CN113604281B - Preparation method and application of natural spice based on snake skin fruits - Google Patents
Preparation method and application of natural spice based on snake skin fruits Download PDFInfo
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- CN113604281B CN113604281B CN202110930248.8A CN202110930248A CN113604281B CN 113604281 B CN113604281 B CN 113604281B CN 202110930248 A CN202110930248 A CN 202110930248A CN 113604281 B CN113604281 B CN 113604281B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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Abstract
The invention discloses a preparation method and application of a natural spice based on snake skin fruits, and the specific method comprises the following steps: s1, taking and crushing the pericarp of the snake skin fruit; s2, adding the crushed pericarps into deionized water for leaching, and then adding combined enzyme for hydrolysis; s3, adding ethanol into the enzymolysis product obtained in the step S2 for hot extraction, centrifuging to obtain peel residues and extract, and then taking an extract filtering membrane; s4, adsorbing the peel residues by zeolite, then washing the zeolite, and adding the washing liquid into the extracting solution for standby; s5, performing ethanol thermal extraction on the peel residues to obtain secondary extract; and S6, mixing the two extracting solutions obtained in the steps S4 and S5, filtering, and concentrating the clear liquid under reduced pressure at low temperature to obtain the natural spice. The natural spice is added into the tobacco shreds of cigarettes, so that the smoking aroma concentration of the cigarettes is increased, the smoke is rich in the self aroma of the snake skin fruits, and the smoking taste is sour, sweet and refreshing like that of a functional drink, so that great satisfaction is brought to consumers.
Description
Technical Field
The invention relates to the technical field of tobacco flavor production, in particular to a preparation method and application of a natural flavor based on snake skin fruits.
Background
The snake skin fruits are mainly distributed in Asian tropical areas such as India, peninsula in China to Malay, etc., and China is mainly distributed in Western of Yunnan province, south China and partial areas of Choerospondias, and are fruits of Serpentis genus plants of Palmaceae. The snake skin fruit contains protein, fat, pectin, carbohydrate, vitamin Bl, vitamin C, calcium element, potassium element, ferrum element and other nutritional components; has effects of supplementing energy, lowering blood pressure, promoting diuresis, increasing bone density, improving body function, caring skin, and is suitable for people suffering from hunger, hypoglycemia, hypertension, body edema, osteoporosis, calcium deficiency, pachylosis, etc. The main raw material of some functional beverages in the market is snake skin fruits. The beverage mainly comprises the following functional components: taurine, lysine, inositol, nicotinamide, vitamin B6, vitamin B1, white granulated sugar, caffeine, and the like. Therefore, the snake skin fruits are sweet in taste, high in nutritive value and rich in similar nutritive components.
Due to the influence of factors such as fertility degradation, untimely rotation, global climate change and the like of tobacco planting soil in a tobacco region in China, the quality of tobacco leaves cannot meet the requirement of the current cigarette product on fragrance and sweet, and the problem is solved by fragrance compensation and modification technology. Meanwhile, the health of cigarette consumers is increasingly concerned, and the tar content of cigarette products in the global market is gradually reduced for 60 years in the rise of the smoke control surge worldwide, so that the aroma and the concentration of the cigarettes are greatly reduced, and the smoking comfort and the physiological satisfaction of the cigarettes are directly influenced. Especially, the problem of the insufficient flavor of the flue-cured tobacco of the traditional Chinese low-tar cigarettes is particularly remarkable, flavor compensation becomes a technical bottleneck for developing the traditional Chinese low-tar cigarette products, and the development of the flavor with the characteristics of enhancing flavor and preserving moisture and highlighting products becomes one of the important points of the research of the traditional Chinese cigarettes.
Chinese patent [ CN202010977230.9 ] discloses an application of ampelopsis grossedentata leaf extract in flavoring and charging of cigarettes, and the specific process is as follows: selecting Ampelopsis grossedentata She Ganpin, pulverizing, sieving, dissolving, and distilling in water bath to obtain leaching solution; filtering the leaching solution with gauze, vacuum filtering, concentrating the filtrate to obtain Ampelopsis grossedentata leaf extract; adding a solvent into the ampelopsis grossedentata leaf extract according to the volume ratio of 1:1 to obtain a diluent, and adding the diluent into the tobacco shreds in the flavoring and feeding process according to 0.05% -0.5% of the total weight of the tobacco shreds. The method effectively improves the aroma quality and the aroma quantity of the cigarettes by adding the ampelopsis grossedentata leaf extract into the tobacco shreds, enriches the aroma of the cigarettes, ensures that the smoke of the cigarettes is fine and smooth and thoroughly emitted, covers miscellaneous gases, and improves the smoking quality obviously. However, the ampelopsis grossedentata leaf has very small amount of extract, the extraction process is complex and slow, the ampelopsis grossedentata leaf is not suitable for large-scale production, and the nutritional value of the ampelopsis grossedentata leaf is not high.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method and application of a natural spice based on snake skin fruits, which comprises the steps of crushing the dried snake skin fruit peel, carrying out enzymolysis treatment, then carrying out hot extraction twice by using ethanol, squeezing to obtain an extracting solution after extraction, mixing the extracting solutions, filtering, and then taking clear liquid for evaporation and concentration to obtain the natural spice. The natural spice is added into the tobacco shreds of cigarettes, so that the aroma and the smoking taste of the cigarettes can be improved, and the prepared cigarettes can meet the market demands of low-tar cigarettes and special styles and meet the quality requirements of consumers on 'relaxed feeling, comfortable feeling and satisfaction' of cigarette products.
