CN114886147A - Extraction method of old medicine orange spice and application of old medicine orange spice in cigarettes - Google Patents
Extraction method of old medicine orange spice and application of old medicine orange spice in cigarettes Download PDFInfo
- Publication number
- CN114886147A CN114886147A CN202210655782.7A CN202210655782A CN114886147A CN 114886147 A CN114886147 A CN 114886147A CN 202210655782 A CN202210655782 A CN 202210655782A CN 114886147 A CN114886147 A CN 114886147A
- Authority
- CN
- China
- Prior art keywords
- orange
- old
- membrane
- medicine
- spice
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Seasonings (AREA)
Abstract
The invention provides a method for extracting an old medicine orange spice, which is characterized in that multistage membrane separation is carried out on an initial extract of the old medicine orange by adopting a separation technology combining microfiltration, ultrafiltration and nanofiltration, and the initial extract is concentrated by 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 water extract of the old medicine orange has unique aroma characteristics of fruit aroma, orange peel aroma and the like. However, although the traditional separation means such as water extraction and alcohol precipitation, filter screen filtration and the like which are used at present can remove part of suspended impurities and insoluble macromolecular impurities in the old medicine orange extract, when the obtained old medicine orange flavor 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 old medicine orange flavor cannot 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, carrying out multi-stage forward concentration at room temperature, and collecting the concentrated solution when the concentrated solution is concentrated to 55% of the solid content of the 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.
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 orange to the water is 1:5-1:10, the extraction times are two, the first ultrasonic extraction is carried out, and the extraction time is 2-3 h; performing ultrasonic extraction for the second time for 1-2 h.
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 crude extract of the old orange is adjusted to 4-8% before microfiltration, and the microfiltration is carried out for 50-90min under the room temperature condition of 0.08-0.12 MPa.
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 limit of the flux 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, when the volume of the trapped fluid is obviously reduced, the flow rate of the filtered fluid is obviously reduced, and the solid content of the trapped fluid is 60% -65%, adding pure water for continuous filtration (V pure water is 0.5V filtrate), repeating for 1-3 times, replacing the filter membrane component, then filtering by using the ultrafiltration membrane with the molecular weight cutoff of 10KDa, when the volume of the trapped fluid is obviously reduced, the flow rate of the filtered fluid is obviously reduced, and the solid content of the trapped fluid is 55% -60%, then adding pure water for continuous filtration (V pure water is 0.5V filtrate), repeating for 1-3 times, stopping, replacing the filter membrane component, then filtering by using the ultrafiltration membrane with the molecular weight cutoff of 5KDa, when the volume of the trapped fluid is obviously reduced, and the flow rate of the filtered fluid is obviously reduced, and when the solid content of the trapped liquid is 50% -55%, adding pure water, continuously filtering (0.5V of filtrate) and repeating for 1-3 times, stopping and collecting the filtrate for later 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 the 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 filtered liquid 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 corn 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 capacity, the concentration is stopped, and the used drawing liquid is used for the penultimate stage concentration of the next batch of samples, so that the cycle is realized.
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 medicinal orange spice to the cut tobacco is 1:1000-10: 1000.
The invention has the following functions:
in the step (1), the traditional Chinese medicine orange is subjected to cell disruption ultrasonic extraction so as to achieve the purpose of fully disrupting cell walls of the traditional Chinese medicine orange peel. 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 primary extract of the old medicine orange contains a large amount of plant tissues, organs, macromolecular substances and the like, mainly suspended substances, insoluble starch, cellulose, pectin, protein and other substances which have very large molecular weight (1500 kD-2500 kD) but no aroma-causing activity, and the primary extract exists in water in the form of colloid, so that the product has poor clarity and unstable quality, is easy to precipitate along with the change of storage time, has appearance changes such as layering and the like, causes the problems of difficult control of the product quality and the like, and brings 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 200-fold 300nm microfiltration membrane has good interception effect on suspended impurities, insoluble protein, pectin and cellulose with larger molecules and larger grain sizes in the extracting solution, and hardly has interception effect on aroma substances, flavone and inorganic acid salts.
