CN113604281A - 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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- CN113604281A CN113604281A CN202110930248.8A CN202110930248A CN113604281A CN 113604281 A CN113604281 A CN 113604281A CN 202110930248 A CN202110930248 A CN 202110930248A CN 113604281 A CN113604281 A CN 113604281A
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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 Chinese wampee fruit, and the specific method comprises the following steps: s1, taking and crushing the peel of the snake skin fruit; s2, adding the crushed pericarp into deionized water for leaching, and then adding the combined enzyme for hydrolysis; s3, adding ethanol into the enzymolysis product in the step S2 for hot extraction, centrifuging to obtain peel residues and an extracting solution, and then taking the extracting solution for filtering by a membrane; s4, adsorbing the peel residues by zeolite, washing the zeolite, and adding a washing solution into the extracting solution for later use; s5, carrying out hot extraction on the peel residues with ethanol to obtain a secondary extracting solution; s6, mixing the two extractive solutions obtained in S4 and S5, filtering, and concentrating the clear solution at low temperature under reduced pressure to obtain natural perfume. The natural spice is added into the tobacco shreds of the cigarettes, so that the smoking aroma concentration of the cigarettes is increased, the smoke is rich in the fragrance of the ophidian, the smoking taste is sour, sweet and tasty like drinking functional beverages, and great satisfaction is brought to consumers.
Description
Technical Field
The invention relates to the technical field of production of tobacco flavors, in particular to a preparation method and application of a natural flavor based on Chinese artichoke fruit.
Background
The snakeskin fruit is mainly distributed in tropical regions of Asia such as India, Hemicentra of Central China to Mali Islands, etc., and China is mainly distributed in western regions, south China and partial regions of Chongqing in Yunnan province, and is the fruit of the snakeskin fruit of the plant of the genus Serpentis of the family Palmaceae. The snake skin fruit contains protein, fat, pectin, carbohydrate, vitamin Bl, vitamin C, calcium element, potassium element, iron element and other nutrient components; has effects of supplementing energy, lowering blood pressure, promoting diuresis, increasing bone density, improving body function, caring skin, and is suitable for people with hunger, hypoglycemia, hypertension, edema, osteoporosis, calcium deficiency, pachylosis, etc. The main raw material of some functional beverages on the market is the snake skin fruit. The functional components contained in the beverage mainly comprise: taurine, lysine, inositol, nicotinamide, vitamin B6, vitamin B1, white granulated sugar, caffeine and the like. Therefore, the snake skin fruit not only has sweet taste, but also has higher nutritional value, and the peel of the snake skin fruit also contains similar rich nutritional ingredients.
Due to the influences of factors such as deterioration of the fertility of tobacco planting soil in tobacco areas in China, untimely crop rotation, global climate change and the like, the quality of tobacco leaves cannot meet the requirement of the current cigarette products on 'fragrance and sweetness', and the problem needs to be solved through a fragrance compensation and modification technology. Meanwhile, the cigarette consumers pay more and more attention to health and control the rise of smoke wave in the world, the tar content of cigarette products in the global market is gradually reduced for 60 years, so that the cigarette fragrance amount and concentration are greatly reduced, and the smoking comfort and physiological satisfaction of the cigarettes are directly influenced. Particularly, the problem of insufficient flavor of the flue-cured tobacco of the Chinese style low-tar cigarette is particularly prominent, flavor compensation becomes a technical bottleneck of the development of Chinese style low-tar cigarette products, and the development of flavors with flavor enhancement, moisture retention and outstanding product characteristics becomes one of the key points of Chinese style cigarette research.
Chinese patent (CN 202010977230.9) discloses an application of Ampelopsis grossedentata leaf extract in flavoring and casing of cigarettes, which comprises the following specific processes: selecting dry Ampelopsis grossedentata leaves, crushing, sieving, dissolving, and distilling in water bath to obtain extract; filtering the leaching solution with gauze, vacuum filtering, and 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 cut tobacco in the flavoring and feeding processes according to 0.05-0.5% of the total weight of the cut tobacco. The method effectively improves cigarette aroma quality and quantity, enriches cigarette aroma, and improves cigarette smoke fineness, covers off miscellaneous gas, and improves smoking quality. However, the amount of the extract of the Ampelopsis grossedentata leaves is very small, the extraction process is complex and slow, the method is not suitable for large-scale production, and the nutritive value of the Ampelopsis grossedentata is not as high as that of the fruits of the snake skin.