The technical scheme of the invention is as follows: in one aspect, the invention provides a method for preparing a snake skin fruit-based natural spice, comprising the following steps:
s1, taking and crushing the pericarp of the snake skin fruit;
s2, adding 12-16g of the pericarp crushed in the step S1 into 100-150ml of deionized water, leaching for 15-20min, then adding 1-1.5g of combined enzyme, regulating the pH value to be 4.0-5.0, and hydrolyzing in a magnetic stirring oil bath at 40-50 ℃ at a rotating speed of 200r/min to obtain an enzymolysis product;
s3, adding ethanol into the enzymolysis product obtained in the step S2, performing ethanol heat extraction, centrifuging at 3200r/min for 12-14min after extraction to obtain pericarp residues and extract, and then filtering the extract with a 0.45 μm filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, then washing potassium ions on the zeolite, and adding the washing liquid into the filtered extracting solution in the step S3 for standby;
s5, carrying out ethanol heat extraction on the peel residues after adsorption in the S4 again to obtain secondary extract;
and S6, mixing the two extracting solutions obtained in the steps S4 and S5, filtering, and concentrating the clear liquid under reduced pressure at low temperature to obtain the natural spice.
Further, before crushing the peel of the snake skin in the step S1, naturally airing the snake skin in a ventilated and shady place, and then crushing the snake skin to 20-40 meshes.
Further, the combined enzyme in the S2 is a mixture of cellulase, hemicellulase, beta-glucanase, pectinase and serine protease, and the mass ratio of the cellulase, the hemicellulase, the beta-glucanase, the pectinase and the serine protease is 1:1:1:1:2.
Further, the water bath temperature of the ethanol heat extraction is 60-70 ℃, and the mass concentration of the ethanol is 70%.
Further, in the step S3, the ethanol is thermally extracted for 2 hours, and the mass ratio of the pericarp to the ethanol is 1:5, a step of; and in the step S5, the ethanol is subjected to heat extraction for 1h, and the mass ratio of the pericarp to the ethanol is 1:4.
and (3) mixing the two extracting solutions in the step (S6), standing, filtering with 200-mesh and 500-mesh filter cloth in sequence, and concentrating the filtered clear liquid at low temperature under reduced pressure.
Further, the vacuum degree of the low-temperature reduced pressure concentration in the step S6 is 80-120mbar, and the water bath temperature is 60-70 ℃.
In another aspect, the present invention provides the use of a snake fruit based natural flavour, in particular for addition to cigarettes.
Further, the natural perfume is uniformly sprayed into tobacco shreds to prepare cigarettes.
Further, the mass ratio of the natural spice to the tobacco shreds is (1-5): 1000.
the snake skin peel contains rich organic acid, and can be used for caring skin. The snake skin is rich in phospholipids and has brain strengthening effect, and is also called as memory fruit. The snake skin contains fructose, glucose, sucrose, multiple minerals, proteins, carbohydrates, calcium, fat, iron, vitamin B1, vitamin C, and carotene. The pectin and the potassium are at the beginning of fruits, and the content of toxic elements Cd and Pb harmful to human bodies in the snake skin peel is low, and the content of Cd is extremely low, so that the snake skin peel is made into the spice which is added into tobacco shreds, the requirements of cigarette products on 'sweet and fragrant flavor' can be met, and beneficial elements can be brought to human bodies.
Most of the extraction target substances in the snake skin fruits are wrapped in the cell walls, and the traditional cell wall breaking method is low in efficiency and low in extraction efficiency. Serine proteinase not only can hydrolyze peptide bond, but also has the functions of hydrolyzing amide bond, ester bond, transesterification and transpeptidation. Because of the specificity of the enzyme, it can only hydrolyze protein and can not act on starch, fat and other substances. Therefore, the combination of the other four enzymes can not only ensure the protein in the snake skin fruit peel to be hydrolyzed as much as possible, but also promote the precipitation of potassium salt and sodium salt in the snake skin fruit peel.
The invention has the beneficial effects that:
1. the invention provides a preparation method and application of a natural spice based on snake skin fruits. The natural spice is added into the tobacco shreds of cigarettes, the aroma concentration of the cigarettes is increased, the natural tobacco aroma is more, the smoke is rich in the aroma of the snake skin fruits, the smoking taste is as same as that of a functional drink, the taste is sour and sweet, and the consumer is satisfied greatly. The prepared cigarettes can meet the market demands of low-tar cigarettes and special styles, and meet the quality requirements of consumers on 'relaxed feeling, comfortable feeling and satisfaction' of cigarette products.
2. The preparation method of the natural spice based on the snake skin fruits provided by the invention has good solubility, can be directly used for charging or perfuming cigarettes, and is convenient to apply.
3. According to the preparation method of the natural spice based on the snake skin fruits, 70% ethanol is adopted for extracting the snake skin fruit peel, the reaction condition is mild, a catalyst and a toxic organic solvent are not needed in the production process, and the pollution is small. In addition, the invention also carries out secondary ethanol heat extraction on the centrifuged peel residues, which can fully extract substances such as amino acid and the like on the peel and greatly improve the extraction rate of the peel.
4. According to the preparation method of the natural spice based on the snake skin fruits, before ethanol thermal extraction, the centrifuged peel residues are adsorbed by using zeolite, then potassium ions on the zeolite are eluted by using a washing liquid, and the washing liquid is added into supernatant to complete recovery of the potassium ions. The potassium ions have a certain promotion effect on the combustion of tobacco, so that the natural perfume prepared by the invention can promote the full combustion of tobacco and ensure the full diffusion of the fragrance on the heated tobacco shreds.
5. According to the preparation method of the natural spice based on the snake skin fruits, provided by the invention, the peel of the snake skin fruits is used as the natural spice, the proportion of sugar and protein in tobacco leaves can be adjusted, the natural spice is a good acid sweetener and a humectant, the natural spice is easy to combine with the tobacco, the contained flavor components are pyrolyzed and converted into flavor substances beneficial to cigarettes, the smoking taste is improved, and the natural spice can be applied to feeding and surface-aroma essence.
6. The preparation method of the natural spice based on the snake skin fruits provided by the invention has the advantages that the peel raw materials of the snake skin fruits are easy to obtain, the economic value and the utilization efficiency of the fruits are improved, the income channel is widened for fruit farmers, and meanwhile, the waste is changed into valuable for fruit processing and related enterprises, so that the treatment problem of the snake skin peel can be effectively solved.
7. The preparation method of the natural spice based on the snake skin fruits has the advantages of simple and easily controlled production process, low process cost, easy popularization and application, no change of the original performance of cigarettes, no change of the original processing process of the cigarettes, and extremely high economic benefit.
Drawings
Fig. 1 is a flowchart of a method for preparing a natural spice based on snake skin fruits according to an embodiment of the invention.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the following description will explain specific embodiments of the present invention with reference to the accompanying drawings.
It is obvious that the drawings in the following description are only examples of the invention, from which other drawings can be obtained and from which other embodiments can be obtained without inventive effort for a person skilled in the art, and that the invention is not limited to these examples.
In the embodiment of the invention, the combined enzyme is a mixture of cellulase, hemicellulase, beta-glucanase, pectinase and serine protease, wherein the mass ratio of the cellulase to the hemicellulase to the beta-glucanase to the pectinase to the serine protease is 1:1:1:1:2.
The specific embodiment of the invention is as follows:
example 1
A preparation method of a natural spice based on snake skin fruits comprises the following specific steps:
s1, naturally airing the snake skin fruit peel in a ventilated and cool place, taking 150g of the aired snake skin fruit peel, and crushing the snake skin peel into 20 meshes;
s2, adding 12g of the pericarp crushed in the step S1 into 100ml of deionized water, leaching for 15min, then adding 1g of combined enzyme, adding acetic acid to adjust the pH value to 4.0, and hydrolyzing in a magnetic stirring oil bath at 40 ℃ at a rotating speed of 200r/min to obtain an enzymolysis product;
s3, adding 70% ethanol into the enzymolysis product obtained in the step S2, performing hot extraction for 2 hours, wherein the water bath temperature is 60 ℃, the solid-liquid mass ratio of the hot ethanol extraction is 1:5, centrifuging at 3200r/min for 12min after extraction to obtain peel residues and extract, and then filtering the extract with a 0.45 mu m filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, washing potassium ions on the zeolite by deionized water, and adding the washing liquid into the extracting solution obtained after filtering the membrane in the step S3 for later use;
s5, adding 70% ethanol into the peel residue adsorbed in the step S4, and performing hot extraction for 1h at a water bath temperature of 60 ℃ to obtain a secondary extract for later use, wherein the mass ratio of the ethanol to the solid-liquid is 1:4;
s6, mixing the two extracting solutions obtained in the steps S4 and S5, standing for 1h, sequentially filtering with 200-mesh and 500-mesh filter cloth for two times, collecting clear liquid, and concentrating under reduced pressure at a water bath temperature of 60 ℃ under a vacuum degree of 80mbar to obtain natural perfume with a yield of 20.5%.