In step (3), the relative molecular weight of the molecules intercepted by the ultrafiltration membrane is in the range of 500-50000. 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. The 10kDa 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 function on flavonoid and carbohydrate in the old medicinal orange extract; the strong retention effect on aroma components is achieved; there was no significant retention of inorganic salts characterized by chloride, nitrate and nitrite. Trapped fluid formed by the aged 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 components of the fragrance of the old medicine orange cannot be damaged, and the fidelity of the fragrant substances is improved. The high fructose corn syrup is preferably selected as a drawing agent for forward membrane concentration of the extracting solution, and has the advantages of higher osmotic pressure, no toxicity, no harm, pure nature, sense quality improvement, harmony with natural tobacco fragrance, smoke sweetness improvement 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-. 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 a 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 medicinal 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 tobacco flavor has unique flavor of fruit and orange peel, fresh sweet and sweet mouthfeel 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 the 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. The old medicinal orange spice is diluted by ethanol for the first time and then uniformly sprayed into tobacco shreds to be used as a natural cigarette spice, and the prepared cigarette has the unique style characteristics of fruit aroma, orange peel aroma, fresh and sweet mouthfeel, aftertaste and the like, can improve throat irritation and aftertaste, increase mouth moistening, body fluid and sweet feeling and 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 3 h; the second ultrasonic extraction time is 2 hours; 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 the old medicine orange microfiltration membrane permeate obtained in the step (2) by an ultrafiltration membrane component, adjusting the operating pressure to 0.3MPa according to the upper limit of the pressure resistance and the flux of a membrane material and the actual flux in the ultrafiltration process at room temperature, filtering by using 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 component, carrying out 10KDa ultrafiltration membrane filtration, adding 2kg of pure water for continuous filtration 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 57%, repeating the steps for 2 times, replacing the membrane component for 5KDa ultrafiltration membrane filtration, 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%, adding 2kg of pure water for continuous filtration, repeating for 2 times, and collecting filtrate to obtain filtrate of the old medicine orange ultrafiltration membrane.
(4) And (3) allowing the filtrate of the old 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 the membrane material and the actual flux in the nanofiltration process, and collecting the trapped fluid when the volume of the trapped fluid is obviously reduced, the flow speed of the filtrate is obviously reduced, and the solid content of the trapped fluid is 18% to obtain the trapped fluid of the old orange nanofiltration membrane.
(5) And (4) 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 rate of an extracting solution and a drawing agent to be 0.6L/min, taking high fructose corn syrup as a drawing 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 55 percent of solid content of the liquid, collecting the concentrated solution for later use to obtain the old medicinal 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 subjected to the following procedures using 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:
TABLE 1 comparison of macromolecular impurities and chloride contents for different processes
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 the conventional hot reflux extraction liquid is evaporated and concentrated, large molecular impurities are abundant, and part of aroma effective components are lost due to the evaporation and concentration under the condition of higher temperature. Macromolecular substances of the old 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 old medicine orange spice which adopts the microfiltration, ultrafiltration, nanofiltration and membrane concentration coupling technology, and in addition, the ethanol precipitation method can not 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 (30m × 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 3 min; raising the temperature to 260 ℃ at the speed of 12 ℃/min, and keeping the temperature for 18 min; sample inlet temperature: 200 ℃; temperature of the column box: 60 ℃; sample introduction mode: shunting; column flow rate: 1 mL/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 2 min.
(2) Mass spectrum conditions: an ionization mode: EI; electron energy: 70 eV; interface temperature: 250 ℃; ion source temperature: 200 ℃; the collection mode is as follows: scan; scanning range: 40-500 amu.
(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 fragrant components are subjected to semi-quantitative analysis by adopting an internal standard method. The content of the aroma component was calculated as follows.
