CN111838746A - A bead, its preparation method and application in cigarette - Google Patents
A bead, its preparation method and application in cigarette Download PDFInfo
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- CN111838746A CN111838746A CN201910362568.0A CN201910362568A CN111838746A CN 111838746 A CN111838746 A CN 111838746A CN 201910362568 A CN201910362568 A CN 201910362568A CN 111838746 A CN111838746 A CN 111838746A
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- industrial hemp
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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
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
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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
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
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Abstract
The invention provides a popping bead, a preparation method thereof and application thereof in cigarettes, wherein the popping bead has special fragrance of industrial hemp, brings better mouthfeel, and simultaneously can reduce the inhalation of harmful substances and reduce the stimulation of tobacco to throat. The preparation method of the blasting bead provided by the invention comprises the following steps of A) preparing a blasting bead substrate: dissolving industrial hemp volatile oil in industrial hemp seed oil, and then adding an emulsifier and an antioxidant to obtain a popping matrix; B) emulsification: adding a calcium salt aqueous solution into the bead blasting matrix, and emulsifying to obtain an emulsion, wherein the mass ratio of the calcium salt aqueous solution to the bead blasting matrix is 1:5-5: 1; C) molding: dripping the emulsion into the wall material solution I for soaking; and drying to obtain the blasting beads.
Description
Technical Field
The invention relates to the field of tobacco, in particular to a bead, a preparation method thereof and application thereof in cigarettes.
Background
A bead for puffing cigarette is a spherical object containing liquid, which is divided into water-based bead and oil-based bead, the outer skin is made of colloidal high-molecular material, the inner container is made of oil-based or water-based matrix, and is placed in the filter tip of cigarette.
Cannabis sativa L, a name of Cannabis sativa L, is a plant of the genus Cannabis of the family Cannabaceae, and has important agricultural and medicinal values. The hemp contains a toxic component Tetrahydrocannabinol (THC), can cause people to be fantastic to addict, can be used as a drug, but the hemp has extremely high economic and medicinal values, the raw material hemp specially used for industrial application is called industrial hemp for short, the THC content in the hemp flower leaves in the growth period is less than three thousandth, the hemp flower leaves do not have the purpose of extracting the toxic component THC, and the hemp flower leaves can be legally planted in a large scale and used for industrial development.
In the prior art, the cigarette blasting beads used have many improvements, such as diversification of taste and reduction of harmful substance absorption while satisfying the taste.
Disclosure of Invention
In view of the above, the present invention provides a popping bead, which has a special fragrance of industrial hemp, brings a better taste, and simultaneously reduces the inhalation of harmful substances and the irritation of tobacco to throat.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a blasting bead, which comprises the following steps,
A) preparing a bead blasting matrix: dissolving industrial hemp volatile oil in industrial hemp seed oil, and then adding an emulsifier and an antioxidant to obtain a popping matrix;
Wherein the mass ratio of the industrial hemp volatile oil to the industrial hemp seed oil is 1:10000-1:100 (such as 1:10000, 1:5000, 1:1000, 1:500, 1:100, etc.); the emulsifier is used in an amount of 0.01-0.1% (e.g., 0.01%, 0.05%, 0.1%, etc.) by mass, and the antioxidant is used in an amount of 0.01-0.1% (e.g., 0.01%, 0.05%, 0.1%, etc.) by mass, based on the total mass of the industrial hemp volatile oil and the industrial hemp seed oil;
B) emulsification: adding a calcium salt aqueous solution into the bead blasting matrix, and emulsifying to obtain an emulsion, wherein the mass ratio of the calcium salt aqueous solution to the bead blasting matrix is 1:5-5:1 (such as 1:5, 1:3, 1:1, 3:1, 5:1 and the like), and the mass concentration of the calcium salt aqueous solution is preferably 1-10%; the emulsification is high-speed emulsification at 6000-25000 r/min;
C) molding: dripping the emulsion into the wall material solution I for soaking, wherein the surface of the emulsion can be solidified after the emulsion is dripped into the wall material solution I, and the solidification effect can be improved through soaking; then drying to obtain the blasting beads; the drying is preferably carried out at 20 to 50 ℃.
In some embodiments, the emulsifier in step a) is selected from one or a combination of two or more of polyethylene glycol, tween and span.
In some embodiments, the antioxidant of step a) is selected from the group consisting of fat-soluble antioxidants; preferably, the antioxidant is selected from one or a combination of two or more of Butylated Hydroxyanisole (BHA), Butylated Hydroxytoluene (BHT), Propyl Gallate (PG), tert-butylhydroquinone (TBHQ), and tocopherol.
In the step B), adding a calcium salt aqueous solution into the bead blasting matrix, wherein the mass ratio of the calcium salt aqueous solution to the bead blasting matrix is 1:5-5:1, so that a good curing effect is favorably achieved, and if the amount of the calcium salt aqueous solution is too large, the calcium salt aqueous solution is easy to become brittle, and if the amount of the calcium salt aqueous solution is too small, the good curing effect cannot be achieved; the calcium salt water solution is added to mainly exchange with gel ions to form a gel-like substance. In some embodiments, the calcium salt in step B) is selected from one or a combination of two or more of calcium bicarbonate, calcium carbonate, calcium chloride, and calcium nitrate.
In some embodiments, in the step C), the emulsion is dropped (preferably dropped at a uniform speed) into the wall material solution I at a speed of 1 to 5ml/min, and is preferably soaked in the wall material solution I for 1 to 10min (for example, soaking for 1min, 3min, 5min, 8min10min, etc.).
In some embodiments, the wall material solution I is preferably an aqueous sodium alginate solution, and more preferably an aqueous sodium alginate solution with a mass concentration of 1-10%.
In some embodiments, in the step C), after the emulsion is dropped into the wall material solution I for soaking and before the drying, the wall material solution II is further soaked, preferably, the time for soaking with the wall material solution II is 1-10min (for example, soaking for 1min, 3min, 5min, 8min 10min, etc.), and by soaking in the wall material solution II again, a layer of skin can be added, and the stability of the blasting beads can be increased. Optionally, after the wall material solution I is soaked, the wall material solution I is washed with water and then soaked with the wall material solution II, which is beneficial to obtaining a better appearance and is beneficial to forming.
In some embodiments, it is preferable that the wall material solution II is an aqueous solution of one or a combination of two or more of gelatin, polysaccharide, carrageenan, pectin, and ichthyol; in some embodiments, it is preferable that the wall material solution II is used at a mass concentration of 1 to 20%.
In some embodiments, the drying in step C) is drum drying, forced air drying or belt drying, preferably drum drying; the drying temperature is preferably 20-50 ℃.
The industrial hemp volatile oil in step A) can be obtained by adopting an extraction process disclosed in the field, for example, the volatile oil extracted from the parts such as leaves, stems and the like of the industrial hemp. In some preferred embodiments, the industrial hemp essential oil described in step a) is prepared by a process comprising the steps of:
1) Drying and dehydrating the hemp flowers and leaves of the industrial hemp to a moisture content of 20 wt% to 30 wt%, for example, 20 wt%, 22 wt%, 24 wt%, 26 wt%, 30 wt%, etc.;
2) pulverizing the dried and dehydrated industrial hemp flowers and leaves obtained in the step 1) into powder, and removing the industrial hemp seeds in the powder, for example, removing the wrapped hemp seeds by air separation;
3) placing the industrial hemp flower and leaf material treated in the step 2) in a heating and drying device, wherein the heating temperature is 100 ℃ and 120 ℃ (for example, 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃ and the like); the air outlet of the heating drying device is connected with a condensing device, and the condensing device is used for condensing the gas exhausted from the air outlet and obtaining condensate containing volatile oil;
4) extracting the condensate obtained in the step 3) with an extracting agent to obtain volatile oil, taking supernatant, wherein the extracting agent is preferably selected from one or a combination of more than two of ethyl acetate, n-heptane, n-butanol, n-hexane, dichloromethane and petroleum ether, and the preferred extracting agent is adopted, so that the yield of the volatile oil is high, and terpene components can be better dissolved;
5) washing the supernatant obtained in the step 4) with water, removing a water layer, and distilling the obtained organic layer to obtain the industrial hemp volatile oil.
