CN114886147B - Method for extracting old medicine orange spice and application of old medicine orange spice in cigarettes - Google Patents
Method for extracting old medicine orange spice and application of old medicine orange spice in cigarettes Download PDFInfo
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- CN114886147B CN114886147B CN202210655782.7A CN202210655782A CN114886147B CN 114886147 B CN114886147 B CN 114886147B CN 202210655782 A CN202210655782 A CN 202210655782A CN 114886147 B CN114886147 B CN 114886147B
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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
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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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- 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
Abstract
The invention provides a method for extracting old medicine orange spice, which adopts a separation technology combining microfiltration, ultrafiltration and nanofiltration to carry out multistage membrane separation on an old medicine orange primary extract, and carries out concentration through a forward concentration technology to finally obtain the old medicine orange spice. The old medicinal orange spice obtained by the invention has unique style characteristics of fruit aroma, orange peel aroma, fresh sweet, sweet aftertaste and the like, is diluted by ethanol and then is uniformly sprayed into tobacco shreds to be used as a natural tobacco spice, and the prepared cigarette has unique style characteristics of fruit aroma, orange peel aroma, fresh sweet, sweet aftertaste and the like, can improve throat stimulation and aftertaste, increase mouth moistening feeling, body fluid sweet feeling and comfortable feeling, and improve cigarette quality. The extraction method of the old medicine orange spice provided by the invention has the advantages of short process period, environmental protection, safety, convenience for large-scale and industrial production and higher economic benefit.
Description
Technical Field
The invention belongs to the technical field of production of tobacco essence flavors, and particularly relates to an extraction method of an old medicine orange flavor and application of the old medicine orange flavor in cigarettes.
Background
The essence and spice are important for improving the smoking quality of cigarette products, and the natural spice is currently the mainstream of people for the advantages of ecology, safety, greenness, environmental protection and the like. In the process of shaping the aroma style of cigarettes, various natural extracts are often added to solve the problems of weak aroma, poor smoke softness, weak sweetness, insufficient thickness and the like.
The old medicinal orange is prepared by picking and cleaning fruit of Fortunella margarita (lour.) Swingle of Fortunella of Rutaceae, boiling with water, removing astringent taste, adding appropriate amount of salt, sugar and other adjuvants (such as fructus crataegi, glycyrrhrizae radix, herba Menthae, cortex Cinnamomi, etc.), and pickling until the surface is brown and the Fortunella margarita (lour.) Swingle is flat and round.
The old medicine orange is strong and attractive in smell, salty and sweet, and the aqueous extract of the old medicine orange has unique fruity aroma, orange peel aroma and other aroma characteristics. However, although the traditional separation means such as water extraction and alcohol precipitation, filter screen filtration and the like used at present can remove part of suspended impurities and insoluble macromolecular impurities in the old medicine orange extracting solution, when the obtained old medicine orange spice is added into cigarettes for evaluation, the mixed gas is heavy, the stimulation is obvious, the aftertaste is uncomfortable, the aroma fidelity is low, and the aroma can not be applied to the cigarettes. Even after multiple times of alcohol precipitation and filtration, the problems can not be solved, and the reason is quite unexpected.
In addition, the existing natural tobacco flavor concentration technology mostly adopts an evaporation concentration process, the heating temperature is high, the concentration time is long, the energy consumption is high in the processing process, and further the problems of great loss of volatile components in the flavor, damage of heat-sensitive substances, low aroma fidelity of products, quality reduction and the like are caused.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention provides a method for extracting an old medicine orange spice, which is characterized by comprising the following steps of:
(1) Mixing old orange with water, performing cell disruption ultrasonic extraction on the obtained mixed solution at room temperature, filtering, refrigerating and settling the obtained filtrate, and performing suction filtration by using a Buchner funnel to obtain an old orange primary extraction solution;
(2) Separating the primary extract of the old medicine orange obtained in the step (1) at room temperature through a microfiltration membrane component, and collecting filtrate to obtain a microfiltration membrane permeate of the old medicine orange;
(3) Separating the old medicine orange microfiltration membrane permeate obtained in the step (2) by using an ultrafiltration membrane component, sequentially filtering by using ultrafiltration membranes with the molecular weight cutoff of 30KDa, 10KDa and 5KDa at room temperature, and collecting filtrate to obtain the old medicine orange ultrafiltration membrane permeate;
(4) Separating the old medicine orange ultrafiltration membrane permeate obtained in the step (3) at room temperature through a nanofiltration membrane component, and collecting trapped fluid to obtain old medicine orange nanofiltration membrane trapped fluid;
(5) And (5) placing the nanofiltration membrane trapped fluid of the old medicine orange obtained in the step (4) into a concentration chamber of a forward membrane concentration device, performing multi-stage forward concentration at room temperature, and collecting the concentrated fluid when the concentrated fluid is concentrated to 55% of solid content of liquid, so as to obtain the old medicine orange spice.
Preferably, the old medicinal orange is an old medicinal orange, and is selected from cumquat fruits which are pickled for more than 3 years.
Preferably, the gauze is 400-500 meshes in size.
Preferably, the temperature for the refrigeration in step (1) is 4 ℃.
Preferably, the specific ultrasonic extraction conditions in step (1) are as follows: the ultrasonic power is 300-500W, the mass ratio of the old medicine orange to water is 1-1; performing ultrasonic extraction for the second time for 1-2h.
Preferably, the specific separation conditions in step (2) are as follows: the molecular weight cut-off of the used microfiltration membrane component is 200-300nm, the solid content of the primary extract of the old medicine orange is adjusted to 4-8% before microfiltration, and the primary extract is subjected to microfiltration for 50-90min under 0.08-0.12MPa at room temperature.
Preferably, the specific separation conditions in step (3) are as follows: adjusting the operating pressure to 0.1-0.5MPa according to the pressure resistance and the upper flux limit of the ultrafiltration membrane and the actual flux in the ultrafiltration process, firstly filtering by using the ultrafiltration membrane with the molecular weight cutoff of 30KDa, and adding pure water for continuous filtration (V) when the volume of the trapped liquid is obviously reduced, the flow speed of the filtered liquid is obviously reduced, and the solid content of the trapped liquid is 60-65 percent Pure water =0.5V Filtrate ) Repeating for 1-3 times, replacing the filter membrane assembly, filtering with ultrafiltration membrane with cut-off molecular weight of 10KDa, adding pure water for continuous filtration (V) when the volume of cut-off liquid is reduced, the flow rate of filtrate is reduced, and the solid content of cut-off liquid is 55-60% Pure water =0.5V Filtrate ) Repeating for 1-3 times, replacing the filter membrane assembly, filtering with ultrafiltration membrane with cut-off molecular weight of 5KDa, adding pure water for continuous filtration (V) when the volume of cut-off liquid is reduced, the flow rate of filtrate is reduced, and the solid content of cut-off liquid is 50% -55% Pure water =0.5V Filtrate ) Repeating for 1-3 times, stopping, and collecting filtrate for use.
Preferably, in the step (4), the nanofiltration membrane separation conditions are as follows: nanofiltration is carried out by using a 100-200Da nanofiltration membrane component NF2, pressure is properly regulated and controlled according to the pressure resistance and the upper flux limit of a membrane material and the actual flux in the nanofiltration process, the pressure is less than or equal to 0.4MPa, and when the volume of trapped liquid is obviously reduced, the flow speed of filtrate is obviously reduced, and the solid content of the trapped liquid is 15-20%, the trapped liquid is collected for standby application.
Preferably, the forward concentration conditions in step (5) are as follows: taking a hollow fiber forward concentration membrane as a separation membrane, controlling the flow rate of an extracting solution and a drawing agent within 1L/min, taking high fructose syrup as the drawing agent, and performing 2-4-stage type recycling drawing agent concentration at room temperature. That is, the drawing liquid used in the last stage is pure high fructose syrup, when the drawing agent loses the drawing capability, the concentration is stopped, and the used drawing liquid is used for the penultimate stage concentration of the next batch of samples, so as to circulate.
The second aspect of the invention provides the use of the old medicinal orange flavor of the first aspect, the old medicinal orange flavor is diluted by ethanol and then uniformly sprayed in tobacco shreds to be used as a natural tobacco flavor, and the prepared cigarette has unique style characteristics of fruit flavor, orange peel flavor, fresh and sweet mouthfeel and the like, can improve throat irritation and aftertaste, increase mouth moistening feeling, body fluid sweet feeling and comfortable feeling, and improve the quality of the cigarette.
Preferably, the mass ratio of the old orange spice to the cut tobacco is 1-10.
The invention has the following functions:
in the step (1), cell disruption ultrasonic extraction is carried out on the traditional Chinese medicine orange so as to achieve the purpose of fully disrupting cell walls of the orange peel of the traditional Chinese medicine orange. In the ultrasonic treatment process, the propagation of ultrasonic waves in the extraction medium can enable the medium to vibrate in the propagation space of the medium, so that materials are collided and rubbed with each other, micro bubbles dissolved in the medium are increased under the action of the ultrasonic waves to form a resonant cavity, then the resonant cavity is closed instantly, the aged medicine orange peel cells can be broken instantly, and effective components such as intracellular volatile oil, flavonoids and the like are dissolved in a solvent. The extracting solution is refrigerated at 4 ℃ and is filtered by a Buchner funnel after sedimentation treatment, and impurities in the pretreated feed liquid are reduced, thereby being beneficial to reducing the problem of membrane pollution in the microfiltration process in the next step.
In the step (2), the old medicinal orange primary extract contains a large amount of plant tissues, organs, macromolecular substances and the like, mainly suspended substances, insoluble starch, cellulose, pectin, protein and other substances, the substances have large molecular weights (1500kD to 2500kD) but have no aroma generating activity, exist in water in a colloid form, cause poor clarity and unstable quality of products, are easy to precipitate along with the change of storage time, have appearance changes such as layering and the like, cause the problems of difficult control of product quality and the like, and bring negative effects in the cigarette smoking process. The old medicine orange primary extract is separated and purified through a microfiltration membrane, so that suspended impurities and macromolecular substances can be effectively removed. The microfiltration membrane of 200-300nm has good retention effect on suspended impurities, insoluble protein with large molecules and large particle size, pectin and cellulose in the extract, and hardly has retention effect on aroma substances, flavone and inorganic acid salts.
In the step (3), the relative molecular weight range of molecules intercepted by the ultrafiltration membrane is between 500 and 50000. The relative molecular mass of the effective components of the natural perfume is mostly not more than 1000, and the relative molecular mass of the ineffective components is more than 50000. The permeate of the old medicine orange microfiltration membrane is separated and refined by an ultrafiltration membrane, and substances which can bring cigarette miscellaneous gas and irritation are further removed. The separation process of the ultrafiltration membrane is a sieve pore separation process, and is a method for separating according to the size difference of the molecules of the separated substances. The invention can further remove macromolecular substances such as protein, pectin, cellulose, pigment, enzyme and the like by using the ultrafiltration membrane of 30 KDa. 10 The kDa ultrafiltration membrane can effectively filter proteins and most of polysaccharide components, and the 5kDa ultrafiltration membrane has strong retention effect on polysaccharide substances. The regulation of polysaccharide and protein in the extract can be realized through 10kDa and 5kDa membranes. The 30kDa, 10kDa and 5kDa membranes have little effect on intercepting volatile flavor components, inorganic ions, nicotine and other small molecules. The combination of multi-stage ultrafiltration membrane separation has high-efficiency removal effect on different macromolecular impurities with large molecular weight in the permeate of the old medicine orange microfiltration membrane.
In the step (4), nanofiltration (NF) is a novel pressure-driven membrane separation process, and the nanofiltration membrane has different retention rates on ions and small organic molecules of 200-2000 Da. A large amount of salt is added in the processing process of pickling the old medicinal orange, the content of chloride ions is not more than 0.8 percent according to the current tobacco industry standard, and the sensory quality of cigarettes can be reduced due to the overhigh content of chloride ions in tobacco. In addition, old preserved orange contains nitrate and nitrite, and generates nitrosamine, oxynitride and the like when the cigarette is burnt, and the substances can cause excessive smoke and miscellaneous gases, influence the sensory quality and simultaneously harm the health of human bodies. Therefore, it is necessary to remove chloride ions, nitrate and nitrite in the extract efficiently and conveniently. The NF2 nanofiltration membrane has strong interception effect on flavonoid and carbohydrate in the old medicinal orange extract; the aromatic substance has strong retention effect on aroma components; there was no significant retention of inorganic salts characterized by chloride, nitrate and nitrite. Trapped liquid formed by the old medicine orange extracting solution through the NF2 nanofiltration membrane contains flavonoid, sugar and aromatic substances and almost no inorganic salt, so the NF2 nanofiltration membrane can realize the removal of inorganic salt chloride, nitrate and nitrite in the extracting solution.
In the step (5), the forward concentration technology is a membrane treatment technology taking solution osmotic pressure as water transmission driving force, has the characteristics of low energy consumption and light membrane pollution, and is widely applied to the fields of water treatment, food and the like. The process has no phase change, low energy consumption, no consumption of chemical reagents and no pollution to products, and the separation process is carried out in a closed loop at normal temperature, so that the aroma components of the old medicine orange cannot be damaged, and the fidelity of aroma substances is improved. The high fructose corn syrup is preferably selected as the drawing agent for forward membrane concentration of the extracting solution, and has the advantages of higher osmotic pressure, no toxicity, no harm, pure nature, enhancement of sensory quality, coordination with natural tobacco fragrance, enhancement of flue gas sweetness and the like.
The technical scheme can be freely combined on the premise of no contradiction.
The invention has the following beneficial effects:
1. the extraction method of the old medicine orange spice provided by the invention adopts the technology of combining microfiltration, ultrafiltration and nanofiltration, and preferably selects a membrane combination process of a microfiltration membrane (200-300 nm), an ultrafiltration membrane (30 KDa, 10KDa, 5 KDa) and a nanofiltration membrane (100-200 Da). The components of the primary extract of the old medicinal orange are accurately separated and regulated according to the molecular weight selectivity, and starch, cellulose, pectin, protein, pigment, enzyme and the like which can bring cigarette miscellaneous gas and macromolecular impurities which can negatively influence cigarette smoking are effectively separated and removed at room temperature, and meanwhile, the damage of heat sensitivity and aroma components is avoided. Meanwhile, the invention also unexpectedly discovers that inorganic salts such as inorganic salt chloride, nitrate, nitrite and the like which seriously affect the sensory quality of cigarette smoking and the health of human bodies can be effectively removed by adopting the nanofiltration membrane process, thereby avoiding the generation of impure gas of cigarettes and greatly improving the cigarette smoking quality.
2. The invention adopts a multi-stage type recycling drawing agent mode to carry out forward membrane concentration, the required drawing agent dosage is less, the concentration time is shorter, the high fructose syrup drawing agent is adopted to improve the sensory quality of the tobacco flavor, and the concentration process is higher in cost performance. Meanwhile, a multistage membrane separation and coupling forward membrane concentration process is adopted, and macromolecular impurities in feed liquid can be removed through the filtration of the multistage membranes, so that the pollution problem of the forward membranes is solved, the service life of the membranes is prolonged, and the product cost is reduced.
3. The invention adopts a membrane separation membrane concentration coupling technology, can effectively solve the problems of high energy consumption, low yield and low control stability in the traditional extraction solution separation and concentration, and can realize fine separation and low-temperature concentration and reduce energy consumption. The energy consumption is far less than that of the traditional separation and concentration. The membrane separation membrane concentration coupling technology is a pure physical process, does not generate phase change in the process, consumes less energy, does not consume harmful chemical reagents, does not pollute products, and does not need heating and freezing. The method has little influence on environment, and can effectively reduce CO 2 The release amount is a green and environment-friendly treatment method.
4. According to the invention, the tobacco flavor prepared from the old medicine orange is applied to the flavoring process of the cut tobacco of the cigarette for the first time through a unique extraction method, and the cigarette flavor has unique flavor of fruit and orange peel, fresh, sweet and sweet taste and other style characteristics, can improve the stimulation and aftertaste of the throat, increase the mouth moistening feeling, the body fluid sweet feeling and the comfortable feeling, and has the effects of high smell, high fidelity and cigarette quality improvement. This effect cannot be expected by the person skilled in the art. The invention enriches the natural sources and types of tobacco essence and flavor, invents the old medicine orange flavor product with adjustable and controllable components, high fragrance, high fidelity and wide applicability, and meets the personalized and diversified requirements of consumers.
5. The method for extracting the old medicine orange spice has the advantages of short process period, environmental protection, safety, convenience for large-scale and industrial production and higher economic benefit.
6. According to the invention, the old medicine orange spice is diluted by ethanol for the first time and then uniformly sprayed into tobacco shreds to be used as a natural tobacco spice, and the prepared cigarette has the unique style characteristics of fruit aroma, orange peel aroma, fresh, sweet and sweet mouthfeel and the like, can improve the stimulation and aftertaste of the throat, increase the mouth moistening feeling, the sweet feeling and the comfortable feeling, and improve the quality of the cigarette.
Drawings
Fig. 1 is a graph showing the flavor pattern of cigarettes in which the old orange flavor obtained in example 1, comparative example 1, and comparative example 2 was added in example 5 of the present invention.
FIG. 2 is a net graph of taste characteristics of cigarettes of example 5 of the present invention, to which the old orange flavor obtained in example 1, comparative example 1, and comparative example 2 was added, during smoking.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A method for extracting an old medicine orange spice comprises the following steps:
(1) 1kg of commercially available aged orange is taken, and 5kg of purified water is added; carrying out cell disruption ultrasonic extraction twice at room temperature, wherein the first ultrasonic extraction time is 3h; the time of the second ultrasonic extraction is 2h; mixing the two extractive solutions, filtering with 400 mesh gauze to obtain filtrate, refrigerating at 4 deg.C for 15 hr for settling, and vacuum filtering with Buchner funnel to obtain the primary extractive solution.
(2) Separating the primary extract of the old orange obtained in the step (1) at room temperature by a 200nm microfiltration membrane module, adjusting the solid content of the feed liquid to be 6%, carrying out microfiltration under 0.11MPa for 80min, wherein the average membrane flux value is 17.16L/(m) 2 H), collecting the filtrate to obtain the old medicine orange microfiltration membrane permeate.
(3) Separating 4kg of old medicine orange microfiltration membrane permeate obtained in the step (2) through an ultrafiltration membrane module, adjusting the operating pressure to 0.3MPa at room temperature according to the upper limit of pressure resistance and flux of a membrane material and the actual flux in the ultrafiltration process, filtering with an ultrafiltration membrane with the molecular weight cutoff of 30KDa, adding 2kg of pure water for continuous filtration when the volume of the retentate is obviously reduced and the flow rate of the filtrate is obviously reduced and the solid content of the retentate is 62%, repeating the steps for 2 times, then replacing the membrane module, performing filtration with 10KDa ultrafiltration membrane, when the volume of the retentate is obviously reduced and the flow rate of the filtrate is obviously reduced and the solid content of the retentate is 57%, adding 2kg of pure water for continuous filtration, repeating the steps for 2 times, then replacing the ultrafiltration membrane module, performing filtration with 5KDa, when the volume of the retentate is obviously reduced, the flow rate of the filtrate is obviously reduced and the solid content of the retentate is 52%, continuing the filtration with adding 2kg of pure water, repeating the steps for 2 times, stopping, and collecting the filtrate for later use, thereby obtaining the old medicine orange permeate.
(4) And (3) allowing the filtrate of the old medicine orange ultrafiltration membrane obtained in the step (3) to pass through a 150Da nanofiltration membrane NF2 component, performing nanofiltration at room temperature, regulating and controlling the pressure to be 0.3MPa according to the pressure resistance and the upper limit of flux of a membrane material and the actual flux in the nanofiltration process, and collecting the trapped liquid when the volume of the trapped liquid is obviously reduced, the solid content of the trapped liquid is 18% after the flow speed of the filtrate is obviously reduced, so as to obtain the trapped liquid of the old medicine orange nanofiltration membrane.
(5) And (5) placing the old medicine orange nanofiltration membrane trapped fluid obtained in the step (4) into a concentration chamber of a forward membrane concentration device, taking a hollow fiber forward concentration membrane as a separation membrane, controlling the flow rates of an extracting solution and an extracting agent to be 0.6L/min, taking high fructose corn syrup as an extracting agent, and performing 3-section forward concentration at room temperature. That is, the drawing liquid used in the third stage is pure fructose-glucose syrup, when the drawing agent loses the drawing capability, the concentration is stopped, and the used drawing liquid is used for the second-stage concentration of the next batch of samples, so that the circulation is realized. And when the concentrated solution is concentrated to the solid content of 55%, collecting the concentrated solution for later use to obtain the old medicine orange spice.
Comparative example 1
A method for extracting old medicine orange spice comprises directly performing hot reflux extraction twice with 5 times of pure water, and directly evaporating and concentrating the extractive solution at 65 deg.C and 80kPa without membrane filtration until the solid content is 55% to obtain the old medicine orange spice.
Comparative example 2
Compared with the method in the example 1, the method for extracting the aged medicinal orange spice comprises the following steps of 1, adding 95% ethanol with the volume being 3 times of that of the extract, refrigerating at 4 ℃ for 24 hours for sedimentation treatment, performing suction filtration by using a Buchner funnel, and performing evaporation concentration on the obtained filtrate at 65 ℃ and 80kPa until the solid content is 55% to obtain the alcohol-precipitated aged medicinal orange spice.
Example 2
The tests for detecting macromolecular impurities, nitrate, nitrite and inorganic salt chloride by comparing the old medicine orange spice extract obtained by the microfiltration, ultrafiltration, nanofiltration and forward concentration coupling technology with the old medicine orange spice extract obtained by the conventional process are as follows:
the old orange flavors prepared in example 1, comparative example 1 and comparative example 2 of the present invention were analyzed by AA3 continuous flow analyzer (Bran luebe, germany), ion chromatograph (srm fly, usa), automatic potentiometric titrator (HACH, usa) according to the related standards: the determination of the starch content refers to a YC/T216-2007 method, the determination of the protein content refers to a YC/T249-2008 method, the determination of the pectin content refers to a YC/T346-2010 method, and the determination of the cellulose content refers to a YC/T347-2010 method. The content of nitrate and nitrite is measured according to the method GB5009.33-2016, and the content of inorganic salt chloride is measured according to the method GB 5009.44-2016. The results are shown in table 1:
therefore, the method can effectively remove insoluble macromolecular impurities such as starch, cellulose, pectin, protein and the like in the primary extract of the old orange by adopting a separation technology combining microfiltration, ultrafiltration and nanofiltration, can also effectively remove inorganic salt chloride, nitrate, nitrite and the like which seriously affect the sensory quality of cigarette smoking and the health of human bodies, avoids the generation of impure gas and irritation of cigarettes, and greatly improves the cigarette smoking quality. In contrast, after evaporation concentration of the traditional hot reflux extraction liquid, large molecular impurities exist, and part of aroma effective components are lost due to the evaporation concentration under the condition of higher temperature. Macromolecular substances of the traditional Chinese medicine orange spice after ethanol precipitation are slightly reduced, which shows that the ethanol precipitation can remove a part of impurities, but the removal effect is far inferior to that of the traditional Chinese medicine orange spice prepared by the method adopting microfiltration, ultrafiltration, nanofiltration and membrane concentration coupling technologies, and in addition, the ethanol precipitation method cannot remove inorganic salt chloride, nitrate and nitrite.
Example 3
The old orange flavor prepared in example 1 was detected by gas chromatography-mass spectrometry combined with GC-MS analysis:
(1) Gas chromatography conditions: a chromatographic column: DB-5MS quartz capillary column (30 m × 0.25mm,0.25 μm); temperature programming: the initial temperature is 60 ℃, the temperature is kept for 1min, the temperature is raised to 170 ℃ at the speed of 8 ℃/min, and the temperature is kept for 3min; raising the temperature to 260 ℃ at the speed of 12 ℃/min, and keeping the temperature for 18min; sample inlet temperature: 200 ℃; temperature of the column box: 60 ℃; sample introduction mode: shunting; column flow rate: 1mL/min; purging flow rate: 3 mL/min; the split ratio is as follows: 5, 1; carrier gas: high purity helium; sample introduction amount: 1 mu L of the solution; solvent retardation: and 2min.
(2) Mass spectrum conditions: an ionization mode: EI; electron energy: 70eV; interface temperature: 250 ℃; ion source temperature: 200 ℃; the collection mode is as follows: scan; scanning range: 40-500amu.
(3) And (3) qualitative analysis: by using the mass spectrum as a detector and combining the mass spectrum with gas chromatography, and utilizing NIST spectral library for retrieval, the aroma components in the particle aroma-endowed cigarette sample can be identified in a short time for qualitative analysis.
(4) Quantitative analysis: the internal standard substance is 99% of naphthalene, and the semi-quantitative analysis is carried out on the aroma components by adopting an internal standard method. The content of the aroma component was calculated as follows.
In the formula:
X-content of each compound,. Mu.g/g;As-integrated peak area for each compound;Ai-integrated peak area of internal standard substance;mi-mass of internal standard substance, g;M-sample mass of aromatised cigarettes, g.
The contents of the specific components are shown in Table 2.
As is clear from table 2, the old orange flavor prepared in example 1 contains a large amount of terpene compounds, and these components impart citrus, grapefruit, licorice, and spicy notes, and have strong effects on the taste of fine and soft smoke, improvement of aftertaste, and reduction of irritation. In addition, alcohol and aldehyde compounds have special aromatic smell, so that the richness of the smoke can be effectively increased. The contents of ester and carboxylic acid aroma substances are also high, and the substances can adjust the pH value of tobacco, bring natural sour fruit aroma and increase the richness and harmony of smoke.
Example 4
In order to investigate the influence of different processes on the aroma substances and the loss rate of the aroma components, the old medicine orange flavors prepared in the embodiment 1, the comparative example 1 and the comparative example 2 are respectively subjected to aroma component analysis, and the different types of contents of the aroma substances and the total amount of the aroma substances are subjected to statistical analysis. The results are shown in Table 3:
the result shows that the total amount of the aroma substances (3459.247 mug/g) in the old medicinal orange spice obtained by adopting the separation technology combining microfiltration, ultrafiltration and nanofiltration is obviously higher than that of the comparative example 1 (1101.311 mug/g) and that of the comparative example 2 (1179.639 mug/g), which is caused by the loss of a large amount of aroma components in the long-time heating and concentration process, so that the content of the aroma substances is low, the aroma concentration is reduced, and the natural fragrance is lost. The invention adopts the microfiltration, ultrafiltration, nanofiltration and membrane concentration coupling technology, has low treatment temperature at room temperature, and has the advantages of being beneficial to maximally preserving the content of aroma substances, keeping the natural and fresh and sweet fruity note of the old orange and the like.
Example 5
Sensory evaluation of cigarettes: the old medicine orange flavor prepared in the embodiment 1, the comparative example 1 and the comparative example 2 of the invention is respectively diluted by 0.5 percent of tobacco shred of each cigarette, and is respectively injected into the cigarettes by adopting a flavor and flavor injection machine, so as to respectively obtain cigarettes, namely the embodiment 1 (50 cigarettes), cigarettes, namely the comparative example 1 (50 cigarettes), and cigarettes, namely the comparative example 2 (50 cigarettes). Blank cigarettes (50 cigarettes) without added flavour were used as control. All the cigarettes are placed in a constant-temperature constant-humidity box (the temperature is 22 +/-1 ℃, and the humidity is 60 +/-2%) to be balanced for 48 hours, and the cigarettes are subjected to smoking evaluation by experts with cigarette smoking evaluation qualification according to GB5606.4-2005 cigarette part 4 sensory technical requirements. The results of the smoke panel are shown in table 4:
the results show that: the old medicine orange spice obtained by the invention has unique style characteristics of fruit aroma, orange peel aroma, fresh sweet and sweet taste and the like, improves throat stimulation, increases mouth moistening feeling, body fluid generating feeling and comfortable feeling, and has the effects of high smell, high fidelity and improvement on smoking quality of heated cigarettes.
Referring to the sensory evaluation results of example 1, comparative example 1 and comparative example 2 in table 4, the mesh pattern of the aroma style is shown in fig. 1, and the mesh pattern of the taste characteristics is shown in fig. 2.
As can be seen from table 4 and fig. 1 and 2, the cigarette added with the old medicine orange flavor prepared by the invention has remarkable smelly flavor styles of fruit flavor and orange peel flavor, and prominent fresh, sweet and sweet taste characteristics during smoking. The old orange flavors of comparative examples 1 and 2 do not have the above-mentioned good effects because the taste characteristics are greatly lost during the extraction or concentration process by heating at high temperature. Meanwhile, in the process of extracting the old medicinal orange spice, the nanofiltration separation technology is adopted, so that inorganic salts such as inorganic salt chloride, nitrate, nitrite and the like which seriously affect the smoking sensory quality of the cigarette are effectively removed, the impure gas is obviously reduced, the irritation is greatly improved when the cigarette added with the old medicinal orange spice prepared by the invention is smoked, and the smoking quality of the cigarette is greatly improved. The old orange flavors in comparative examples 1 and 2 have no such good effects.
Claims (7)
1. The method for extracting the traditional Chinese medicine orange spice is characterized by comprising the following steps of:
(1) Mixing old orange with water, performing cell disruption ultrasonic extraction on the obtained mixed solution at room temperature, filtering, refrigerating and settling the obtained filtrate, and performing suction filtration by using a Buchner funnel to obtain an old orange primary extraction solution; the old medicine orange is fruit of kumquat of Rutaceae, by picking and cleaning, boiling with water, removing astringent taste, adding appropriate amount of salt, sugar and fructus crataegi, glycyrrhrizae radix, herba Menthae and cortex Cinnamomi, and pickling until the surface is brown and the kumquat is flat and round;
(2) Separating the primary extract of the old medicine orange obtained in the step (1) at room temperature through a microfiltration membrane component, and collecting filtrate to obtain a microfiltration membrane permeate of the old medicine orange; the specific conditions for the separation are as follows: the molecular weight cut-off of the used microfiltration membrane component is 200-300nm, the solid content of the primary extract of the old medicine orange is adjusted to 4-8% before microfiltration, and the primary extract is subjected to microfiltration for 50-90min under 0.08-0.12MPa at room temperature;
(3) Separating the old medicine orange microfiltration membrane permeate obtained in the step (2) by an ultrafiltration membrane component, sequentially filtering by ultrafiltration membranes with the molecular weight cut-off of 30KDa, 10KDa and 5KDa at room temperature, and collecting filtrate to obtain the old medicine orange ultrafiltration membrane permeate;
(4) Separating the permeation liquid of the old medicine orange ultrafiltration membrane obtained in the step (3) at room temperature through a nanofiltration membrane component, and collecting trapped liquid to obtain old medicine orange nanofiltration membrane trapped liquid; the specific conditions for the separation are as follows: nanofiltration is carried out by using a 100-200Da nanofiltration membrane component NF2, pressure is properly regulated and controlled according to the pressure resistance and the upper flux limit of a membrane material and the actual flux in the nanofiltration process, the pressure is less than or equal to 0.4MPa, and when the volume of trapped liquid is obviously reduced, the flow velocity of filtrate is obviously reduced, and the solid content of the trapped liquid is 15-20%, the trapped liquid is collected for standby application;
(5) And (3) placing the nanofiltration membrane trapped fluid of the old medicine orange obtained in the step (4) into a concentration chamber of a forward membrane concentration device, carrying out multi-stage forward concentration at room temperature, taking a hollow fiber forward concentration membrane as a separation membrane, controlling the flow rate of an extracting solution and an extracting agent within 1L/min, taking high fructose syrup as an extracting agent, and carrying out 2-4-stage cyclic use of the extracting agent for concentration at room temperature, namely, the extracting solution used in the last stage is pure high fructose syrup, stopping concentration when the extracting agent loses the extracting capability, using the used extracting solution for the penultimate second stage concentration of a next batch of samples, circulating the solution, and collecting the concentrated solution when the solid content of the concentrated solution is 55%, thus obtaining the old medicine orange perfume.
2. The method for extracting aged medicinal orange flavor according to claim 1, wherein the aged medicinal orange is aged medicinal orange, specifically selected from preserved cumquat fruit for more than 3 years.
3. The method for extracting spice from old orange as claimed in claim 1, wherein the specific ultrasonic extraction conditions in step (1) are as follows: the ultrasonic power is 300-500W, the mass ratio of the old medicine orange to water is 1-1; performing ultrasonic extraction for 1-2h.
4. The method for extracting spice of old medicine orange according to claim 1, wherein the specific separation conditions in the step (3) are as follows: adjusting the operation pressure to 0.1-0.5MPa according to the pressure resistance and the upper flux limit of the ultrafiltration membrane and the actual flux of the ultrafiltration process, filtering with the ultrafiltration membrane with the molecular weight cutoff of 30KDa, adding pure water for continuous filtration when the volume of the cutoff liquid is obviously reduced, the flow speed of the filtrate is obviously reduced, and the solid content of the cutoff liquid is 60% -65%, and V Pure water =0.5V Filtrate Repeating for 1-3 times, replacing the filter membrane component, filtering with ultrafiltration membrane with cut-off molecular weight of 10KDa, adding pure water for continuous filtration when the volume of cut-off liquid is obviously reduced, the flow speed of filtrate is obviously reduced, and the solid content of cut-off liquid is 55% -60%, and V Pure water =0.5V Filtrate Repeating for 1-3 times, replacing the filter membrane assembly, filtering with ultrafiltration membrane with cut-off molecular weight of 5KDa, adding pure water for continuous filtration when the volume of cut-off liquid is reduced, the flow rate of filtrate is reduced, and the solid content of cut-off liquid is 50% -55%, and filtering Pure water =0.5V Filtrate Repeating for 1-3 times, stopping, and collecting filtrate for use.
5. The method for extracting spice of old medicine orange as claimed in claim 1, wherein the filtering in step (1) is performed by gauze with a specification of 400-500 meshes.
6. The use of the old medicinal orange flavor obtained by the method of claim 1 as a natural tobacco flavor by diluting the old medicinal orange flavor with ethanol and uniformly spraying the diluted old medicinal orange flavor in tobacco shreds.
7. The use as claimed in claim 6, wherein the mass ratio of the old medicinal orange spice to the cut tobacco is 1-10.
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