In the formula:
x-content per compound,. mu.g/g; as-integrated peak area per compound; ai-integrated peak area of internal standard substance; mi-mass of internal standard substance, g; m-sample mass of aromatized cigarette, g.
The contents of the specific components are shown in Table 2.
Table 2 volatile components and relative amounts analysis of the aged medicinal orange flavor prepared in example 1
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:
TABLE 3 statistics of the content of different types of aroma components
The result shows that the total amount of the aroma substances (3459.247 mu g/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 mu g/g) and the comparative example 2(1179.639 mu g/g), because a large amount of aroma components are lost in the long-time heating and concentration process, 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%) and balanced for 48 hours, and the cigarettes are smoked by experts qualified for cigarette smoking according to the technical requirements of GB5606.4-2005 cigarette No. 4 part sensory technology. The results of the smoke panel are shown in table 4:
TABLE 4 old medicine orange flavor cigarette smoking evaluation result analysis
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 (10)
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;
(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, carrying out multi-stage forward concentration at room temperature, and collecting the concentrated solution when the concentrated solution is concentrated to 55% of the solid content of the liquid, so as to obtain the old medicine orange spice.
2. The extraction method according to claim 1, wherein the old orange is aged orange, and is selected from the group consisting of pickled cumquat fruit for 3 years or more.
3. The extraction method according to claim 1, wherein the specific conditions of the ultrasonic extraction in the step (1) are as follows: the ultrasonic power is 300-500W, the mass ratio of the old orange to the water is 1:5-1:10, the extraction times are two, the first ultrasonic extraction is carried out, and the extraction time is 2-3 h; performing ultrasonic extraction for the second time for 1-2 h.
4. The extraction method according to claim 1, wherein the 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 crude extract of the old orange is adjusted to 4-8% before microfiltration, and the microfiltration is carried out for 50-90min under the room temperature condition of 0.08-0.12 MPa.
5. The extraction method according to claim 1, wherein the 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 limit of the flux 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, when the volume of the trapped fluid is obviously reduced, the flow rate of the filtered fluid is obviously reduced, and the solid content of the trapped fluid is 60% -65%, adding pure water for continuous filtration (V pure water is 0.5V filtrate), repeating for 1-3 times, replacing the filter membrane component, then filtering by using the ultrafiltration membrane with the molecular weight cutoff of 10KDa, when the volume of the trapped fluid is obviously reduced, the flow rate of the filtered fluid is obviously reduced, and the solid content of the trapped fluid is 55% -60%, then adding pure water for continuous filtration (V pure water is 0.5V filtrate), repeating for 1-3 times, stopping, replacing the filter membrane component, then filtering by using the ultrafiltration membrane with the molecular weight cutoff of 5KDa, when the volume of the trapped fluid is obviously reduced, and the flow rate of the filtered fluid is obviously reduced, and when the solid content of the trapped liquid is 50% -55%, adding pure water, continuously filtering (0.5V of filtrate) and repeating for 1-3 times, stopping and collecting the filtrate for later use.
6. The extraction method as claimed in claim 1, wherein 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 the 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 filtered liquid is obviously reduced, and the solid content of the trapped liquid is 15-20%, the trapped liquid is collected for standby application.
7. The extraction method according to claim 1, wherein the forward concentration conditions of step (5) are: the method comprises the steps of taking a hollow fiber forward concentration membrane as a separation membrane, controlling the flow rate of extracting solution and a drawing agent within 1L/min, taking high fructose corn syrup as the drawing agent, and carrying out 2-4-stage type circulation using the drawing agent for concentration at room temperature, namely, the drawing solution used at the last stage is pure high fructose corn syrup, stopping concentration when the drawing agent loses the drawing capability, and using the used drawing solution for the penultimate stage concentration of a next batch of samples, so as to circulate.
8. The extraction method as claimed in claim 1, wherein the gauze is 400-500 mesh.
9. 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.