The volatile oil is extracted from the industrial hemp according to the steps, so that the technical defect that the volatile oil component of the industrial hemp is not utilized but is discharged along with waste gas in the prior art can be overcome; the method for extracting the industrial hemp volatile oil needs less organic solvent and has low organic solvent residue. The obtained volatile oil has special fragrance of industrial hemp.
Extracting industrial hemp volatile oil by adopting the steps 1) -5), wherein in the step 1), the moisture of the industrial hemp leaves is controlled to be 20-30 wt%, so that the volatile oil in the step 3) is favorably carried out, and the extraction rate of the volatile oil is improved; if the water content is too low, the volatile oil is not easy to be brought out during subsequent heating and drying; if the moisture content is too high, the energy consumption will be increased due to the excessive moisture of the material. In the step 3), heating and drying are carried out at the temperature of 100-120 ℃, so that more than 95% of volatile oil components can be volatilized at the temperature; on the other hand, the method can carry out decarboxylation reaction on the cannabinol acid components, is beneficial to the subsequent extraction process of the cannabinol substances, and can increase the yield of the cannabinol components. The industrial hemp volatile oil obtained by the steps 1) to 5) mainly contains terpenes, and is characterized by containing p-cymene, alpha-bisabolol, ocimene, alpha-terpinene, beta-caryophyllene, guaiol, geraniol, beta-pinene, beta-ocimene, isoterpinene, beta-pinene, trans-nerolidol, 4-methoxybenzyl alcohol, isopulegol, alpha-lupinene, beta-myrcene, limonene, nerolidol, linalool and/or gamma-terpinene and the like. The obtained industrial hemp volatile oil has special fragrance of industrial hemp.
The industrial hemp flowers and leaves used in step 1) are preferably industrial hemp flowers and leaves which have not been subjected to extraction treatment of hemp phenols, for example, volatile oil extraction is carried out before the extraction of hemp phenols.
In step 1), the drying and dehydration are, for example, drying in the shade; preferably, in the step 1), the drying and dehydration are carried out at a temperature of 10-30 ℃.
In the step 2), the pulverized powder is preferably coarse powder which is pulverized into 10-20 meshes (such as 10 meshes, 13 meshes, 15 meshes, 18 meshes, 20 meshes and the like), so that the volatile components are volatilized, and the method is more convenient for continuously extracting the cannabis phenolic components at a later stage.
In some preferred embodiments, in step 3), the industrial hemp flower and leaf material is heated in the heating and drying device at 100-. In some preferred embodiments, in step 3), the heating and drying device is preferably a thermal circulation dryer (or called a hot air circulation dryer) or a belt dryer, and preferably, the two types of heating and drying devices are favorable for extracting volatile oil of industrial hemp flower and leaf materials, and then continuing to extract the hemp phenolic components, so as to reduce the influence on the hemp phenolic components.
In some preferred embodiments, the condensing device comprises a condensing pipe connected with the air outlet of the heating and drying device, the temperature of the condensing pipe is controlled to be-5 ℃ to 5 ℃ (for example, -5 ℃, 2 ℃, 0 ℃, 3 ℃, 5 ℃ and the like), and the condensing pipe is connected with a volatile oil storage tank; the volatile oil storage tank is externally provided with a heat-insulating layer, the temperature of the heat-insulating layer is controlled to be 2-10 ℃ (such as 2 ℃, 5 ℃, 7 ℃, 10 ℃ and the like), and the condensed volatile oil paste can be prevented from continuously volatilizing, so that the effect of cold storage is achieved. And finally obtaining volatile oil condensed cream, namely the volatile oil cream in a volatile oil storage tank.
In some preferred embodiments, the ratio of the mass of industrial cannabis leaves before drying and dewatering in step 1) to the volume of extractant used in a single extraction in step 4) is from 10:1 to 1:1 (e.g., 10:1, 7:1, 5:1, 3:1, 1:1, etc.) in kg/L; preferably, the extraction in step 4) is performed two or more times.
In some preferred embodiments, the washing in step 5) is performed with water in a volume ratio of 10:1 to 1:5 to the extractant used in step 4), and the washing with water is performed to dissolve impurities dissolved in water into a water layer and purify the terpene-based component; preferably, the washing in step 5) is performed two or more times.
