 0.5-3 h.

Preferably, the mass ratio of the filter residue to the ethanol in the S3 is 100: (5-15).

Preferably, the distillation conditions of the first molecular distillation in S4 are as follows: the pressure in the molecular distiller system is 10-50 Pa, the feeding rate is 2.0mL/min, the rotating speed of a knifing is 300rpm, the distilling temperature is 30-60 ℃, the condensing temperature is 10-25 ℃, and the preheating temperature is 20-50 ℃.

Preferably, the distillation conditions of the secondary molecular distillation in S4 are as follows: the distillation pressure is 10-50 Pa, the rotating speed of the knifing is 300rpm, the material flow rate is 2 mL/min, the distillation temperature is 60-80 ℃, the condensation temperature is 10-25 ℃, and the preheating temperature is 50-70 ℃.

In another aspect, the present invention provides the use of the jasmine extract with antioxidant activity prepared as described above, and specifically as follows, the natural perfume is used to add to a heated cigarette.

Preferably, the jasmine flower extract is diluted and injected into the cigarette core of the heated cigarette by adopting an essence and spice injection machine to prepare the heated cigarette.

Preferably, the mass ratio of the jasmine flower extract to the heating cigarette core material is (1-5): 1000.

the invention has the beneficial effects that:

1. according to the preparation method of the jasmine extract with the antioxidant activity, provided by the invention, the cell walls can be sufficiently broken through the pretreatment and enzymolysis of the jasmine, so that the effective components in the cell walls are diffused as much as possible, and the later-stage extraction and separation are convenient.

2. The jasmine extract contains a large amount of compounds such as plant alcohol, methyl jasmonate, eugenol, terpenes and the like, has good antioxidant activity, and the content of the compounds is much higher than that of jasmine perfume extracted by conventional petroleum ether. Moreover, the activity of eliminating DPPH and ABTS free radicals of the jasmine extract is obviously higher than that of the jasmine extract prepared by the traditional petroleum ether extraction method, so that the jasmine extract can be used as a natural antioxidant substance and has higher economic benefit.

3. According to the preparation method and the application of the jasmine extract with the antioxidant activity, the jasmine extract can well delay oxidative deterioration of aroma components in the spice of the heated cigarette and has the effect of prolonging the quality guarantee period of the heated cigarette. Therefore, the jasmine flower extract can be used as a spice to improve the aroma quality of cigarettes and can also be used for preventing the cigarette spice from being rotten and deteriorated.

Drawings

FIG. 1 is a flow chart of a method for preparing an extract of jasmine flower with antioxidant activity according to an embodiment of the present invention;

FIG. 2 is a graph of DPPH radical scavenging efficiency of jasmine extracts prepared in example 2 and comparative example 1;

fig. 3 is a graph showing ABTS free radical scavenging rates of the jasmine extracts prepared in example 2 and comparative example 1.

Detailed Description

In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the following will describe the specific embodiments of the present invention with reference to the accompanying drawings.

It is obvious that the drawings in the following description are only some examples of the invention, and it is obvious to a person skilled in the art that other drawings and other embodiments can be obtained from these drawings without inventive effort, and the invention is not limited to this example.

The specific embodiment of the invention is as follows:

example 1

A preparation method of flos Jasmini sambac extract with antioxidant activity comprises the following steps:

s1, taking Yunnan Yuanjiang bivalve jasmine as a raw material, removing leaves and impurities, then placing the jasmine in dilute hydrochloric acid with the mass concentration of 0.5%, treating for 10min at 30 ℃, filtering and washing to obtain the pretreated jasmine.

S2, adding 500g of the pretreated jasmine obtained in the step S1 into 10L of deionized water for leaching for 10min, then adding 100g of combined enzyme, adjusting the pH value to 4.0, hydrolyzing at a 30 ℃ magnetic stirring oil bath pot at a rotating speed of 200r/min for 20min, centrifuging the hydrolyzed sample at 3200r/min for 15min, and then passing through a fiber ultrafiltration membrane to obtain clear liquid and filter residue.