10. The use as claimed in claim 9, wherein the mass ratio of the old medicinal orange spice to the cut tobacco is 1:1000-10: 1000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210655782.7A CN114886147B (en) | 2022-06-10 | 2022-06-10 | Method for extracting old medicine orange spice and application of old medicine orange spice in cigarettes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210655782.7A CN114886147B (en) | 2022-06-10 | 2022-06-10 | Method for extracting old medicine orange spice and application of old medicine orange spice in cigarettes |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114886147A true CN114886147A (en) | 2022-08-12 |
| CN114886147B CN114886147B (en) | 2022-12-23 |
Family
ID=82727743
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210655782.7A Active CN114886147B (en) | 2022-06-10 | 2022-06-10 | Method for extracting old medicine orange spice and application of old medicine orange spice in cigarettes |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114886147B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115462552A (en) * | 2022-09-16 | 2022-12-13 | 湖南中烟工业有限责任公司 | Spice with fruit sweet fragrance, preparation method thereof and application thereof in cigarettes |
| CN115644493A (en) * | 2022-11-10 | 2023-01-31 | 云南中烟工业有限责任公司 | Method for preparing tobacco flavor by membrane separation plant extract and application |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998024331A1 (en) * | 1996-12-02 | 1998-06-11 | Barth Fruit Ag | Method of processing, in particular concentrating, fruit and/or vegetable juice and arrangement for carrying out this method |
| CN103349351A (en) * | 2013-07-24 | 2013-10-16 | 江苏久吾高科技股份有限公司 | Method for reconstituting tobacco leaves by paper making method based on membrane separation technique |
| CN105533607A (en) * | 2015-12-08 | 2016-05-04 | 浙江绿晶香精有限公司 | Natural green kumquat flavor and preparation method thereof |
| CN110200181A (en) * | 2019-06-27 | 2019-09-06 | 揭阳职业技术学院 | A kind of plant beverage and preparation method thereof |
| CN110234596A (en) * | 2016-11-30 | 2019-09-13 | 安海斯-布希英博有限公司 | The method of carbonic acid beer is produced and deployed by beer concentrate |
| CN111040879A (en) * | 2019-12-31 | 2020-04-21 | 云南中烟新材料科技有限公司 | Preparation method and application of grape concentrated juice for preparing tobacco flavor |
| CN112358512A (en) * | 2020-11-17 | 2021-02-12 | 哈工大机器人南昌智能制造研究院 | Method for preparing hesperidin from citrus |
| EP3800238A1 (en) * | 2019-06-27 | 2021-04-07 | China Tobacco Guangdong Industrial Co., Ltd. | Slow-release flavorant and application thereof in chinese-flavor tobacco product |
| CN112716028A (en) * | 2020-12-18 | 2021-04-30 | 云南天宏香精有限公司 | Additive for composite cigarette, preparation method and application |
-
2022
- 2022-06-10 CN CN202210655782.7A patent/CN114886147B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998024331A1 (en) * | 1996-12-02 | 1998-06-11 | Barth Fruit Ag | Method of processing, in particular concentrating, fruit and/or vegetable juice and arrangement for carrying out this method |
| CN103349351A (en) * | 2013-07-24 | 2013-10-16 | 江苏久吾高科技股份有限公司 | Method for reconstituting tobacco leaves by paper making method based on membrane separation technique |
| CN105533607A (en) * | 2015-12-08 | 2016-05-04 | 浙江绿晶香精有限公司 | Natural green kumquat flavor and preparation method thereof |
| CN110234596A (en) * | 2016-11-30 | 2019-09-13 | 安海斯-布希英博有限公司 | The method of carbonic acid beer is produced and deployed by beer concentrate |
| CN110200181A (en) * | 2019-06-27 | 2019-09-06 | 揭阳职业技术学院 | A kind of plant beverage and preparation method thereof |
| EP3800238A1 (en) * | 2019-06-27 | 2021-04-07 | China Tobacco Guangdong Industrial Co., Ltd. | Slow-release flavorant and application thereof in chinese-flavor tobacco product |
| CN111040879A (en) * | 2019-12-31 | 2020-04-21 | 云南中烟新材料科技有限公司 | Preparation method and application of grape concentrated juice for preparing tobacco flavor |