In some preferred embodiments, in step 5), the distillation is carried out at a temperature < 60 ℃ (preferably 40-60 ℃) and at a pressure of-0.02 to-0.05 MPa; preferably, the distillation ends at a distillate outflow rate of less than 10 drops/min.
The method of the steps 1) to 5) is adopted to extract the industrial hemp volatile oil, the terpene components in the industrial hemp volatile oil can be extracted to a great extent, the organic solvent residue is low (the organic solvent residue is below 200 ppm), and the special aroma of the industrial hemp can be reduced; after the volatile oil is extracted from the industrial hemp flowers and leaves by adopting the method, the hemp phenols can be continuously extracted from the industrial hemp flowers and leaves, so that the volatile oil can be prevented from being discharged along with waste gas and not being effectively utilized, and the subsequent extraction of the hemp phenols is not influenced.
The second aspect of the invention provides a bead blasting method, which comprises the steps of preparing a bead blasting matrix as a core material, wherein the bead blasting matrix comprises industrial hemp volatile oil, industrial hemp seed oil, an emulsifier and an antioxidant; the mass ratio of the industrial hemp volatile oil to the industrial hemp seed oil is 1:10000-1: 100; based on the total mass of the industrial hemp volatile oil and the industrial hemp seed oil, the mass dosage of the emulsifier is 0.01-0.1%, and the mass dosage of the antioxidant is 0.01-0.1%.
In some embodiments, it is preferable that the emulsifier is selected from one or a combination of two or more of polyethylene glycol, tween and span.
In some embodiments, it is preferable that the antioxidant is selected from fat-soluble antioxidants, and it is further preferable that the antioxidant is selected from one or a combination of two or more of Butylated Hydroxyanisole (BHA), Butylated Hydroxytoluene (BHT), Propyl Gallate (PG), Tertiary Butyl Hydroquinone (TBHQ), and tocopherol.
In some embodiments, the wall material is preferably selected from one or a combination of two or more of sodium alginate, gelatin, polysaccharide, carrageenan, pectin and ichthyol, and preferably the combination of two or more wall materials at least contains sodium alginate.
In some embodiments, it is preferred that the popple is made using the method of making as described above.
The invention also provides a cigarette, which contains the popping beads prepared by the preparation method or the popping beads prepared by the preparation method.
In the invention, the used industrial hemp volatile oil and industrial hemp seed oil are both from industrial hemp varieties with THC content below 3 per mill, have no social hazard, and have been legally and normatively planted in Yunnan, Heilongjiang and other places.
The technical scheme provided by the invention has the following beneficial effects:
the industrial hemp fragrance type bead blasting developed by the invention is added with the industrial hemp volatile oil, contains the main flavor source terpene components in the industrial hemp, takes the industrial hemp seed oil as the main substrate, has the special fragrance of the industrial hemp, has natural and lasting fragrance and smooth mouthfeel, and can meet the diversified and individual requirements.
The blasting beads developed by the invention not only can enrich the fragrance of tobacco, but also can bring special fragrance of industrial hemp; and the industrial hemp seed oil and the industrial hemp volatile oil are added simultaneously, so that the throat-moistening tea has special fragrance of industrial hemp, can remove free radicals to reduce cigarette harm, can moisten throat when in use, and can adsorb harmful substances such as tar, nicotine and carbon monoxide in the combustion of tobacco, thereby reducing the stimulation of the tobacco to the throat, having better taste and reducing the inhalation of the harmful substances.
The invention has good bead bursting formability, high yield, easy extrusion and stable quality when in use.
Drawings
FIGS. 1-2 are, in sequence, the total ion flow diagrams of the industrial hemp volatile oils of examples 6-7, respectively.
Detailed Description
In order to better understand the technical solution of the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
The raw materials used in the following examples are all commercially available conventional raw materials unless otherwise specified.
Example 1
Dissolving 1g of industrial hemp volatile oil into 100g of industrial hemp seed oil, and adding 0.1g of polyethylene glycol 400 and 0.05g of tert-butyl hydroquinone (TBHQ) to obtain a blasting bead matrix;
adding 100g of 5 wt% calcium bicarbonate aqueous solution into the bead blasting matrix, and emulsifying at 10000r/min for 10min to obtain emulsion;
dripping the emulsion into 5 wt% sodium alginate aqueous solution at a rate of 3ml/min, soaking for 5min, adding 10 wt% fish scale glue aqueous solution, soaking for 10min, taking out, drying at 40 deg.C, and obtaining the bead with particle size of 2-3 mm.
The industrial hemp volatile oil used in this example was the industrial hemp volatile oil prepared in example 6 below.
Example 2
Dissolving 0.1g industrial hemp volatile oil into 100g industrial hemp seed oil, adding 0.1g span and 0.05g Propyl Gallate (PG), to obtain blasting pill matrix;
Adding 20g of 1 wt% calcium bicarbonate aqueous solution into the blasting bead matrix, and emulsifying at 6000r/min at a high speed for 5min to obtain emulsion;
dripping the emulsion into 1 wt% sodium alginate aqueous solution at a rate of 2ml/min, soaking for 10min, adding into 5 wt% fish scale glue aqueous solution, soaking for 1min, taking out, drying at 30 deg.C, and obtaining the pop beads with particle size of 2-3 mm.
The industrial hemp volatile oil used in this example was the industrial hemp volatile oil prepared in example 7 below.
Example 3
Dissolving 0.01g industrial hemp volatile oil into 100g industrial hemp seed oil, adding 0.1g tween 80 and 0.1g Butylated Hydroxyanisole (BHA), and making into blasting pill matrix;
adding 50ml of 5 wt% calcium bicarbonate aqueous solution into the blasting bead matrix, and emulsifying at a high speed of 15000r/min for 5min to obtain emulsion;
dripping 5ml/min of the emulsion into 10 wt% sodium alginate aqueous solution, soaking for 5min, adding 10 wt% gelatin aqueous solution, soaking for 10min, taking out, drying at 50 deg.C, and obtaining the bead with particle size of 2-3 mm.
The industrial hemp volatile oil used in this example was the industrial hemp volatile oil prepared in example 6 below.
Example 4
Dissolving 0.05g of industrial hemp volatile oil into 100g of industrial hemp seed oil, and adding 0.1g of tween 80 and 0.04g of tocopherol to obtain a blasting pill matrix;
Adding 500g of 1 wt% calcium bicarbonate aqueous solution into the bead blasting matrix, and emulsifying at a high speed of 25000r/min for 5min to obtain emulsion;
dripping 1ml/min of the emulsion into 7 wt% sodium alginate aqueous solution, soaking for 1min, adding 20 wt% gelatin aqueous solution, soaking for 10min, taking out, drying at 20 deg.C, and obtaining the bead with particle size of 2-3 mm.
The industrial hemp volatile oil used in this example was the industrial hemp volatile oil prepared in example 7 below.
Example 5
The effect of the blasting beads prepared in examples 1-4 on total particulate matters TPM, tar, total nicotine content and CO content of cigarette smoke is detected by a smoking machine (Borgwaldt, Germany, RM200), all experimental cigarettes are Hongtahan 1956, the position of adding the blasting beads is the position of a filter tip, the dosage is 1 particle per cigarette, and the detection result is as follows:
TABLE 1 influence of bead blasting on the total particulate matter TPM, tar, total nicotine content, CO content of cigarette smoke
As can be seen from Table 1, compared with the comparative example, the total particulate matter TMP, tar, total nicotine and CO content of the smoke are all significantly reduced after the bead blasting is added, which shows that the bead blasting of the invention can significantly reduce the harmful substances generated in the combustion of the tobacco after the bead blasting is added into the cigarette.
Example 6
The industrial hemp volatile oil used in examples 1 and 3 was prepared as follows:
1) Taking 100kg of fresh industrial hemp flower and leaf, drying in the shade at 30 ℃ for 72h, wherein the moisture content of the industrial hemp flower and leaf is 21 wt%;
2) beating the industrial hemp flowers and leaves obtained in the step 1) into coarse powder (20 meshes), and removing the coated industrial hemp seeds by air separation;
3) placing the coarse powder obtained in the step 2) in a heat circulation dryer (namely a hot air circulation dryer), and heating for 1h at 100 ℃; the air outlet of the thermal cycle dryer is connected with a condenser pipe, and the temperature of the condenser pipe is-5 ℃; the condensation pipe is connected with a volatile oil storage tank in a downward connection mode, and a heat insulation layer is arranged outside the volatile oil storage tank and is at the temperature of 5 ℃; collecting condensed ointment in a volatile oil storage tank;
4) extracting the condensed paste with 100L ethyl acetate twice, and mixing the supernatants;
5) and (3) adding purified water with the same amount as the ethyl acetate in the step (4) to wash twice, and distilling the ethyl acetate layer (60 ℃, the pressure is-0.05 MPa) to less than 10 drops/min to obtain the distillation end point, thereby obtaining the industrial hemp volatile oil.