S3, placing the filter residue obtained in the step S2 in a supercritical extraction kettle, adding edible ethanol with the mass concentration of 95%, performing supercritical extraction to obtain an extract, freezing the extract at 4 ℃ for 6 hours, and filtering to obtain a yellow oily jasmine flower extract. The conditions of the supercritical extraction are as follows: the extraction temperature of the carbon dioxide fluid is 30 ℃, the pressure is 15MPa, and the flow of the carbon dioxide is 3L/h; the pressure of the separation kettle is 5.0MPa, and the separation temperature is 25 ℃; the extraction time was 0.5 h. Wherein the mass ratio of the filter residue to the ethanol is 100: 5.

s4, performing primary molecular distillation on the jasmine flower extract obtained in the step S3 to obtain a primary distillate, wherein the distillation conditions of the primary molecular distillation are as follows: the pressure in the molecular distiller system is 10Pa, the feeding rate is 2.0mL/min, the rotating speed of a knifing is 300rpm, the distilling temperature is 30 ℃, the condensing temperature is 10 ℃, and the preheating temperature is 20 ℃. And (3) performing secondary molecular distillation to remove heavy component impurities, wherein the distillation conditions of the secondary molecular distillation are as follows: the distillation pressure is 10Pa, the film scraping rotation speed is 300rpm, the material flow rate is 2 mL/min, the distillation temperature is 60 ℃, the condensation temperature is 10 ℃, and the preheating temperature is 50 ℃. Collecting the light component extract obtained by secondary distillation, namely the jasmine flower extract.

Example 2

s1, taking Yunnan Yuanjiang bivalve jasmine as a raw material, removing leaves and impurities, then placing the jasmine in dilute hydrochloric acid with the mass concentration of 0.8%, treating for 8min at 25 ℃, filtering and washing to obtain the pretreated jasmine.

S2, adding 800g of the pretreated jasmine obtained in the step S1 into 15L of deionized water for leaching for 15min, then adding 150g of combined enzyme, adjusting the pH value to 4.5, hydrolyzing for 18min at a speed of 200r/min in a magnetic stirring oil bath kettle at 35 ℃, centrifuging the hydrolyzed sample for 18min at 3200r/min, and then passing through a fiber ultrafiltration membrane to obtain clear liquid and filter residue.

S3, placing the filter residue obtained in the step S2 in a supercritical extraction kettle, adding ethanol with the mass concentration of 95%, performing supercritical extraction to obtain an extract, freezing the extract at 4 ℃ for 12 hours, and filtering to obtain a yellow oily jasmine flower extract. The conditions of the supercritical extraction are as follows: the extraction temperature of the carbon dioxide fluid is 45 ℃, the pressure is 25MPa, and the flow of the carbon dioxide is 10L/h; the pressure of the separation kettle is 8.0MPa, and the separation temperature is 35 ℃; the extraction time was 2 h. Wherein the mass ratio of the filter residue to the ethanol is 100: 10.

s4, performing primary molecular distillation on the jasmine flower extract obtained in the step S3 to obtain a primary distillate, wherein the distillation conditions of the primary molecular distillation are as follows: the pressure in the molecular distiller system is 20Pa, the feeding rate is 2.0mL/min, the rotating speed of a knifing is 300rpm, the distilling temperature is 50 ℃, the condensing temperature is 10 ℃, and the preheating temperature is 40 ℃. And (3) performing secondary molecular distillation to remove heavy component impurities, wherein the distillation conditions of the secondary molecular distillation are as follows: the distillation pressure is 30 Pa, the film scraping rotation speed is 300rpm, the material flow rate is 2 mL/min, the distillation temperature is 70 ℃, the condensation temperature is 15 ℃, and the preheating temperature is 60 ℃. Collecting the light component extract obtained by secondary distillation, namely the jasmine flower extract.

Example 3

s1, taking Yunnan Yuanjiang bivalve jasmine as a raw material, removing leaves and impurities, then placing the jasmine in 1% dilute hydrochloric acid by mass concentration, treating at 20 ℃ for 10min, filtering and washing to obtain the pretreated jasmine.

S2, adding 1kg of pretreated jasmine obtained in the step S1 into 20L of deionized water, leaching for 20min, adding 200g of combined enzyme, adjusting the pH value to 5.0, hydrolyzing for 15min at a 40 ℃ magnetic stirring oil bath at a rotating speed of 200r/min, centrifuging the hydrolyzed sample for 20min at 3200r/min, and passing through a fiber ultrafiltration membrane to obtain clear liquid and filter residue.

S3, placing the filter residue obtained in the step S2 in a supercritical extraction kettle, adding ethanol with the mass concentration of 80%, performing supercritical extraction to obtain an extract, freezing the extract at 4 ℃ for 24 hours, and filtering to obtain a yellow oily jasmine flower extract. The conditions of the supercritical extraction are as follows: the extraction temperature of the carbon dioxide fluid is 55 ℃, the pressure is 40MPa, and the flow rate of the carbon dioxide is 30L/h; the pressure of the separation kettle is 10.0MPa, and the separation temperature is 40 ℃; the extraction time was 3 h. Wherein the mass ratio of the filter residue to the ethanol is 100: 15.

s4, performing primary molecular distillation on the jasmine flower extract obtained in the step S3 to obtain a primary distillate, wherein the distillation conditions of the primary molecular distillation are as follows: the pressure in the molecular distiller system is 50Pa, the feeding rate is 2.0mL/min, the rotating speed of a knifing is 300rpm, the distilling temperature is 60 ℃, the condensing temperature is 25 ℃, and the preheating temperature is 50 ℃. And (3) performing secondary molecular distillation to remove heavy component impurities, wherein the distillation conditions of the secondary molecular distillation are as follows: the distillation pressure is 50Pa, the film scraping rotation speed is 300rpm, the material flow rate is 2 mL/min, the distillation temperature is 80 ℃, the condensation temperature is 25 ℃, and the preheating temperature is 70 ℃. Collecting the light component extract obtained by secondary distillation, namely the jasmine flower extract.

Comparative example 1

On the basis of example 2, the supercritical extraction was replaced by conventional petroleum ether solvent extraction to obtain jasmine flower extract.

Test example 1

The jasmine extracts prepared in example 2 and comparative example 1 were examined by gas chromatography-mass spectrometry combined with GC-MS analysis:

gas chromatography conditions: the chromatographic column is DB-5MS (30 m × 0.25 mm, 0.25 μm); the temperature of a sample inlet is 220 ℃; the carrier gas is high-purity helium gas, and the flow rate is 1 ml/min; the split ratio is 20: 1, sampling amount is 2 mu l; temperature programming: the initial column temperature was 50 ℃ and held for 5min, and the temperature was raised to 200 ℃ at a rate of 5 ℃/min and held for 10 min. Mass spectrum conditions: electron bombardment ion source; the electron energy is 70 eV; the ion source temperature is 220 ℃; the temperature of the transmission line is 220 ℃; the scanning range is 40-400 amu, the solvent delay: 3 min.

And (3) searching in an NIST standard spectrum library by using a chemical workstation data processing system, and carrying out spectrogram analysis by combining with related documents to carry out qualitative analysis. And calculating the relative content of each component by adopting a peak area normalization method according to the ratio of the peak area of each aroma component to the total peak area.

The contents of the specific components are shown in Table 1.

Table 1 comparison of the components and relative amounts of jasmine extracts prepared in example 2 and comparative example 1

Note: "-" indicates that the component was not detected.

As can be seen from table 1, the jasmine extract prepared in example 2 contains a large amount of compounds such as phytol (13.64%), methyl jasmonate (6.08%), eugenol (5.45%) and terpenes, which have been proved to have good antioxidant activity through a large amount of research and the content thereof is much higher than that of the jasmine extract prepared in comparative example 1.

The extract prepared in example 2 was subjected to a comparative analysis of antioxidant activity test, expressed as the magnitude of the ability to scavenge DPPH and ABTS radicals, with respect to the extract prepared in comparative example 1:

test example 2

The DPPH method: the jasmine flower extracts prepared in example 2 and comparative example 1 are respectively diluted into sample solutions of 0.1, 0.2, 0.4, 1, 2, 5 and 10 mL/mL by ethanol, and 0.1mmol/LDPPH solutions of 50 muL and 150 muL of essential oil are taken and uniformly mixed in a 96 micro-well plate. After 30min at room temperature in the dark, the absorbance A1 at wavelength 517nm was measured. Simultaneously, the absorbance A0 of the mixed DPPH solution and absolute ethyl alcohol is measured, and the inhibition rate of ascorbic acid on DPPH free radicals is measured by the same method by taking 10 mu g/mL ascorbic acid as a positive control. The radical clearance was calculated according to the following formula:

in the formula: a0 is the absorbance of the mixture of DPPH solution and absolute ethyl alcohol; a1 is the absorbance of the mixture of jasmine extract and DPPH solution.

The DPPH radical scavenging ability of various jasmine extracts was evaluated, and the results are shown in FIG. 2. The jasmine extract extracted in comparative example 1 has relatively weak DPPH removing ability, and the radical removing rate is about 95.12% at a perfume concentration of 10%. The jasmine extract prepared in example 2 has strong oxidation resistance, when the concentration is 0.1%, the DPPH free radical removal rate reaches 96.56%,

test example 3

ABTS method: preparing 7mmol/L ABTS solution and 2.6mmol/L K₂S₂O₈And (3) solution. Mixing, storing at room temperature in dark for 12-16h, and diluting until the light absorption value is 0.7 + -0.02. Respectively diluting the jasmine flower extracts prepared in the example 2 and the comparative example 1 into 0.1, 0.2, 0.4, 1, 2, 5 and 10 mL/mL sample solutions by using ethanol, mixing 50 muL of essential oil and 150 muL of ABTS reaction solution, reacting for 30min, measuring the absorbance A1 at the wavelength of 734nm, simultaneously measuring the absorbance A0 after mixing the ABTS solution and absolute ethanol, and measuring the inhibition rate of ascorbic acid on ABTS free radicals by using 50 mug/mL ascorbic acid as a positive control by using the same method. The radical scavenging was calculated according to the following formulaRate:

in the formula:A ₀the absorbance of the ABTS solution mixed with absolute ethyl alcohol;A ₁is the absorbance of the mixture of jasmine extract and ABTS solution.

The results are shown in FIG. 3. Within the range of the assay, the scavenging capacity of free radicals of the same concentration of jasmine extract is: the jasmine extract prepared in example 2 > the jasmine extract prepared in comparative example 1. The ABTS free radical scavenging rate of 96.60% was already achieved when the concentration of jasmine extract prepared in example 1 was 0.1%, whereas the concentration of jasmine extract prepared in comparative example 1 was about 96.08% at a free radical scavenging rate of 5%.

From the above results, it can be seen that both experimental examples 2 and 3 demonstrate that the antioxidant activity of the jasmine extract prepared by the method provided by the present invention is significantly superior to that of the jasmine extract extracted by the conventional petroleum ether method.

Test example 4

The characteristics of the jasmine extracts prepared in examples 1 to 3 and the jasmine extract prepared in comparative example 1 were set as shown in table 2:

TABLE 2 comparison of the traits of jasmine extracts prepared in examples 1-3 and comparative example 1

In terms of characteristics, the jasmine extracts prepared in examples 1 to 3 have good aroma quality, are free of offensive odor, and are closer to natural flower aroma. In contrast, the jasmine extract extracted by hot reflux with petroleum ether of comparative example 1 had solvent residue with a cooking smell. And contains a large amount of wax and pigment, thereby influencing the next use.

Test example 5

The jasmine extract prepared in example 2 was added as a flavor to the flavor of heated cigarettes, and then the flavor change was observed. The results are shown in Table 3.

TABLE 3 deterioration of flavor of heated cigarette to which jasmine flower extract prepared in example 2 was added

As can be seen from Table 3: the shelf life of the perfume prepared in example 2 was only 12 months without addition. After 0.1%, 0.2% and 0.5% of the spices prepared in example 2 are added, the quality guarantee period can be respectively prolonged to 18 months, 24 months and 30 months, which shows that the jasmine flower extract prepared in example 2 can better delay the oxidative deterioration of aroma components in the spices and has the effect of prolonging the quality guarantee period of heated cigarettes.

Sensory evaluation of cigarettes: the jasmine flower extract prepared in the embodiment 2 of the invention is diluted by 1-5 per cigarette core, is injected into the cigarette core of a heated cigarette by adopting an essence and spice injection machine, is placed in a constant temperature and humidity box (the temperature is 22 +/-1 ℃, and the humidity is 60 +/-2%) for balancing for 48 hours, and then is evaluated by an expert with cigarette evaluation qualification. The results show that: the jasmine flower extract disclosed by the invention has the effects of improving the quality of a heated cigarette product, endowing the heated cigarette with a fragrant and elegant style, making smoke thin and soft, enriching the fragrance of the cigarette, reducing the stimulation of the throat, covering miscellaneous gas and improving aftertaste.

The above-described aspects may be implemented individually or in various combinations, and such variations are within the scope of the present invention.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.

The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the specific embodiments of the invention be limited to these descriptions. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

Claims

1. A preparation method of a jasmine flower extract with antioxidant activity is characterized by comprising the following steps:

2. The method of claim 1, wherein the pretreatment in S1 comprises: placing jasmine in 0.5-1% diluted hydrochloric acid, and treating at 20-40 deg.C for 5-10 min.

3. The method for preparing a jasmine extract with antioxidant activity, according to claim 1, wherein the combined enzyme in S2 is a mixture of cellulase, hemicellulase, beta-glucanase and pectinase, and the mass ratio of the cellulase, hemicellulase, beta-glucanase and pectinase is 1:1:1: 1.

4. The method of claim 1, wherein the supercritical extraction conditions in S3 are as follows: the extraction temperature of the carbon dioxide fluid is 30-55 ℃, the pressure is 15-40MPa, and the flow of the carbon dioxide is 3-30L/h; the pressure of the separation kettle is 5.0-10.0MPa, and the separation temperature is 25-40 ℃; the extraction time is 0.5-3 h.

5. The method for preparing a jasmine extract with antioxidant activity according to claim 1, wherein the mass ratio of the filter residue to the ethanol in S3 is 100: (5-15).

6. The method of claim 1, wherein the distillation conditions of the first molecular distillation in S4 are as follows: the pressure in the molecular distiller system is 10-50 Pa, the feeding rate is 2.0mL/min, the rotating speed of a knifing is 300rpm, the distilling temperature is 30-60 ℃, the condensing temperature is 10-25 ℃, and the preheating temperature is 20-50 ℃.

7. The method of claim 1, wherein the distillation conditions of the secondary molecular distillation in S4 are as follows: the distillation pressure is 10-50 Pa, the rotating speed of the knifing is 300rpm, the material flow rate is 2 mL/min, the distillation temperature is 60-80 ℃, the condensation temperature is 10-25 ℃, and the preheating temperature is 50-70 ℃.

8. Use of a jasmine extract with antioxidant activity according to any one of claims 1-7, wherein the jasmine extract is used for addition to a cigarette.

9. The use of jasmine extract with antioxidant activity according to claim 8, wherein jasmine extract is uniformly sprayed in tobacco shreds to make cigarettes.

10. The application of the jasmine extract with the antioxidant activity, as claimed in claim 9, wherein the mass ratio of the jasmine extract to tobacco shreds is (1-5): 1000.