| CN112358512A (en) * | 2020-11-17 | 2021-02-12 | 哈工大机器人南昌智能制造研究院 | Method for preparing hesperidin from citrus |
| CN112716028A (en) * | 2020-12-18 | 2021-04-30 | 云南天宏香精有限公司 | Additive for composite cigarette, preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 王璐等: "不同前处理方法对青金桔致香成分测定的影响", 《香料香精化妆品》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115462552A (en) * | 2022-09-16 | 2022-12-13 | 湖南中烟工业有限责任公司 | Spice with fruit sweet fragrance, preparation method thereof and application thereof in cigarettes |
| CN115462552B (en) * | 2022-09-16 | 2023-09-05 | 湖南中烟工业有限责任公司 | Spice with fruit fragrance, preparation method thereof and application thereof in cigarettes |
| CN115644493A (en) * | 2022-11-10 | 2023-01-31 | 云南中烟工业有限责任公司 | Method for preparing tobacco flavor by membrane separation plant extract and application |
| CN115644493B (en) * | 2022-11-10 | 2024-05-14 | 云南中烟工业有限责任公司 | Method for preparing tobacco flavor by membrane separation of plant extract and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114886147B (en) | 2022-12-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114886147B (en) | Method for extracting old medicine orange spice and application of old medicine orange spice in cigarettes | |
| CN102161935B (en) | Endogenous perfume from tobacco as well as preparation method and application thereof | |
| CN108384637B (en) | Preparation method of bouquet type Maillard spice and application of bouquet type Maillard spice in cigarettes | |
| CN103865651A (en) | Preparation method of melon and fruit perfume for cigarettes | |
| CN103349351A (en) | Method for reconstituting tobacco leaves by paper making method based on membrane separation technique | |
| CN108851198B (en) | Tobacco stem processing method and preparation method of tobacco stem extract | |
| CN102796615B (en) | Method for preparing cigarette strawberry extract by using pectinase | |
| CN107232638A (en) | A kind of upgrading purification process of raisin extract and its application | |
| CN101637303A (en) | Lemon extract, preparation method thereof and application thereof in cigarette flavoring | |
| CN107637858A (en) | A kind of plant for improving water extraction and alcohol precipitation method extraction causes perfumery and extracting method and application | |
| CN111789283B (en) | Tobacco stem multi-stage utilization method based on supercritical CO2 extraction technology | |
| CN103881815A (en) | Black plum extract, preparation method for same and application of extract to cigarette | |
| CN113638265B (en) | Cigarette flavor for cigarette paper coating liquid and application thereof, cigarette paper coating liquid and cigarette | |
| CN111040879A (en) | Preparation method and application of grape concentrated juice for preparing tobacco flavor | |
| CN113633017A (en) | Tobacco extract, preparation method and application thereof, and tobacco product | |
| CN107446704A (en) | A kind of preparation method of cigarette strawberry extract | |
| CN114836261B (en) | Extraction method of old medicine orange spice and application of old medicine orange spice in cigarette filter tips | |
| CN114794527B (en) | Sophora flower extract, preparation method thereof and cigarette flavoring | |
| CN109527641B (en) | Tobacco extract and preparation method thereof | |
| CN104497163A (en) | Korla pear polysaccharide extracting method and method for applying korla pear polysaccharide to cigarettes | |
| CN105154230A (en) | Preparation method of cigarette pineapple flavor | |
| CN116355692A (en) | Preparation method of coffee spice, atomized essence and smoking set | |
| CN114751944B (en) | Preparation method of proline-glucose Amadori compound | |
| CN106987315A (en) | A kind of lychee flavor, its preparation method and the application in cigarette | |
| CN114041623A (en) | Tobacco characteristic aroma component, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |