CN117180791A - Preparation method and application of chicory sweet aroma spice product with heavy components - Google Patents
Preparation method and application of chicory sweet aroma spice product with heavy components Download PDFInfo
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- CN117180791A CN117180791A CN202210615151.2A CN202210615151A CN117180791A CN 117180791 A CN117180791 A CN 117180791A CN 202210615151 A CN202210615151 A CN 202210615151A CN 117180791 A CN117180791 A CN 117180791A
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- 235000013599 spices Nutrition 0.000 title abstract description 5
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- Seasonings (AREA)
Abstract
The application relates to a preparation method and application of a chicory sweet flavor product with a recombinant component, which comprises the steps of selecting a set solvent to dissolve a chicory extract into a solution, sequentially passing through a membrane with the pore diameter of 200nm, 50nm, the molecular weight cut-off of 80KD or the pore diameter of 15nm and the molecular weight cut-off of 1KD or the pore diameter of 2nm, discarding the cut-off liquid and the penetrating liquid of part of the steps, reasonably and uniformly recombining and mixing the retained cut-off liquid and the penetrating liquid according to a set proportion through the indirect contribution component of the flavor and the direct contribution component of the flavor to obtain the chicory sweet flavor product with the recombinant component, and applying the product to tobacco shreds of a tobacco. The product obtained by the technical scheme can endow the tobacco with pleasant burnt sweet smell, has more obvious style and more concentrated aroma components, and avoids adverse effects or unnecessary flavor characteristics after the spice crude product is applied to tobacco shreds of the tobacco.
Description
Technical Field
The application belongs to the technical field of tobacco flavor, and particularly relates to a preparation method and application of a chicory sweet flavor product with a heavy component.
Background
The tobacco pipe is a tobacco product which is specially used for smoking by using the tobacco pipe. The main raw materials of the tobacco pipe are sun-cured tobacco, air-cured tobacco or flue-cured tobacco, and a proper amount of spice or vegetable oil is mixed. Foreign tobacco consumption history is long, but most of the products are based on local markets, are designed for local consumers as audiences, and have thick regional characteristics. These products are substantially unsuitable for taste preference of domestic tobacco consumers. In the domestic tobacco market, the tobacco pipe is still in the market cultivation stage, belongs to 'masses' tobacco consumer products, and the tobacco pipe products of Chinese tobacco production enterprises are not found to be marketed on a large scale at present. The development of a tobacco product suitable for the taste of Chinese tobacco consumers has received attention from related research institutions or people in China.
The sweet aroma is an important aroma of the aroma style characteristics of the Chinese style cigarettes, is coordinated with the aroma of the flue-cured tobacco, reflects the main characteristics of the aroma style of the Chinese style flue-cured tobacco, and is also the aroma characteristics commonly accepted and favored by domestic tobacco consumers. Compounds with the characteristic of sweet and sour flavor such as furans, furanones, cyclopentenones, pyrones and the like are discovered in the research of tobacco smoke condensate at home and abroad in succession, and mainly include Maltol (Maltol), 4-hydroxy-2, 5-dimethyl-3 (2H) -furanone (Furaneol), methylcyclopentenolone (cyclote), ethylcyclopentenolone (3-Ethyl-2-hydroxy-2-cyclical-1-one), 5-Methylfurfural (5-methylfurfurfural) and the like. These substances are contained in addition to tobacco, in chicory extracts.
Chicory (Cichorium intybus l.) is a perennial herb of the genus chicory of the family chicory. The extract prepared by roasting and leaching the chicory root dry slices has the burnt sweet flavor similar to cocoa or coffee, is used for perfuming cigarettes, and has the effects of improving the smoke concentration and texture, harmonizing the smoke flavor, covering miscellaneous gases and improving aftertaste.
However, chicory extracts obtained by conventional solvent extraction and concentration have complex internal component constitution, and may cause bad performances such as bitterness, irritation, residue, etc. when applied to tobacco shreds of tobacco, or cause unnecessary flavor characteristics in product design. Natural perfume for the tobacco pipe which accords with domestic tobacco consumer preference is limited, and research reports of accurate separation and preparation of characteristic flavor groups of chicory extract for fresh tobacco are provided. Conventional fine processing technology of natural spice for cigarettes aims at removing impurities, and the quality of the obtained finished product is improved, but the functional focusing degree of the product is insufficient. On the other hand, unlike synthetic flavors, the flavor profile of natural flavors still derives from the combined action of multiple components, and the precise positioning of flavor clusters is not the same as the purpose and method of separating single compounds in the medical field. The chicory special flavor group with focused functions and multiple components is obtained, the characteristic of the sweet and burnt fragrance of the chicory is fully highlighted, and the method provides more abundant and effective fragrance raw material supply for developing the tobacco products meeting the taste preference of domestic consumers and has practical significance.