Disclosure of Invention
The invention provides a preparation method of natural spice based on snake skin fruit and application thereof, which comprises the steps of crushing peel of dried snake skin fruit, carrying out enzymolysis treatment, then carrying out heat extraction twice by using ethanol, squeezing to obtain extracting solution after extraction, mixing the extracting solutions obtained in the two steps, filtering, and then taking clear liquid for evaporation and concentration to obtain the natural spice. The natural spice is added into the cigarette tobacco shreds, so that the aroma and the smoking taste of the cigarettes can be improved, the prepared cigarettes can meet the market demands of low-tar cigarettes and special styles, and the quality demands of consumers on the relaxation, comfort and satisfaction of cigarette products are met.
The technical scheme of the invention is as follows: in one aspect, the invention provides a preparation method of a natural spice based on the Chinese wampee fruit, which comprises the following steps:
s1, taking and crushing the peel of the snake skin fruit;
s2, adding 12-16g of crushed peel of the S1 into 150ml of deionized water, leaching for 15-20min, adding 1-1.5g of combined enzyme, adjusting the pH value to 4.0-5.0, and hydrolyzing in a magnetic stirring oil bath kettle at 40-50 ℃ at the rotating speed of 200r/min to obtain an enzymolysis product;
s3, adding ethanol into the enzymolysis product in the S2, carrying out ethanol heat extraction, centrifuging for 12-14min at 3200r/min after extraction to obtain pericarp residues and an extracting solution, and then filtering the extracting solution through a 0.45-micrometer filter membrane;
s4, adsorbing the pericarp residues in the S3 by zeolite, washing potassium ions on the zeolite, and adding a washing solution into the filtered extracting solution in the S3 for later use;
s5, carrying out hot extraction on the pericarp residues adsorbed in the step S4 with ethanol again to obtain a secondary extracting solution;
s6, mixing the two extractive solutions obtained in S4 and S5, filtering, and concentrating the clear solution at low temperature under reduced pressure to obtain natural perfume.
Further, before being crushed, the pericarp of the snake skin fruit in the S1 is naturally dried in a ventilated and cool place, and then is crushed into 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: 2.
Further, the temperature of the water bath for hot extraction of the ethanol is 60-70 ℃, and the mass concentration of the ethanol is 70%.
Further, in the step S3, the ethanol is subjected to heat extraction for 2 hours, and the mass ratio of the pericarp to the ethanol is 1: 5; and in the S5, the ethanol is subjected to heat extraction for 1h, and the mass ratio of the pericarp to the ethanol is 1: 4.
further, in the step S6, the two extraction solutions are mixed, and then allowed to stand, and are sequentially filtered through 200-mesh and 500-mesh filter cloth, and the filtered clear solution is subjected to low-temperature reduced-pressure concentration.
Further, the vacuum degree of low-temperature reduced pressure concentration in the S6 is 80-120mbar, and the water bath temperature is 60-70 ℃.
In another aspect, the invention provides the use of a natural flavour based on fruit of snake skin, in particular for adding to cigarettes.
Further, the natural spice is uniformly sprayed into tobacco shreds to prepare the cigarette.
Further, the mass ratio of the natural spice to the cut tobacco is (1-5): 1000.
the pericarp of the snake skin fruit contains rich organic acid, and can be used for caring skin. The pericarp of the fruit of the snake skin is rich in phospholipid and has the function of strengthening the brain, and is also called as a memory fruit. The pericarp of the snake skin fruit contains fructose, glucose, sucrose, various minerals, proteins, carbohydrates, calcium, fat, iron, vitamin B1, vitamin C, carotene, etc. The pectin and the potassium are the first of fruits, and the toxic elements Cd and Pb which are harmful to human bodies in the snake skin peel are low, wherein the content of Cd is extremely low, so that the snake skin peel is prepared into spice to be added into tobacco shreds, the requirements of cigarette products on fragrance and sweetness can be met, and beneficial elements can be brought to human bodies.