Taste of the obtained industrial hemp volatile oil: has special fragrance of industrial hemp.
And (3) identification: the following characteristic components (detection limit 10ppm) were detected by GC-MS detection,
p-cymene (1), alpha-bisabolol (2), ocimene (3), alpha-terpinene (4), beta-caryophyllene (5), guaiol (6), geraniol (7), alpha-pinene (8), beta-ocimene (9), isoterpinene (10), beta-pinene (11), trans-nerolidol (12), 4-methoxybenzyl alcohol (13), isopulegol (14), alpha-lupinene (15), beta-myrcene (16), limonene (17), nerolidol (18), linalool (19) and gamma-terpinene (20).
Referring to fig. 1, the total ion current of industrial hemp volatile oil is shown in the following table:
| peak number | Retention time | Identification of components |
| 1 | 20.8431 | P-cymene |
| 2 | 24.6419 | Alpha-bisabolol |
| 3 | 36.2232 | Ocimum basilicum |
| 4 | 36.4626 | Alpha-terpinene |
| 5 | 37.4119 | Beta-caryophyllene |
| 6 | 38.4571 | Guaiol |
| 7 | 38.7662 | Geraniol |
| 8 | 41.239 | Alpha-pinene |
| 9 | 41.3389 | Beta-ocimene |
| 10 | 41.6722 | Terpinolene |
| 11 | 42.6882 | Beta-pinene |
| 12 | 44.7024 | Trans-nerolidol |
| 13 | 45.3459 | 4-Methoxybenzyl alcohol |
| 14 | 47.0311 | Isopulegol |
| 15 | 48.2081 | Alpha-lupinenes |
| 16 | 49.1931 | Beta-myrcene |
| 17 | 51.4322 | Limonene |
| 18 | 52.1775 | Nerolidol |
| 19 | 55.3664 | Linalool |
| 20 | 55.7843 | Gamma-terpinene |
Example 7:
the industrial hemp volatile oil used in examples 2 and 4 was prepared as follows:
1) taking 10kg of fresh industrial hemp flower and leaf, drying in the shade at 24 ℃ for 36h, wherein the moisture content of the industrial hemp flower and leaf is 25 wt%;
2) beating the industrial hemp flowers and leaves obtained in the step 1) into coarse powder (10 meshes), and removing the coated industrial hemp seeds by air separation;
3) placing the coarse powder obtained in the step 2) in a thermal circulation dryer, and heating for 2 hours at 120 ℃; an air outlet of the thermal cycle dryer is connected with a condensing pipe, and the temperature of the condensing pipe is 5 ℃; the condensation pipe is connected with a volatile oil storage tank in a downward connection mode, and a heat insulation layer is arranged outside the volatile oil storage tank and is at the temperature of 10 ℃; collecting condensed ointment in a volatile oil storage tank;
4) extracting the condensed paste with n-hexane twice, wherein the amount of n-hexane is 1L each time, and mixing the supernatants;
5) And (3) adding purified water with the same amount of n-hexane as the amount used in the step 4) to wash twice, and distilling the n-hexane layer (at the temperature of 40 ℃, the pressure of-0.02 MPa) until the concentration is less than 10 drops/min to obtain the industrial hemp volatile oil.
Taste of the obtained industrial hemp volatile oil: has special fragrance of industrial hemp.
And (3) identification: the following characteristic components (detection limit 10ppm) can be detected by GC-MS detection:
p-cymene (1), alpha-bisabolol (2), ocimene (3), alpha-terpinene (4), beta-caryophyllene (5), guaiol (6), geraniol (7), beta-pinene (8), beta-ocimene (9), isoterpinene (10), beta-pinene (11), trans-nerolidol (12), 4-methoxybenzyl alcohol (13), isopulegol (14), alpha-lupinene (15), beta-myrcene (16), limonene (17), nerolidol (18), linalool (19) and gamma-terpinene (20).
Referring to fig. 2, the total ion current chart of industrial hemp volatile oil is shown in the following table:
example 8
The residual solvents of the industrial hemp volatile oils of examples 6 to 7 above were examined:
chromatographic conditions and system applicability test: a capillary column taking 100% dimethyl polysiloxane (or similar polarity) as a stationary liquid is taken as a chromatographic column; the initial temperature is 40 ℃, the temperature is kept for 6 minutes, and then the temperature is increased to 120 ℃ at the rate of 10 ℃ per minute; the temperature of a sample inlet is 200 ℃; the temperature of the detector is 250 ℃; the headspace bottle had an equilibration temperature of 90 ℃ and an equilibration time of 30 minutes. Taking a reference substance solution to perform headspace sample injection; a blank sample is 4ml of methanol and precisely added into a headspace bottle to serve as a blank control.
Control solution: taking about 300mg of the extracted organic solvent, precisely weighing, placing in a volumetric flask, diluting with chromatographic methanol to a constant volume of 1000ml, precisely weighing 4ml, placing in a headspace flask, sealing, and using as a reference solution.
Preparation of a test solution: the industrial cannabis volatile oil prepared in the above examples was taken as the product (about 200mg), precisely weighed, placed in a headspace bottle, precisely added with chromatographic methanol solution 4m l, sealed and dissolved, as the test solution.
The determination method comprises the following steps: respectively injecting a reference substance solution and a test substance solution, recording a chromatogram, and calculating by peak area according to an external standard method, wherein the result is shown in the following table:
the GC-MS assays referred to in examples 6-7 above are illustrated below:
gas chromatography conditions: the column was DB5, (30.0m × 200 μm, 0.25 μm); the split ratio is 20: 1; the temperature of a sample inlet is 250 ℃; the starting temperature was 50 deg.C (held for 1min) and increased to 210 deg.C (held for 5min) at a rate of 4 deg.C/min.
Mass spectrum conditions: EI source, electron energy 70eV, ion source 210 ℃, mass spectrometer: finniqan ITD800, solvent retardation of 5min, scanning mass range of 40-400 u, electron energy of 70 eV.
The hemp flowers and leaves used in the examples were all industrial hemp flowers and leaves.
It will be appreciated by those skilled in the art that modifications or adaptations to the invention may be made in light of the teachings of the present specification. Such modifications or adaptations are intended to be within the scope of the present invention as defined in the claims.
Claims (10)
1. A preparation method of the blasting bead is characterized by comprising the following steps,
A) preparing a bead blasting matrix: dissolving industrial hemp volatile oil in industrial hemp seed oil, and then adding an emulsifier and an antioxidant to obtain a popping matrix;
wherein the mass ratio of the industrial hemp volatile oil to the industrial hemp seed oil is 1:10000-1: 100;
based on the total mass of the industrial hemp volatile oil and the industrial hemp seed oil, the mass usage of the emulsifier is 0.01-0.1%, and the mass usage of the antioxidant is 0.01-0.1%;
B) emulsification: adding a calcium salt aqueous solution into the bead blasting matrix, and emulsifying to obtain an emulsion, wherein the mass ratio of the calcium salt aqueous solution to the bead blasting matrix is 1:5-5:1, and the mass concentration of the calcium salt aqueous solution is preferably 1-10%;
C) molding: dripping the emulsion into the wall material solution I for soaking; and drying to obtain the blasting beads.
2. The method according to claim 1, wherein the emulsifier in step A) is selected from one or more of polyethylene glycol, tween and span.
3. The process according to claim 1 or 2, wherein the antioxidant of step a) is selected from fat-soluble antioxidants;
preferably, the antioxidant is selected from one or a combination of more than two of butyl hydroxy anisole, dibutyl hydroxy toluene, propyl gallate, tert-butyl hydroquinone and tocopherol.
4. The method according to any one of claims 1 to 3, wherein the calcium salt in step B) is selected from one or a combination of two or more of calcium bicarbonate, calcium carbonate, calcium chloride and calcium nitrate.
5. The method according to any one of claims 1 to 4, wherein in step C), the emulsion is dropped into the wall material solution I at a speed of 1 to 5ml/min, preferably the wall material solution I is soaked for 1 to 10 min;
preferably, the wall material solution I is a sodium alginate aqueous solution, and more preferably a sodium alginate aqueous solution with the mass concentration of 1-10%.
6. The method according to any one of claims 1 to 5, wherein in step C), after the emulsion is dropped into the wall material solution I for soaking and before the drying, the wall material solution II is soaked, preferably for 1 to 10 min;
Preferably, the wall material solution II is an aqueous solution of one or a combination of more than two of gelatin, polysaccharide, carrageenan, pectin and fish scale glue;
preferably, the mass concentration of the wall material solution II is 1-20%.
7. The method according to any one of claims 1 to 6, wherein the drying in step C) is drum drying, air-blast drying or belt drying, preferably drum drying; the drying temperature is preferably 20-50 ℃.
8. The process according to any one of claims 1 to 7, wherein the industrial hemp volatile oil of step A) is obtained by a process comprising the steps of:
1) drying and dehydrating the hemp flowers and leaves of the industrial hemp to ensure that the moisture content of the hemp flowers and leaves is 20 to 30 weight percent; preferably, the drying and dehydration in the step 1) are carried out at the temperature of 10-30 ℃;
2) pulverizing the dried and dehydrated industrial hemp flowers and leaves in the step 1) into powder, and removing industrial hemp seeds; preferably, the powdering in the step 2) is powdering into 10-20 meshes of coarse powder;
3) placing the industrial hemp flower and leaf material treated in the step 2) in a heating and drying device, wherein the heating temperature is 100-120 ℃; the air outlet of the heating drying device is connected with a condensing device, and the condensing device is used for condensing the gas exhausted from the air outlet and obtaining condensate containing volatile oil; preferably, the heating and drying device is a heat circulation dryer or a belt dryer;
4) Extracting the condensate obtained in the step 3) with an extracting agent to obtain volatile oil, and taking supernatant, wherein the extracting agent is preferably one or a combination of more than two of ethyl acetate, n-heptane, n-butanol, n-hexane, dichloromethane and petroleum ether;
preferably, the ratio of the mass of the industrial hemp flowers before being dried and dehydrated in the step 1) to the volume of the extracting agent used in the extraction of the step 4) for one time is 10:1-1:1, and the unit is kg/L; preferably, the extraction in step 4) is carried out two or more times;
5) washing the supernatant obtained in the step 4) with water, removing a water layer, and distilling the obtained organic layer to obtain industrial hemp volatile oil;
preferably, the distillation in step 5) is carried out at a temperature of < 60 ℃ and a pressure of-0.02 to-0.05 MPa; it is further preferred that the temperature of the distillation is 40-60 ℃.
9. The blasting bead is characterized by comprising a wall material and a blasting bead matrix serving as a core material, wherein the blasting bead matrix comprises industrial hemp volatile oil, industrial hemp seed oil, an emulsifier and an antioxidant; the mass ratio of the industrial hemp volatile oil to the industrial hemp seed oil is 1:10000-1: 100; based on the total mass of the industrial hemp volatile oil and the industrial hemp seed oil, the mass usage of the emulsifier is 0.01-0.1%, and the mass usage of the antioxidant is 0.01-0.1%;
Preferably, the emulsifier is selected from one or a combination of more than two of polyethylene glycol, tween and span;
preferably, the antioxidant is selected from fat-soluble antioxidants, and more preferably, the antioxidant is selected from one or a combination of more than two of butyl hydroxyanisole, dibutyl hydroxytoluene, propyl gallate, tert-butyl hydroquinone and tocopherol;
preferably, the wall material is one or a combination of more than two of sodium alginate, gelatin, polysaccharide, carrageenan, pectin and fish scale glue, preferably a combination of more than two wall materials and at least contains sodium alginate;
preferably, the blasting bead is prepared by the preparation method of any one of claims 1 to 8.
10. A cigarette comprising a popping bead produced by the method of any one of claims 1 to 8 or the popping bead of claim 9.
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