Example 2
A preparation method of a natural spice based on snake skin fruits comprises the following specific steps:
s1, naturally airing the snake skin fruit peel in a ventilated and cool place, taking 150g of the aired snake skin fruit peel, and crushing the snake skin peel into 20 meshes;
s2, adding 14g of the pericarp crushed in the step S1 into 120ml of deionized water, leaching for 18min, then adding 1.3g of combined enzyme, adding acetic acid to adjust the PH value to 4.0, and hydrolyzing in a magnetic stirring oil bath at 45 ℃ at a rotating speed of 200r/min to obtain an enzymolysis product;
s3, adding 70% ethanol into the enzymolysis product obtained in the step S2, performing hot extraction for 2 hours, wherein the water bath temperature is 60 ℃, the solid-liquid mass ratio of the hot ethanol extraction is 1:5, centrifuging at 3200r/min for 13min after extraction to obtain peel residues and extract, and then filtering the extract with a 0.45 mu m filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, washing potassium ions on the zeolite by deionized water, and adding the washing liquid into the extracting solution obtained after filtering the membrane in the step S3 for later use;
s5, adding 70% ethanol into the peel residue adsorbed in the step S4, and performing hot extraction for 1h at a water bath temperature of 60 ℃ to obtain a secondary extract for later use, wherein the mass ratio of the ethanol to the solid-liquid is 1:4;
s6, mixing the two extracting solutions obtained in the steps S4 and S5, standing for 1h, sequentially adopting 200-mesh filter cloth and 500-mesh filter cloth to carry out twice filter cloth filtration, taking clear liquid, and carrying out low-temperature reduced-pressure concentration at the water bath temperature of 65 ℃ under the vacuum degree of 100mbar to obtain the natural spice, wherein the yield is 20.7%.
Example 3
A preparation method of a natural spice based on snake skin fruits comprises the following specific steps:
s1, naturally airing the snake skin fruit peel in a ventilated and cool place, taking 150g of the aired snake skin fruit peel, and crushing the snake skin peel into 20 meshes;
s2, adding 16g of the pericarp crushed in the step S1 into 150ml of deionized water, leaching for 20min, then adding 1.5g of combined enzyme, adding acetic acid to adjust the pH value to 5.0, and hydrolyzing in a magnetic stirring oil bath at 50 ℃ at a rotating speed of 200r/min to obtain an enzymolysis product;
s3, adding 70% ethanol into the enzymolysis product obtained in the step S2, performing hot extraction for 2 hours, wherein the water bath temperature is 60 ℃, the solid-liquid mass ratio of the hot ethanol extraction is 1:5, centrifuging at 3200r/min for 14min after extraction to obtain peel residues and extract, and then filtering the extract with a 0.45 mu m filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, washing potassium ions on the zeolite by deionized water, and adding the washing liquid into the extracting solution obtained after filtering the membrane in the step S3 for later use;
s5, adding 70% ethanol into the peel residue adsorbed in the step S4, and performing hot extraction for 1h at a water bath temperature of 60 ℃ to obtain a secondary extract for later use, wherein the mass ratio of the ethanol to the solid-liquid is 1:4;
s6, mixing the two extracting solutions obtained in the steps S4 and S5, standing for 1h, sequentially adopting 200-mesh filter cloth and 500-mesh filter cloth to carry out twice filter cloth filtration, taking clear liquid, and carrying out low-temperature reduced-pressure concentration at the water bath temperature of 70 ℃ under the vacuum degree of 120mbar to obtain the natural spice, wherein the yield is 21.9%.
Comparative example 1
The snake skin pulp is used as a raw material to replace peel, and the natural spice is prepared by evaporating and concentrating.
A preparation method of a natural spice based on snake skin fruits comprises the following specific steps:
s1, removing the cores of 34kg of snake skin fruits, squeezing, filtering with 200-mesh filter cloth to obtain primary filtrate, standing and settling for 10h, and filtering with 200-mesh filter cloth and 500-mesh filter cloth to obtain clear fresh snake skin juice raw juice with 18% of solid content, wherein the juice yield is 39%;
s2, taking 1.2kg of the clear fresh snake skin juice stock solution prepared in the step S1, placing the clear fresh snake skin juice stock solution in a rotary evaporator at a water bath temperature of 70 ℃ under a vacuum degree of 100mbar, and evaporating and concentrating until the solid content of the extract is 41.7%, thus obtaining the natural spice.
Comparative example 2
The snake skin pulp is used as a raw material to replace peel to prepare natural spice through forward osmosis concentration.
A preparation method of a natural spice based on snake skin fruits comprises the following specific steps:
s1, removing the cores of 34kg of snake skin fruits, squeezing, filtering with 200-mesh filter cloth to obtain primary filtrate, standing and settling for 10 hours, and filtering with 200-mesh filter cloth and 500-mesh filter cloth to obtain clear fresh snake skin juice raw juice with 18% of solid content, wherein the juice yield is 39%;
s2, taking 4.4kg of the clear fresh snake skin juice stock solution prepared in the step S1, placing the clear fresh snake skin juice stock solution in a concentration chamber of a forward osmosis concentration device, taking a aquaporin hollow fiber forward osmosis membrane as a separation membrane, taking saturated NaCl solution as a drawing agent, and carrying out multistage concentration at room temperature, wherein the flow rates of the clear snake skin juice stock solution and the drawing solution are controlled to be 0.7L/min. And (3) carrying out primary concentration by using 1L of saturated NaCl solution as a drawing agent, when the drawing agent loses the drawing capability, replacing the saturated NaCl solution with the same amount as the drawing agent for secondary concentration, and similarly replacing the drawing liquid until the solid content of the snake skin fruit extract is 41.8%, thereby obtaining the natural spice.
Comparative example 3
The snake skin pomace is used as a raw material to replace pericarp to prepare natural spice.
S1, taking 4kg of pomace of fresh snake skin fruits, and soaking the pomace for 12 hours by using 95% ethanol, wherein the mass ratio of the ethanol to the pomace is 1:1, filtering with 200 mesh filter cloth, filtering with absorbent cotton to obtain extractive solution, placing the extractive solution in a rotary evaporator at 70deg.C under vacuum degree of 100mbar, evaporating and concentrating to obtain fruit residue ethanol extract with 77% yield.
Comparative example 4
The ethanol with the mass concentration of 70% is replaced by ethanol with the mass concentration of 95% for heat extraction.
A preparation method of a natural spice based on snake skin fruits comprises the following specific steps:
s1, naturally airing the snake skin fruit peel in a ventilated and cool place, taking 150g of the aired snake skin fruit peel, and crushing the snake skin peel into 20 meshes;
s2, adding 12g of the pericarp crushed in the step S1 into 100ml of deionized water, leaching for 15min, then adding 1g of combined enzyme, adding acetic acid to adjust the pH value to 4.0, and hydrolyzing in a magnetic stirring oil bath at 40 ℃ at a rotating speed of 200r/min to obtain an enzymolysis product;
s3, adding ethanol with the mass concentration of 95% into the enzymolysis product obtained in the step S2, performing hot extraction for 2 hours, wherein the water bath temperature is 60 ℃, the mass ratio of the ethanol to the solid and the liquid is 1:5, centrifuging at 3200r/min for 12min after extraction to obtain peel residues and extract, and then taking the extract to pass through a 0.45 mu m filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, washing potassium ions on the zeolite by deionized water, and adding the washing liquid into the extracting solution obtained after filtering the membrane in the step S3 for later use;
s5, adding 95% ethanol into the peel residue adsorbed in the step S4, and performing hot extraction for 1h at a water bath temperature of 60 ℃ to obtain a secondary extract for later use, wherein the mass ratio of the ethanol to the solid-liquid is 1:4;
s6, mixing the two extracting solutions obtained in the steps S4 and S5, standing for 1h, sequentially filtering with 200-mesh and 500-mesh filter cloth for two times, collecting clear liquid, and concentrating under reduced pressure at a water bath temperature of 60 ℃ under a vacuum degree of 80mbar to obtain natural perfume with a yield of 20%.
Comparative example 5
Without pretreatment with combined enzymes
A preparation method of a natural spice based on snake skin fruits comprises the following specific steps:
s1, naturally airing the snake skin fruit peel in a ventilated and cool place, taking 150g of the aired snake skin fruit peel, and crushing the snake skin peel into 20 meshes;
s2, adding 70% ethanol into the crushed product obtained in the step S1, performing hot extraction for 2 hours, wherein the water bath temperature is 60 ℃, the solid-liquid mass ratio of the hot ethanol extraction is 1:5, centrifuging at 3200r/min for 12min after extraction to obtain peel residues and extract, and then filtering the extract with a 0.45 mu m filter membrane;
s3, adsorbing the peel residues in the step S2 by zeolite, washing potassium ions on the zeolite by deionized water, and adding the washing liquid into the extracting solution obtained after filtering the membrane in the step S2 for later use;
s4, adding 70% ethanol into the peel residue adsorbed in the step S3, and performing hot extraction for 1h at a water bath temperature of 60 ℃ to obtain a secondary extract for later use, wherein the mass ratio of the ethanol to the solid-liquid is 1:4;
s5, mixing the two extracting solutions obtained in the steps S3 and S4, standing for 1h, sequentially filtering with 200-mesh and 500-mesh filter cloth for two times, collecting clear liquid, and concentrating under reduced pressure at a water bath temperature of 60 ℃ under a vacuum degree of 80mbar to obtain natural perfume with a yield of 20%.
The natural flavors prepared in examples 1 to 3 and comparative examples 1 to 5 were added to the respective corresponding tobacco shreds, respectively, to prepare cigarettes, and then the seven cigarettes were subjected to sensory evaluation for smoking and preliminary judgment, and the results are shown in table 1.
TABLE 1 suction evaluation results of natural flavors prepared in examples 1-3 and comparative examples 1-5 added to tobacco shreds
As can be seen from the results of table 1, the natural perfume prepared in comparative example 2 was added to tobacco shreds, and the sucked sweet taste was the most intense, indicating that forward osmosis concentration can retain the fragrance substance of snake skin fruits to the greatest extent, but the fragrance of comparative example 2 was single, the smoke fragrance was slightly narrow, and the irritation was slightly small, indicating that the natural perfume prepared in comparative example 2 was not suitable as a fragrance substance of tobacco shreds.
The natural perfume prepared in comparative example 4 was added to tobacco shred, and the feeling of smoking was clear and improved, the sour and sweet fruit charm, the sour and sweet taste were little, the smoothness of smoke was improved, and there was a moist feeling, but the aroma concentration was reduced, the aroma amount was reduced, the aroma was submerged, there was still oily smell, the smoke was soft and astringent, there was a granular feeling, the swallowing was uncomfortable, and there was a coating feeling.
The natural perfume prepared in the examples 1-3 is added into tobacco shred, the aroma concentration is increased, the natural tobacco aroma is more, the smoke is rich in the aroma of the snake skin fruit, the sucking taste is as same as that of the drinking functional beverage, the taste is sour and sweet, and the great satisfaction is brought to consumers. The method is characterized in that the snake skin is selected as a raw material, 70% ethanol is adopted for extraction, and the natural spice prepared by evaporation concentration is most suitable to be used as a flavoring substance of tobacco shreds.
The natural perfume prepared in comparative example 5 is added into tobacco shreds, the aroma concentration is reduced, the richness of sour and sweet fruits is poor, which indicates that the extraction rate of peel without enzyme treatment is poor, the separated amino acid is less, the pumped aroma concentration is reduced, and the richness of sour and sweet fruits is poor.
Detection of aroma components
The natural flavors prepared in example 1 and comparative examples 1 to 3 were subjected to aroma-generating component detection, and each sample was numbered with the juice raw juice of fresh snake skin fruit as a blank, and the specific numbers are shown in table 2.
TABLE 2 sample names and numbers for fragrance-generating ingredient detection
| Sample numbering | Sample name | Sample number of sample feeding |
| Example 1 | Extracting fresh snake skin peel with 70% ethanol, evaporating, concentrating | spg1 |
| Comparative example 2 | Forward concentration of fresh snake skin fruit juice | spg2 |
| Comparative example 1 | Evaporating and concentrating the juice of fresh snake skin fruit | spg3 |
| Blank control | Juice stock of fresh snake skin fruit | spg4 |
| Comparative example 3 | Extracting residues of fresh fructus Serpentis with 95% ethanol, evaporating, concentrating | spg5 |
| Comparative example 5 | Extracting fresh snake skin peel with 70% ethanol, evaporating, concentrating without enzyme treatment | Spg6 |
The results of the detection of the content of the aroma components of the natural perfume prepared in example 1 are shown in table 3.
Table 3-spg sample prepared aroma component content of Natural fragrance
The results of the detection of the content of the aroma components of the natural perfume prepared in comparative example 2 are shown in table 4.
Table 4-spg sample preparation of aroma component content of Natural fragrance
The results of the detection of the content of the aroma components of the natural perfume prepared in comparative example 1 are shown in table 5.
Table 5-spg sample preparation of aroma component content of Natural fragrance
The detection results of the aroma component content of the natural perfume prepared by taking the juice raw juice of the fresh snake skin fruits as a blank control are shown in table 6.
Table 6-spg sample preparation of aroma component content of Natural fragrance
The results of the detection of the content of the aroma components of the natural perfume prepared in comparative example 3 are shown in table 7.
Table 7-spg sample preparation of aroma component content of Natural fragrance
The results of the detection of the content of the aroma components of the natural perfume prepared in comparative example 5 are shown in table 8.
Table 8-spg sample prepared aroma component content of Natural aroma
As can be seen from tables 3 to 8, the types of the aroma-generating components of spg, spg2, spg3, spg4, spg5 and spg6 are: 22. 11, 10, 11, 25 and 18, wherein the juice of the fresh snake skin fruits has 11 aroma-causing component types in spg and only 10 aroma-causing component types in spg, and the aroma-causing components are destroyed by evaporation concentration of the juice after the juice of the fresh snake skin fruits is squeezed, the types and the total amount are less than those of a control (raw juice), and the juice of the fresh snake skin fruits is not suitable for being used as a raw material of natural perfume; spg6 has less than spg 1.1 aroma components and less content, and is characterized by poor purification rate of snake skin and peel due to no addition of combined enzyme; while spg and spg have significantly more aroma types than spg2, spg3 and spg4, it is demonstrated that the natural flavors prepared using ethanol to extract the peel of fresh snake skin contain more aroma components than the natural flavors prepared using fresh snake skin juice. The comprehensive sensory evaluation absorbs the aroma components of the peel, the fruit juice and the pomace, the aroma components of the peel are more in variety and content, and the sensory quality is better.
The content of amino acid and organic acid in the natural perfume of spg-spg is detected, and the detection results are shown in Table 8.
Table 8-spg 1-spg 6 results of detection of amino acid and organic acid content of natural perfume prepared from sample
| Sequence number | Inspection item | Unit (B) | spg1 | Spg2 | Spg3 | Spg4 | Spg5 | Spg6 |
| 1 | Amino acid content | % | 0.12 | 0.043 | 0.042 | 0.025 | 0.094 | 0.10 |
| 2 | Aspartic acid | % | 0.01 | 0.015 | 0.014 | 0.011 | 0.023 | 0.01 |
| 3 | Glutamic acid | % | 0.013 | 0.0056 | 0.004 | Go undetected (definite) Limit of amount: 0.001) | 0.018 | 0.005 |
| 4 | Serine (serine) | % | 0.037 | 0.0077 | 0.008 | 0.0052 | 0.017 | 0.018 |
| 5 | Histidine | % | Go undetected (definite) Limit of amount: 0.002) | Go undetected (definite) Limit of amount: 0.002) | Go undetected (definite) Limit of amount: 0.002) | Go undetected (definite) Limit of amount: 0.002) | Go undetected (definite) Limit of amount: 0.002) | Not detected (quantitative) Limit: 0.002) |
| 6 | Glycine (Gly) | % | 0.0045 | 0.0044 | 0.0044 | 0.0028 | 0.010 | 0.0045 |
| 7 | Threonine (Thr) | % | Go undetected (definite) Limit of amount: 0.001) | Go undetected (definite) Limit of amount: 0.001) | Go undetected (definite) Limit of amount: 0.001) | Go undetected (definite) Limit of amount: 0.001) | Go undetected (definite) Limit of amount: 0.001) | Not detected (quantitative) Limit: 0.001) |
| 8 | Arginine (Arg) | % | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Not detected (quantitative) Limit: 0.010) |
| 9 | Alanine (Ala) | % | 0.049 | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | 0.021 |
| 10 | Tyrosine | % | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Not detected (quantitative) Limit: 0.010) |
| 11 | Valine (valine) | % | Go undetected (definite) Limit of amount: 0.001) | Go undetected (definite) Limit of amount: 0.001) | Go undetected (definite) Limit of amount: 0.001) | Go undetected (definite) Limit of amount: 0.001) | Go undetected (definite) Limit of amount: 0.001) | Not detected (quantitative) Limit: 0.001) |
| 12 | Isoleucine (Ile) | % | 0.0072 | 0.0089 | 0.0094 | 0.0052 | 0.022 | 0.0072 |
| 13 | Phenylalanine (Phe) | % | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Not detected (quantitative) Limit: 0.010) |
| 14 | Lysine | % | 0.0024 | 0.0012 | 0.0018 | 0.0011 | 0.0039 | 0.0024 |
| 15 | Leucine (leucine) | % | Go undetected (definite) Limit of amount: 0.005) | Go undetected (definite) Limit of amount: 0.005) | Go undetected (definite) Limit of amount: 0.005) | Go undetected (definite) Limit of amount: 0.005) | Go undetected (definite) Limit of amount: 0.005) | Not detected (quantitative) Limit: 0.005) |
| 16 | Proline (proline) | % | Not detected(determination of Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Not detected (quantitative) Limit: 0.010) |
| 17 | Methionine | % | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Go undetected (definite) Limit of amount: 0.010) | Not detected (quantitative) Limit: 0.010) |
| Total amount of amino acids | % | 0.2431 | 0.0563 | 0.0858 | 0.0836 | 0.0503 | 0.1562 | |
| 18 | Citric acid | g/kg | 2.8 | 1.3 | 1.5 | 0.51 | 3.3 | 1.5 |
| 19 | Malic acid | g/kg | 13 | 5.8 | 5.0 | 2.2 | 11 | 10 |
| Total amount of organic acids | g/kg | 15.8 | 7.1 | 6.5 | 2.71 | 14.3 | 10.34 |
As can be seen from Table 8, the total amino acid content of the spg (fresh snake skin peel, 70% ethanol extract, heat extraction, evaporation and concentration) sample is highest, and the variety is also higher, which is consistent with the sensory quality results, which shows that the 70% ethanol extract peel, heat extraction, evaporation and concentration sample is richer in sensory quality, especially taste characteristics.
From the aspect of the total organic acid, spg (pericarp of fresh snake skin fruit, 70% ethanol extract, heat extraction, evaporation and concentration) samples have the highest total organic acid, and specifically comprise citric acid and malic acid. The citric acid can be used as a pH regulator, so that the tobacco leaf seasoning effect can be achieved, and the quality of tobacco leaves can be maintained. The citric acid has the characteristics of chelating and regulating pH value, so that the performance of the antioxidant can be improved in the processing process, and the shelf life is prolonged. Compared with citric acid, malic acid has high acidity (20% stronger than citric acid), but soft taste (higher buffer index), has special flavor, does not damage the oral cavity and teeth, is favorable for amino acid absorption in metabolism, does not accumulate fat, and has extremely high economic benefit when being added into cigarette tobacco shreds.
And combining with the sensory quality result, the 70% ethanol extract peel is illustrated, the thermal extraction evaporation concentration sample has more obvious sour feel on the sensory quality, especially on the aspect of taste characteristics, and the sour and sweet feel is better, so that the point can be further illustrated.
The above description may be implemented alone or in various combinations and these modifications are within the scope of the present invention.
It is noted that relational terms such as first and second, and the like are 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. Moreover, 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 one …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises an element.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific examples described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (8)
1. The preparation method of the natural spice based on the snake skin fruits is characterized by comprising the following steps of:
s1, taking and crushing the pericarp of the snake skin fruit;
s2, adding 12-16g of the pericarp crushed in the step S1 into 100-150ml of deionized water, leaching for 15-20min, then adding 1-1.5g of combined enzyme, regulating the pH value to be 4.0-5.0, and hydrolyzing in a magnetic stirring oil bath at the temperature of 40-50 ℃ at the speed of 200r/min to obtain an enzymolysis product;
s3, adding ethanol into the enzymolysis product obtained in the step S2, performing ethanol heat extraction, centrifuging at 3200r/min for 12-14min after extraction to obtain pericarp residues and extract, and then filtering the extract with a 0.45 μm filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, then washing potassium ions on the zeolite, and adding the washing liquid into the filtered extracting solution in the step S3 for standby;
s5, carrying out ethanol heat extraction on the peel residues after adsorption in the S4 again to obtain secondary extract;
s6, mixing the two extracting solutions obtained in the steps S4 and S5, filtering, and concentrating the clear liquid at low temperature under reduced pressure to obtain natural perfume;
the combined enzyme in the S2 is a mixture of cellulase, hemicellulase, beta-glucanase, pectinase and serine protease, and the mass ratio of the cellulase to the hemicellulase to the beta-glucanase to the pectinase to the serine protease is 1:1:1:1:2;
the water bath temperature of the ethanol heat extraction is 60-70 ℃, and the mass concentration of the ethanol is 70%.
2. The method for preparing a natural spice based on snake skin fruits as claimed in claim 1, wherein the peel of the snake skin fruits in S1 is naturally dried in the shade before being crushed, and then crushed to 20-40 mesh.
3. The method for preparing the natural spice based on the snake skin fruits according to claim 1, wherein the ethanol is extracted for 2 hours in the step S3, and the mass ratio of the pericarp to the ethanol is 1:5, a step of; and in the step S5, the ethanol is subjected to heat extraction for 1h, and the mass ratio of the pericarp to the ethanol is 1:4.
4. the method for preparing the natural spice based on the snake skin fruits, which is characterized in that in the step S6, after mixing the two extracting solutions, standing, filtering with 200-mesh and 500-mesh filter cloth in sequence, and concentrating the filtered clear liquid at low temperature and under reduced pressure.
5. The method for preparing a natural spice based on snake skin fruits as claimed in claim 1, wherein the vacuum degree of the low-temperature reduced-pressure concentration in the step S6 is 80-120mbar, and the water bath temperature is 60-70 ℃.
6. Use of a natural snake fruit based flavour as claimed in any of claims 1 to 5 for addition to cigarettes.
7. The use of a natural spice based on snake skin fruits as claimed in claim 6, wherein the natural spice is uniformly sprayed into tobacco shreds to make cigarettes.
8. Use of a natural spice based on snake skin fruits according to claim 7, characterized in that the mass ratio of natural spice to tobacco shreds is (1-5): 1000.
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