The method has the advantages that the cellulase, the hemicellulase, the beta-glucanase and the pectinase are added, so that the cell wall damage rate can be obviously improved, the extracted target substance is more fully released, and the extraction rate is improved. The serine protease can hydrolyze peptide bonds, and also has the functions of hydrolyzing amide bonds, ester bonds, transesterification and transpeptidation. Because of the specificity of the enzyme, the enzyme can only hydrolyze protein and can not act on substances such as starch, fat and the like. Therefore, the combination of the simultaneous action of other four enzymes can not only ensure that the protein in the snake skin pericarp is hydrolyzed as much as possible, but also promote the separation of potassium salt and sodium salt in the snake skin pericarp.
The invention has the beneficial effects that:
1. the invention provides a preparation method and application of natural spice based on snake skin fruit. The natural spice is added into the tobacco shreds of cigarettes, the aroma concentration of the cigarettes is increased, the natural cigarette fragrance is more, the smoke is rich in the fragrance of the Chinese wampee, the smoking taste is as the drinking of functional beverages, the mouth feel is sour, sweet and tasty, and great satisfaction is brought to consumers. The prepared cigarette can meet the market demands of low-tar cigarettes and special styles, and meets the quality demands of consumers on the cigarette products of relaxed feeling, comfortable feeling and satisfaction.
2. The natural spice prepared by the invention has good solubility, can be directly used for feeding or perfuming cigarettes, and is convenient to apply.
3. According to the preparation method of the natural spice based on the snake skin fruit, which is provided by the invention, the snake skin fruit peel is extracted by adopting 70% ethanol, the reaction condition is mild, no catalyst or toxic organic solvent is needed in the production process, and the pollution is small. In addition, the method also carries out secondary ethanol heat extraction on the centrifuged pericarp residues, can fully extract substances such as amino acid and the like on the pericarp, and greatly improves the extraction rate of the pericarp.
4. According to the preparation method of the natural spice based on the snake skin fruit, provided by the invention, before ethanol heat extraction, centrifuged peel residues are adsorbed by zeolite, then potassium ions on the zeolite are eluted by washing liquid, and the washing liquid is added into a supernatant to complete the recovery of the potassium ions. The potassium ions have certain promotion effect on the combustion of the tobacco, so that the natural spice prepared by the invention can promote the sufficient combustion of the tobacco and can ensure the sufficient diffusion of the fragrance on the heated tobacco shreds.
5. According to the preparation method of the natural spice based on the fruit of the snake skin, the fruit peel of the fruit of the snake skin is used as the natural spice, the proportion of sugar and protein in tobacco leaves can be adjusted, the natural spice is a good sour and sweet taste material and a humectant, the natural spice is easy to combine with tobacco, the contained fragrant components are converted into fragrant substances beneficial to cigarettes through pyrolysis, the smoking taste is improved, and the natural spice can be applied to both feeding and surface fragrance.
6. According to the preparation method of the natural spice based on the snake skin fruit, provided by the invention, the peel raw material of the snake skin fruit is easy to obtain, the economic value and the utilization efficiency of the fruit are improved, the fruit grower is helped to widen the income channel, the fruit processing and related enterprises are helped to realize 'changing waste into valuable', and the problem of processing the peel of the snake skin fruit can be effectively solved.
7. The preparation method of the natural spice based on the Chinese wampee fruit, provided by the invention, has the advantages of simple and easily-controlled production process, lower process cost, easiness in 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 flow chart of a method for preparing a natural spice based on snake skin fruit in an embodiment of the present 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 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.
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: 2.
The specific embodiment of the invention is as follows:
example 1
A preparation method of a natural spice based on Chinese wampee fruit comprises the following specific steps:
s1, naturally airing peel of the snake skin fruit in a ventilated and cool place, taking 150g of the aired peel of the snake skin fruit, and crushing to 20 meshes;
s2, adding 12g of the pericarp crushed in the step S1 into 100ml of deionized water for leaching for 15min, then adding 1g of combined enzyme, adding acetic acid to adjust the pH value to 4.0, and hydrolyzing at the rotating speed of 200r/min in a magnetic stirring oil bath kettle at the temperature of 40 ℃ to obtain an enzymolysis product;
s3, adding 70% ethanol into the enzymolysis product obtained in the step S2, performing hot extraction for 2 hours at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:5, centrifuging for 12min at 3200r/min after extraction to obtain peel residues and an extracting solution, and then filtering the extracting solution through a 0.45-micron filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, washing potassium ions on the zeolite by deionized water, and adding a washing solution into the extracting solution subjected to the filtration membrane in the step S3 for later use;
s5, adding 70% ethanol into the pericarp residues adsorbed in the step S4, and performing hot extraction for 1h at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:4 to obtain a secondary extracting solution for later use;
s6, mixing the two extracting solutions obtained in the steps S4 and S5, standing for 1h, filtering with 200-mesh and 500-mesh filter cloth for two times in sequence, taking clear liquid, and concentrating at low temperature under vacuum degree of 80mbar and water bath temperature of 60 ℃ to obtain the natural perfume with the yield of 20.5%.
Example 2
A preparation method of a natural spice based on Chinese wampee fruit comprises the following specific steps:
s1, naturally airing peel of the snake skin fruit in a ventilated and cool place, taking 150g of the aired peel of the snake skin fruit, and crushing to 20 meshes;
s2, adding 14g of the pericarp crushed in the step S1 into 120ml of deionized water for leaching for 18min, then adding 1.3g of combined enzyme, adding acetic acid to adjust the pH value to 4.0, and hydrolyzing at the rotation speed of 200r/min in a magnetic stirring oil bath kettle at the temperature of 45 ℃ to obtain an enzymolysis product;
s3, adding 70% ethanol into the enzymolysis product obtained in the step S2, performing hot extraction for 2 hours at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:5, centrifuging for 13 minutes at 3200r/min after extraction to obtain peel residues and an extracting solution, and then filtering the extracting solution through a 0.45-micron filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, washing potassium ions on the zeolite by deionized water, and adding a washing solution into the extracting solution subjected to the filtration membrane in the step S3 for later use;
s5, adding 70% ethanol into the pericarp residues adsorbed in the step S4, and performing hot extraction for 1h at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:4 to obtain a secondary extracting solution for later use;
s6, mixing the two extracting solutions obtained in the steps S4 and S5, standing for 1h, filtering with 200-mesh and 500-mesh filter cloth for two times in sequence, taking clear liquid, and concentrating at low temperature under reduced pressure under the conditions of 100mbar vacuum degree and water bath temperature of 65 ℃ to obtain the natural perfume with the yield of 20.7%.
Example 3
A preparation method of a natural spice based on Chinese wampee fruit comprises the following specific steps:
s1, naturally airing peel of the snake skin fruit in a ventilated and cool place, taking 150g of the aired peel of the snake skin fruit, and crushing to 20 meshes;
s2, adding 16g of the pericarp crushed in the step S1 into 150ml of deionized water for leaching for 20min, then adding 1.5g of combined enzyme, adding acetic acid to adjust the pH value to 5.0, and hydrolyzing at the rotation speed of 200r/min in a magnetic stirring oil bath kettle at the temperature of 50 ℃ to obtain an enzymolysis product;
s3, adding 70% ethanol into the enzymolysis product obtained in the step S2, performing hot extraction for 2 hours at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:5, centrifuging for 14 minutes at 3200r/min after extraction to obtain peel residues and an extracting solution, and then filtering the extracting solution through a 0.45-micron filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, washing potassium ions on the zeolite by deionized water, and adding a washing solution into the extracting solution subjected to the filtration membrane in the step S3 for later use;
s5, adding 70% ethanol into the pericarp residues adsorbed in the step S4, and performing hot extraction for 1h at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:4 to obtain a secondary extracting solution for later use;
s6, mixing the two extracting solutions obtained in the steps S4 and S5, standing for 1h, filtering with 200-mesh and 500-mesh filter cloth for two times in sequence, taking clear liquid, and concentrating at low temperature under reduced pressure under the conditions of vacuum degree of 120mbar and water bath temperature of 70 ℃ to obtain the natural perfume with the yield of 21.9%.
Comparative example 1
The natural spice is prepared by taking the pulp of the snake skin fruit as a raw material to replace fruit peel through evaporation and concentration.
A preparation method of a natural spice based on Chinese wampee fruit comprises the following specific steps:
s1, removing cores from 34kg of snake skin fruit pulp, squeezing, filtering with 200-mesh filter cloth to obtain primary filtrate, standing for 10h, and filtering with 200-mesh and 500-mesh filter cloth to obtain clarified fresh snake skin fruit juice with 18% of solid content, wherein the juice yield is 39%;
s2, taking 1.2kg of the clarified fresh snake skin juice raw juice prepared in the step S1, placing the juice in a rotary evaporator under the vacuum degree of 100mbar, the water bath temperature is 70 ℃, and evaporating and concentrating until the solid content of the extract is 41.7%, thus obtaining the natural spice.
Comparative example 2
The natural spice is prepared by taking the pulp of the snake skin fruit as a raw material to replace the fruit peel through forward osmosis concentration.
A preparation method of a natural spice based on Chinese wampee fruit comprises the following specific steps:
s1, removing cores from 34kg of snake skin fruit pulp, squeezing, filtering with 200-mesh filter cloth to obtain primary filtrate, standing for 10h, and filtering with 200-mesh filter cloth and 500-mesh filter cloth to obtain clarified fresh snake skin fruit juice with 18% of solid content, wherein the juice yield is 39%;
s2, taking 4.4kg of the clarified fresh snake skin juice raw juice prepared in the step S1, placing the clarified fresh snake skin juice raw juice into a concentration chamber of a forward osmosis concentration device, taking a aquaporin hollow fiber forward osmosis membrane as a separation membrane, taking a saturated NaCl solution as a drawing agent, and carrying out multistage concentration at room temperature, wherein the flow rates of the clarified snake skin juice raw juice and the drawing agent are both controlled to be 0.7L/min. And (3) using 1L of saturated NaCl solution as a drawing agent in the first-stage concentration, when the drawing agent loses the drawing capability, replacing the same amount of saturated NaCl solution as the drawing agent to perform second-stage concentration, and replacing the drawing solution in the same way until the solid content of the snakeskin fruit extract is 41.8%, thereby obtaining the natural perfume.
Comparative example 3
The natural spice is prepared by using the snake skin fruit residues as raw materials to replace fruit peels.
S1, taking 4kg of pomace of fresh snakeskin fruits, and soaking the pomace in 95% ethanol for 12 hours, 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 under 100mbar vacuum degree, water bath temperature of 70 deg.C, and evaporating and concentrating to obtain fruit residue ethanol extract to obtain natural perfume with yield of 77%.
Comparative example 4
And (3) exchanging the ethanol with the mass concentration of 70% for 95% to perform hot extraction.
A preparation method of a natural spice based on Chinese wampee fruit comprises the following specific steps:
s1, naturally airing peel of the snake skin fruit in a ventilated and cool place, taking 150g of the aired peel of the snake skin fruit, and crushing to 20 meshes;
s2, adding 12g of the pericarp crushed in the step S1 into 100ml of deionized water for leaching for 15min, then adding 1g of combined enzyme, adding acetic acid to adjust the pH value to 4.0, and hydrolyzing at the rotating speed of 200r/min in a magnetic stirring oil bath kettle at the temperature of 40 ℃ to obtain an enzymolysis product;
s3, adding 95% ethanol into the enzymolysis product obtained in the step S2, performing hot extraction for 2 hours at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:5, centrifuging for 12min at 3200r/min after extraction to obtain peel residues and an extracting solution, and then filtering the extracting solution through a 0.45-micron filter membrane;
s4, adsorbing the peel residues in the step S3 by zeolite, washing potassium ions on the zeolite by deionized water, and adding a washing solution into the extracting solution subjected to the filtration membrane in the step S3 for later use;
s5, adding 95% ethanol into the pericarp residues adsorbed in the step S4, and performing hot extraction for 1h at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:4 to obtain a secondary extracting solution for later use;
s6, mixing the two extracting solutions obtained in the steps S4 and S5, standing for 1h, filtering with 200-mesh and 500-mesh filter cloth for two times in sequence, taking clear liquid, and concentrating at low temperature under vacuum degree of 80mbar and water bath temperature of 60 ℃ to obtain the natural perfume with yield of 20%.
Comparative example 5
Without pretreatment with combinatorial enzymes
A preparation method of a natural spice based on Chinese wampee fruit comprises the following specific steps:
s1, naturally airing peel of the snake skin fruit in a ventilated and cool place, taking 150g of the aired peel of the snake skin fruit, and crushing to 20 meshes;
s2, adding 70% ethanol into the crushed product obtained in the step S1, performing hot extraction for 2 hours at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:5, centrifuging for 12min at 3200r/min after extraction to obtain peel residues and an extracting solution, and then filtering the extracting solution through a 0.45-micron filter membrane;
s3, adsorbing the peel residues in the step S2 by zeolite, washing potassium ions on the zeolite by deionized water, and adding a washing solution into the extracting solution subjected to the filtration membrane in the step S2 for later use;
s4, adding 70% ethanol into the pericarp residues adsorbed in the step S3, and performing hot extraction for 1h at the water bath temperature of 60 ℃ and the solid-liquid mass ratio of the ethanol hot extraction of 1:4 to obtain a secondary extracting solution for later use;
s5, mixing the two extracting solutions obtained in the steps S3 and S4, standing for 1h, filtering with 200-mesh and 500-mesh filter cloth for two times in sequence, taking clear liquid, and concentrating at low temperature under vacuum degree of 80mbar and water bath temperature of 60 ℃ to obtain the natural perfume with yield of 20%.
The natural flavors prepared in examples 1 to 3 and comparative examples 1 to 5 were added to the respective cut tobaccos to prepare cigarettes, and then the seven cigarettes were subjected to sensory smoking evaluation and preliminary judgment, with the results shown in table 1.
TABLE 1-evaluation results of smoking of natural flavors prepared in examples 1 to 3 and comparative examples 1 to 5 added to tobacco shreds
As can be seen from the results in table 1, the natural flavor prepared in comparative example 2 was added to tobacco shreds with the highest sweetness upon smoking, indicating that forward osmosis concentration can retain the aroma of the fruit of the Chinese artichoke to the greatest extent, but the natural flavor prepared in comparative example 2 has a single aroma, a slightly narrow smoke aroma and a slightly less irritating flavor, indicating that the natural flavor prepared in comparative example 2 is not suitable as an aroma substance of tobacco shreds.
The natural perfume prepared in comparative example 4 was added to tobacco shreds, and the smoking feeling was clear and increased, the fruit note was sour and sweet, much sour and sweet, and increased smoothness of the smoke, with a moist feeling, but the aroma concentration was decreased, the amount of aroma was decreased, the aroma was sunken, still with a greasy smell, and the smoke was smooth and astringent, with a grainy feeling, uncomfortable swallowing, and with a coated feeling.
The natural flavors prepared in examples 1 to 3 are added to tobacco shreds, so that the flavor concentration is increased, the natural tobacco fragrance is more, the smoke is rich in the flavor of the Chinese wampee fruit, the smoking taste is as same as that of drinking functional beverages, the mouth feel is sour, sweet and tasty, and great satisfaction is brought to consumers. The natural spice prepared by selecting the skin of the snake skin, extracting by adopting 70 percent ethanol and evaporating and concentrating is most suitable for being used as the aroma substance of the cut tobacco.
The natural perfume prepared in the comparative example 5 is added into the cut tobacco, so that the aroma concentration is reduced, and the richness of sour and sweet fruits is poor, which indicates that the extraction rate of the peel which is not treated by enzyme is poor, and the separated amino acid is less, so that the aroma concentration of the tobacco is reduced, and the richness of the sour and sweet fruits is poor.
Aroma component detection
The natural flavors prepared in example 1 and comparative examples 1 to 3 were subjected to aroma component detection, and the juice of fresh Chinese artichoke fruit was used as a blank control, and each sample was numbered, and the specific numbers are shown in table 2.
TABLE 2 sample name and number for aroma component detection
| Sample numbering | Sample name | Sample number of sample presentation |
| Example 1 | Extracting fresh fruit peel of snake skin with 70% ethanol, concentrating by evaporation | spg1 |
| Comparative example 2 | Forward concentration of fresh snake skin fruit juice | spg2 |
| Comparative example 1 | Evaporating and concentrating fruit juice of fresh fructus Serpentis | spg3 |
| Blank control | Juice of fresh snake skin fruit | spg4 |
| Comparative example 3 | Extracting fruit residue of fresh fructus Cnidii with 95% ethanol, concentrating by evaporation | spg5 |
| Comparative example 5 | Extracting fresh fruit peel of fruits of snake skin with 70% ethanol, concentrating by heat extraction and evaporation, and treating with no enzyme | Spg6 |
The results of measuring the content of the fragrant components of the natural perfume prepared in example 1 are shown in table 3.
Table 3-spg1 shows the aroma content of the natural perfumes prepared by the samples
The results of measuring the content of the fragrant components of the natural perfume prepared in comparative example 2 are shown in table 4.
TABLE 4-spg2 content of perfuming ingredients in the natural perfumes prepared by the samples
The results of measuring the content of the fragrant components of the natural perfume prepared in comparative example 1 are shown in table 5.
Tables 5-spg3 the aroma content of the natural fragrances prepared from the samples
The results of measuring the aroma component content of the natural spice prepared by using the juice of the fresh Chinese artichoke fruit as a blank control are shown in table 6.
Table 6-spg4 shows the aroma content of the natural perfumes prepared by the samples
The results of measuring the content of the fragrant components of the natural perfume prepared in comparative example 3 are shown in table 7.
Tables 7-spg5 the aroma content of the natural fragrances prepared from the samples
The results of measuring the content of the fragrant components of the natural perfume prepared in comparative example 5 are shown in table 8.
TABLE 8-spg6 content of perfuming ingredients in the natural perfumes prepared by the samples
As can be seen from tables 3 to 8, the types of the aroma components of spg1, spg2, spg3, spg4, spg5 and spg6 are: 22. 11, 10, 11, 25 and 18 types, wherein the types of aroma components in spg4 of the juice of the fresh Chinese artichoke fruits are 11, and the types of aroma components in spg3 are only 10, because the aroma components are damaged by evaporation and concentration of the juice after the fresh Chinese artichoke fruits are squeezed, the types and the total amount are less than those of a control (the juice), and meanwhile, the juice of the fresh Chinese artichoke fruits is not suitable for being used as a raw material of natural spices; spg6 the types and contents of aroma components are less than spg1, because the purification rate of the pericarp of the snake skin is poor due to no addition of the combined enzyme; spg1 and spg5 show a significantly higher number of aroma components than spg2, spg3 and spg4, indicating that natural flavors made using ethanol extraction of the pericarp of fresh hops peel contain more aroma components than natural flavors made using extraction of fresh hops peel juice. Comprehensive sensory evaluation and aroma components of the pericarp, the fruit juice and the pomace, the type and the content of the aroma components of the pericarp are more, and the sensory quality is better.
The amino acid and organic acid contents of the natural spices spg 1-spg 6 are detected, and the detection results are shown in table 8.
Results of content detection of amino acids and organic acids in natural perfume prepared from samples in tables 8-spg 1-spg 6
| Serial number | Inspection item | Unit of | 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 | Undetected (limit of quantitation: 0.001） | 0.018 | 0.005 |
| 4 | serine | % | 0.037 | 0.0077 | 0.008 | 0.0052 | 0.017 | 0.018 |
| 5 | Histidine | % | Undetected (limit of quantitation: 0.002） | undetected (limit of quantitation: 0.002） | undetected (limit of quantitation: 0.002） | undetected (limit of quantitation: 0.002） | undetected (limit of quantitation: 0.002） | undetected (limit of quantitation: 0.002） |
| 6 | glycine | % | 0.0045 | 0.0044 | 0.0044 | 0.0028 | 0.010 | 0.0045 |
| 7 | Threonine | % | Undetected (limit of quantitation: 0.001） | not detected (And (4) quantitative limit: 0.001） | undetected (limit of quantitation: 0.001） | undetected (limit of quantitation: 0.001） | undetected (limit of quantitation: 0.001） | undetected (limit of quantitation: 0.001） |
| 8 | arginine | % | Undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） |
| 9 | alanine | % | 0.049 | Undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | 0.021 |
| 10 | tyrosine | % | Undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） |
| 11 | valine | % | Undetected (limit of quantitation: 0.001） | undetected (limit of quantitation: 0.001） | undetected (limit of quantitation: 0.001） | undetected (limit of quantitation: 0.001） | undetected (limit of quantitation: 0.001） | undetected (limit of quantitation: 0.001） |
| 12 | isoleucine | % | 0.0072 | 0.0089 | 0.0094 | 0.0052 | 0.022 | 0.0072 |
| 13 | Phenylalanine | % | Undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） |
| 14 | lysine | % | 0.0024 | 0.0012 | 0.0018 | 0.0011 | 0.0039 | 0.0024 |
| 15 | Leucine | % | Undetected (limit of quantitation: 0.005） | undetected (limit of quantitation: 0.005） | undetected (limit of quantitation: 0.005） | undetected (limit of quantitation: 0.005） | undetected (limit of quantitation: 0.005） | undetected (limit of quantitation: 0.005） |
| 16 | proline | % | Undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） |
| 17 | methionine | % | Undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 0.010） | undetected (limit of quantitation: 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 amino acid total amount of spg1 (pericarp of fresh snake skin fruit, 70% ethanol extract, concentrated by thermal evaporation) samples was the highest in amino acid total amount and higher in type, which is consistent with the sensory quality results, indicating that the pericarp of 70% ethanol extract is more abundant in sensory quality, especially in taste characteristics.
Spg1 (pericarp of fresh fructus Serpentis, 70% ethanol extract, heat extraction, evaporation and concentration) sample has highest total organic acid content, specifically including citric acid and malic acid. The citric acid can be used as pH regulator, not only has flavoring effect, but also can maintain tobacco leaf quality. The citric acid has the characteristics of chelation and pH value adjustment, so that the performance of an antioxidant can be improved in the processing process, and the shelf life is prolonged. Compared with citric acid, malic acid has high acidity (acidity is 20% stronger than citric acid), but has soft taste (higher buffer index), special fragrance, no damage to oral cavity and teeth, good metabolism for amino acid absorption, no accumulation of fat, and high economic benefit when added into tobacco shreds.
And the sensory quality result shows that the peel of the 70% ethanol extract and the hot-extraction evaporation concentrated sample have more obvious sourness and better sourness in the sensory quality, particularly the taste characteristic, and can be further explained.
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 (10)
1. A preparation method of a natural spice based on the Chinese wampee fruit is characterized by comprising the following steps:
s1, taking and crushing the peel of the snake skin fruit;
s2, adding 12-16g of crushed peel of the S1 into 150ml of deionized water, leaching for 15-20min, adding 1-1.5g of combined enzyme, adjusting the pH value to 4.0-5.0, and hydrolyzing in a magnetic stirring oil bath kettle at 40-50 ℃ at the rotating speed of 200r/min to obtain an enzymolysis product;
s3, adding ethanol into the enzymolysis product in the S2, carrying out ethanol heat extraction, centrifuging for 12-14min at 3200r/min after extraction to obtain pericarp residues and an extracting solution, and then filtering the extracting solution through a 0.45-micrometer filter membrane;
s4, adsorbing the pericarp residues in the S3 by zeolite, washing potassium ions on the zeolite, and adding a washing solution into the filtered extracting solution in the S3 for later use;
s5, carrying out hot extraction on the pericarp residues adsorbed in the step S4 with ethanol again to obtain a secondary extracting solution;
s6, mixing the two extractive solutions obtained in S4 and S5, filtering, and concentrating the clear solution at low temperature under reduced pressure to obtain natural perfume.
2. The method of claim 1, wherein the pericarp of the fruit of the snake skin is naturally dried in the shade before being pulverized in S1, and then pulverized to 20-40 mesh.
3. The method for preparing the natural spice based on the snake skin fruit as claimed in claim 1, wherein the combined enzyme in S2 is a mixture of cellulase, hemicellulase, beta-glucanase, pectinase and serine protease, and the mass ratio of the cellulase, hemicellulase, beta-glucanase, pectinase and serine protease is 1:1:1: 2.
4. The method for preparing natural spice based on snake skin fruit as claimed in claim 1, wherein the temperature of the water bath for hot extraction with ethanol is 60-70 ℃, and the mass concentration of ethanol is 70%.
5. The method for preparing natural spice based on snake skin fruit as claimed in claim 1, wherein the ethanol heat extraction in S3 is carried out for 2h, and the mass ratio of peel to ethanol is 1: 5; and in the S5, the ethanol is subjected to heat extraction for 1h, and the mass ratio of the pericarp to the ethanol is 1: 4.
6. the method of claim 1, wherein the two extracts are mixed at S6, left to stand, filtered through 200 mesh and 500 mesh filter cloth, and the filtered supernatant is concentrated at low temperature under reduced pressure.
7. The method for preparing natural spice based on fruit of snake skin as claimed in claim 1, wherein vacuum degree of low temperature reduced pressure concentration in S6 is 80-120mbar, and water bath temperature is 60-70 ℃.
8. Use of a natural snake fruit based flavour according to any of claims 1-7, wherein said natural flavour is used for addition to cigarettes.
9. The use of the natural cnidium fruit-based spice according to claim 8, wherein the natural spice is uniformly sprayed into tobacco shreds to form cigarettes.
10. Use of a natural cnidium fruit-based flavour according to claim 9, wherein the mass ratio of said natural flavour to cut tobacco is (1-5): 1000.
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