The use characteristics of the natural perfume for cigarettes determine that the natural perfume for cigarettes consists of two parts, namely an indirect flavor contribution component (contributing flavor after combustion) and a direct flavor contribution component (prototype transfer to smoke). The ultrafiltration technology of membrane separation has the capability of separating flavor precursors, the nanofiltration technology has the capability of enriching flavor direct contribution components, the multistage membrane separation technology is reasonably applied, the advantages of the technology are exerted, the functions of the technology are complementary, and the accurate preparation of different flavor components of natural flavors for cigarettes can be well realized.
Disclosure of Invention
The application aims to provide a preparation method and application of a chicory sweet flavor product with a heavy component, which are used for accurately separating and preparing the sweet flavor component by applying a proper separation technology to a chicory extract and applying the chicory extract to flavoring of tobacco shreds of a tobacco pipe so as to solve the defect that the prior chicory extract has the application aspect of the flavor.
In order to achieve the above purpose, the application is realized by the following technical scheme:
a preparation method of a chicory sweet flavor product with heavy components comprises the following steps:
s1, raw material treatment:
selecting a set solvent to dissolve chicory extract into a solution with a set concentration, then carrying out solid-liquid separation, and collecting liquid obtained by the solid-liquid separation;
s2, multistage membrane separation:
selecting a set membrane to carry out multistage membrane separation on the chicory extract solution treated in the step S1, and carrying out step-by-step separation according to the pore diameter of the membrane from large to small; the method comprises the following specific steps: the chicory extract solution is firstly passed through a membrane with the aperture of 200nm, the trapped fluid A is discarded, the permeate A is further passed through a membrane with the aperture of 50nm, the trapped fluid B is collected, the permeate B is then passed through a membrane with the molecular weight of 80KD or the aperture of 15nm, the trapped fluid C is discarded, the permeate C is further passed through a membrane with the molecular weight of 1KD or the aperture of 2nm, and the trapped fluid D and the permeate D are collected;
s3, recombination of effective components:
uniformly mixing the trapped fluid B, the trapped fluid D and the penetrating fluid D according to a set proportion to obtain the chicory sweet aroma flavor product with the recombinant components.
Further, the solvent in the step S1 is water, a mixture of water and ethanol and/or propylene glycol.
Further, the solvent is added in the step S1 in an amount of 1-30 times the mass of the dry matter in the chicory extract.
Further, the solvent is added in the step S1 in an amount of 2-15 times the mass of the dry matter in the chicory extract.
In step S1, the chicory extract is diluted into a solution with a set concentration, and the solution is left for a set period of time at a low temperature and then filtered or centrifuged to remove insoluble substances, so that the plant wax is removed more effectively.
Further, the film in step S2 is an organic film or a ceramic film.
Further, in step S3, the amount of the trapped liquid B is 2-8 times of that of the permeate liquid D based on the permeate liquid D according to the dry matter mass ratio of each solution, and the amount of the trapped liquid D is 2-5 times of that of the permeate liquid D.
The use of a recombinant chicory sweet flavor product of any one of the above as additive for flavoring tobacco shreds of a tube tobacco.
Furthermore, the addition amount of the chicory sweet flavor product with the heavy components is 0.005-0.5% of the mass of tobacco shreds of the chest tobacco, and the chicory sweet flavor product can be used alone or blended with other flavors to form essence.
The dry matter in the present application means a matter obtained after completely removing the solvent in the system.
The application has the following beneficial effects:
aiming at the sweet and aromatic components in chicory, the technical scheme selects a multistage membrane separation technology which is easy for large-scale production, realizes the accurate positioning and effective separation of the sweet and aromatic components in the chicory extract, prepares the chicory sweet and aromatic flavor product of the heavy components suitable for flavoring the tobacco shreds of the tobacco cigarettes, has more obvious style of the obtained product and more concentrated aroma components, and avoids adverse effects or unnecessary flavor characteristics introduced after the crude flavor product is applied to the tobacco shreds of the tobacco cigarettes.
According to the preparation method, proteins, pectin, cellulose and macromolecular pigment substances contained in the chicory extract are removed by using a 200nm microfiltration membrane, so that the problem of poor sensory comfort caused by the fact that the components are added into tobacco shreds of the tobacco is avoided; the 50nm membrane retentate was selectively enriched in flavor precursors; the 80kD (15 nm) membrane removed some of the components that caused oral irritation and production of miscellaneous gases; the 1kD (2 nm) membrane trapped fluid and the permeate effectively enrich the flavor direct contribution components; finally, the optimal application effect is achieved through reasonable recombination of the flavor indirect contribution component and the flavor direct contribution component.
The chicory sweet flavor product of the recombinant component of the technical scheme is rich in micromolecular saccharides and various sweet flavor components, wherein the sweet flavor components mainly comprise furans, furanones, pyrones, cyclopentenones and pyrazines, and most of the substances have characteristic flavors of sweet flavor, baking flavor or nut flavor.
The production process is simple and easy to control, the production process is economic and environment-friendly, and the method is suitable for large-scale industrial production application.
Drawings
FIG. 1 is a total ion flow diagram of GC-MS qualitative analysis of chicory extract of example 1.
FIG. 2 is a GC-MS quantitative chromatogram of the relevant ingredients of the scorch aroma of chicory of the recombinant composition prepared by the method of example 1.
FIG. 3 is an HPLC-ELSD chromatogram of small molecule saccharide fraction in chicory sweet aroma of the recombinant fraction prepared by the method of example 1.
FIG. 4 is a GC-MS quantitative chromatogram of the relevant ingredients of the scorch aroma of chicory of the recombinant composition prepared by the method of example 2.
FIG. 5 is an HPLC-ELSD chromatogram of small molecule saccharide fraction in chicory sweet aroma of the recombinant fraction prepared by the method of example 2.
Detailed Description
The following detailed description of the present application is provided by way of example only, and is not to be construed as limiting the scope of the application.
The chicory extract related in the technology can be extractum, absolute, tincture, powder and the like prepared by different pretreatment processes and different extraction processes, or various extracts obtained by fermentation, enzymolysis and the like.
Example 1
S1, raw material treatment:
chicory extract, purchased from Zhengzhou middle-aged biology limited. The dry mass fraction (about 70.98%) was calculated by measuring the content of 4 common solvents, water, ethanol, 1, 2-propanediol, glycerol, in the extract using standard methods, subtracting the solvent content. Adding 40% ethanol solution (volume fraction) with the mass of 8.6 times of the dry matter into the extract, and fully and uniformly mixing to prepare a diluent with the mass fraction of 10% of the dry matter; standing at-5 ℃ for more than 4 hours; the insoluble material was removed by centrifugation (7000 rpm,10min, -5 ℃).
S2, multistage membrane separation:
(1) Separating the centrifuged clear liquid by adopting a ceramic membrane with the aperture of 200nm, setting the frequency of a pressurizing pump to 45Hz, and the pressure before the membrane to 3.0bar, wherein the pressure after the membrane is 2.4bar, the temperature of the feed liquid is about 27 ℃, and the membrane flux is 53.2L/(h/m) 2 ). And (3) adding a small amount of dialysate (namely, a solvent for diluting the extract and 40% ethanol) into the charging basket for multiple times until the membrane separation is carried out at the end stage, so that the mass of the permeate is approximately equal to the mass of the feed liquid before separation. After separation, the trapped fluid A is discarded after a small amount of sample is reserved, the permeate A is directly subjected to 50nm ceramic membrane separation after a small amount of sample is reserved, and the reserved small amount of sample is only used for sensory evaluation.
(2) Adding the permeate A into a 50nm ceramic membrane equipment feed cylinder, setting a pressurizing pump frequency of 45Hz, and a membrane front pressure of 3.5bar, wherein the membrane rear pressure is 1.6bar, the feed liquid temperature is about 30 ℃, and the membrane flux is 29.2L/(h.m) 2 ). And (3) adding a small amount of dialysate into the charging basket for many times until the membrane separation is carried out at the end stage, so that the quality of the permeate is approximately equal to that of the feed liquid before separation. After separation, collecting trapped fluid B, and directly carrying out 80kD roll-type organic membrane separation after a small amount of sample is reserved in permeate fluid B.
(3) Adding the permeate B into a feed cylinder of an 80kD organic membrane device, setting a pressurizing pump frequency of 45Hz, and a membrane front pressure of 4.0bar, wherein the membrane rear pressure is 3.2bar, the feed liquid temperature is about 25 ℃, and the membrane flux is 48.9L/(h.m) 2 ). And (3) adding a small amount of dialysate into the charging basket for many times until the membrane separation is carried out at the end stage, so that the quality of the permeate is approximately equal to that of the feed liquid before separation. After separation, the trapped fluid C is discarded after a small amount of sample is reserved, and the permeate fluid C is directly subjected to 1kD organic membrane separation after a small amount of sample is reserved.
(4) Adding the permeate C into a 1kD organic membrane equipment feed cylinder, setting a pressurizing pump frequency of 45Hz, and a membrane front pressure of 4.5bar, wherein the membrane rear pressure is 3.6bar, the feed liquid temperature is about 31 ℃, and the membrane flux is 27.6L/(h.m) 2 ). And (3) adding a small amount of dialysate into the charging basket for many times until the membrane separation is carried out at the end stage, so that the quality of the permeate is approximately equal to that of the feed liquid before separation. After the separation, the retentate D and the permeate D were collected.
S3, recombination of effective components, component analysis and sensory effect evaluation:
(1) Recombination of active ingredients:
and respectively measuring the solvent content of the trapped fluid B (50 nm trapped fluid), the trapped fluid D (1 kD trapped fluid) and the permeate D (1 kD permeate), calculating the mass fractions of the dry matters, and uniformly mixing the corresponding solutions according to the mass ratio of the dry matters of 4:3:1 to obtain the chicory sweet flavor product P1 with the recombinant components.
(2) Aroma component analysis of the recombinant chicory sweet aroma product:
product P1 was freeze-dried for instrumental analysis.
A certain amount of freeze-dried P1 is accurately weighed, fully oscillated and extracted by an internal standard extract (a methanol solution of styryl propionate with the concentration of 0.318 mu g/mL), and the supernatant is detected by a gas chromatograph-mass spectrometer (GC-MS) after passing through a 0.22 mu m needle filter head.
Chromatographic column: DB-WAX (60 m. Times.0.25 mm. Times.0.25 μm); carrier gas: he,99.999%; flow rate: 1.0mL/min; sample inlet temperature: 250 ℃; sample injection mode: sample introduction without diversion; sample injection amount: 1 μl; heating program:solvent delay: for 10min; transmission line temperature: 250 ℃; ion source: EI; electron energy: 70eV; ion source temperature: 230 ℃; quadrupole temperature: 150 ℃; scanning mode: full scanning; mass scan range: 33-500a.m.u.
After qualitative analysis of aroma components in P1 (total ion flow diagram is shown in figure 1), quantitative determination of sweet aroma, baked aroma and nut aroma substances is carried out by adopting selective ion scanning. The qualitative and quantitative ion parameters of the target are shown in Table 1.
Chromatographic column: DB-WAX (60 m. Times.0.25 mm. Times.0.25 μm); carrier gas: he,99.999%; flow rate: 1.0mL/min; sample injection mode: sample introduction without diversion; sample injection amount: 1 μl; sample inlet temperature: 250 ℃; programming temperature: 60 ℃ (1 min), 5 ℃/min to 250 ℃ (5 min); GC/MS transmission line temperature: 250 ℃, EI ion source temperature: 230 ℃, four-stage bar temperature: 150 ℃; EI ionization energy: 70eV. Scanning mode: ion scanning is selected.
TABLE 1 target and internal Standard selection ion parameter Table
Preparing 7-level concentration gradient mixed standard solution of the target objects, respectively performing GC-MS analysis, taking the ratio of the concentration of each target object to the concentration of the internal standard as an abscissa (x), and taking the ratio of each target object to the area of the internal standard peak as an ordinate (y), so as to obtain a standard working curve and a linear correlation coefficient R of each target object 2 See table 2.
TABLE 2 Standard Curve, detection Limit and quantitative Limit for 25 targets
Quantitative analysis results of aroma components related to the sweet aroma in the chicory sweet aroma product prepared in the embodiment are shown in Table 3, and a chromatogram is shown in FIG. 2. The odor description and the cigarette sensory contribution description of each component are reported by references in combination with laboratory self-evaluation. As can be seen from the analysis results, the aroma component of P1 is rich in furans (furfural, furfuryl alcohol, 5-methylfurfural, 5-hydroxymethylfurfural, 2-acetylfuran), furanones (4-hydroxy-2, 5-dimethyl-3 (2H) -furanone, 2-methyltetrahydrofuran-3-one), pyrones (maltol, DDMP), cyclopentenones (methylcyclopentenolone, ethylcyclopentenolone), and various pyrazine and pyrrole compounds. Wherein various substances are inherent components of cigarette smoke. Maltol, methylcyclopentenolone, ethylcyclopentenolone, 4-hydroxy-2, 5-dimethyl-3 (2H) -furanone, and the like have typical sweet odor; furfural, 5-methylfurfural, 5-hydroxymethylfurfural, DDMP and furfuryl alcohol are main products of caramelization reaction or Maillard reaction of food, and have caramel-like and fermented flavor; most of pyrazine substances have nut fragrance and baking fragrance, and can assist in increasing the sweet fragrance of smoke and harmonizing with the fragrance of smoke.
Table 3 results of analysis of major aroma components of P1
(3) Sweet component analysis of a recombinant chicory sweet flavor product
100.00mg of lyophilized P1 was weighed into a small beaker, dissolved with a small amount of distilled water, transferred into a 10mL volumetric flask and fixed in volume. Accurately weighing standard substances of glucose (105.5 mg), fructose (29.9 mg), sucrose (29.7 mg), maltose (30.2 mg), arabitol (19.7 mg), D-sorbitol (30.6 mg), myo-glucose (30.7 mg) and maltotriose (31.5 mg) in the same small beaker, dissolving the standard substances in distilled water, transferring the dissolved standard substances into a 10mL volumetric flask and fixing the volume; the sugar mixed standard mother solutions 50, 100, 250, 500, 750, 1000 and 1250 mu L are respectively taken in different 10mL volumetric flasks, distilled water is used for constant volume, and 7 mixed standard solutions with concentration are prepared. Separately, standard solutions of these 8 sugars were prepared at a concentration of about 1 mg/mL. And (3) taking the mixed standard, the single standard and the sample solution, analyzing by using an HPLC-ELSD instrument, establishing a standard curve (see Table 4), and accurately quantifying the to-be-detected substances in the sample.
Instrument conditions: chromatographic column: prevail Carbohydrate ES sugar column (250X 4.6mm,5 μm) equipped with the same type of pre-column (7.5X 4.6mm,5 μm). Mobile phase: acetonitrile (a), water (B); gradient elution: 0 to 20min,20 to 25 percent of B; 20-35 min, 25-45% B; 35-40 min,45% of B; 40-45 min, 45-20% B. Flow rate: 0.8mL/min. Sample injection amount: 10 mu L. Column temperature: 30 ℃. ELSD drift tube temperature: 80 ℃; nitrogen flow rate: 2.2L/min.
Table 48 standard working curves for sugars
Target object | Linear regression equation | R 2 | Linear range (mg/mL) |
Arabitol | lny=2.0527 lnx+3.1544 | 0.9989 | 0.00985~0.2463 |
Fructose | lny=1.9029 lnx+2.9735 | 0.999 | 0.01495~0.3738 |
D-sorbitol | lny=2.0025 lnx+2.9999 | 0.9998 | 0.0153~0.3825 |
Glucose | lny=1.8347 lnx+2.2796 | 0.9991 | 0.05275~1.3188 |
Myo-candy | lny=1.8511 lnx+2.8416 | 0.9992 | 0.01535~0.3838 |
Sucrose | lny=1.7536 lnx+2.9604 | 0.9992 | 0.01485~0.3713 |
Maltose | lny=1.747 lnx+2.6641 | 0.999 | 0.01359~0.3398 |
Maltotriose | lny=1.8267 lnx+2.3924 | 0.999 | 0.01575~0.3938 |
HPLC-ELSD chromatogram of P1 is shown in FIG. 3, and analysis results of saccharide composition are shown in Table 5. As can be seen from the analysis results, P1 is rich in fructose and contains a small amount of glucose, D-sorbitol, sucrose, maltose and maltotriose. The small molecular sugar components can be added into the tobacco pipe to increase the sweet feeling of the tobacco pipe, reduce the stimulation and improve the comfort of suction; meanwhile, reducing sugar can also generate Maillard reaction with amino acid during combustion and absorption, so as to generate various substances with sweet flavor and increase the sweet characteristic of smoke.
Table 5 results of analysis of saccharide compositions in P1
(4) Sensory evaluation of a high-component chicory sweet aroma flavor product in a tube tobacco
The prepared P1 is diluted by 40 percent ethanol, and is applied to the tobacco shreds of the tobacco in a feeding procedure in a spraying mode, and the dosage of the diluted P1 is 0.01 percent of the mass of the tobacco shreds of the tobacco after being converted into dry matters. The control sample is prepared by adding chicory extract (Zhengzhou middle-intention organism limited company) with equal dry matter mass onto tobacco shred of herba Cichorii by the same method, and balancing under constant temperature and humidity for a period of time. The results of the comprehensive evaluation by 7 or more panelists (table 6) are shown: compared with a control sample, when the pipe tobacco shred added with the P1 provided by the application is smoked, the burnt sweet smell of the smoke is obviously felt to be more outstanding, the smoke is coordinated with the smoke smell, the smoke concentration is increased, the aftertaste is sweet and comfortable, the stimulus of the oral cavity and the throat is small, and the overall sensory quality is better.
TABLE 6 sensory quality comparison and smoking results of control and test cut tobacco
Example 2
S1, raw material treatment:
chicory extracts were purchased from the company of the finkset trade, zhengzhou cloud, in the form of a powder. Adding distilled water with the mass 11.5 times of that of the extract into the extract to prepare a diluent with the mass fraction of dry matters of 8 percent; insoluble materials were removed using a plate and frame filter press.
S2, multistage membrane separation:
(1) Separating the centrifuged clear liquid by adopting a ceramic membrane with the aperture of 200nm, setting the frequency of a pressurizing pump to 40Hz, and the pressure before the membrane to 3.0bar, wherein the pressure after the membrane is 2.1bar, the temperature of the feed liquid is about 30 ℃, and the membrane flux is 67.3L/(h.m) 2 ). And (3) adding a small amount of dialysate (namely distilled water) into the charging basket for many times until the membrane separation is carried out at the end stage, so that the quality of the permeate is approximately equal to that of the feed liquid before separation. After the separation is finished, the trapped fluid A is discarded after a small amount of sample is reserved, and the permeate A is directly subjected to 50nm ceramic membrane separation after a small amount of sample is reserved.
(2) Adding the permeate A into a 50nm ceramic membrane equipment feed cylinder, setting the frequency of a pressurizing pump to 40Hz, and the pressure before membrane is 3.0bar, wherein the pressure after membrane is 1.9bar, the temperature of feed liquid is about 27 ℃, and the membrane flux is 59.4L/(h.m) 2 ). And (3) adding a small amount of dialysate into the charging basket for many times until the membrane separation is carried out at the end stage, so that the quality of the permeate is approximately equal to that of the feed liquid before separation. After the separation is finished, the trapped liquid B is collected, and a small amount of sample is left in the permeate liquid B and then is directly separated by a 15nm ceramic membrane.
(3) Adding the permeate B into a 15nm ceramic membrane equipment feed cylinder, setting the frequency of a pressurizing pump to 40Hz, and the pressure before membrane is 3.5bar, wherein the pressure after membrane is 2.6bar, the temperature of feed liquid is about 34 ℃, and the membrane flux is 39.5L/(h.m) 2 ). And (3) adding a small amount of dialysate into the charging basket for many times until the membrane separation is carried out at the end stage, so that the quality of the permeate is approximately equal to that of the feed liquid before separation. After separation, the trapped fluid C is discarded after a small amount of sample is left, and the permeate fluid C is directly subjected to 2nm ceramic membrane separation after a small amount of sample is left.
(4) Adding the permeate C into 2nm ceramic membrane equipment materialSetting up the pressure pump frequency 45Hz, the pressure 4.0bar before the membrane, the pressure 2.9bar after the membrane, the temperature of the feed liquid about 33 ℃ and the flux 20.4L/(h.m) 2 ). And (3) adding a small amount of dialysate into the charging basket for many times until the membrane separation is carried out at the end stage, so that the quality of the permeate is approximately equal to that of the feed liquid before separation. After the separation, the retentate D and the permeate D were collected.
S3, recombination of effective components, component analysis and sensory effect evaluation:
(1) Recombination of active ingredients
And respectively measuring the solvent content of the trapped fluid B (50 nm trapped fluid), the trapped fluid D (2 nm trapped fluid) and the permeate fluid D (2 nm permeate fluid), calculating the mass fractions of the dry matters, and uniformly mixing the corresponding solutions according to the mass ratio of the dry matters of 3:2:1 to obtain the chicory sweet flavor product P2 with the recombinant components.
(2) Aroma component analysis of a heavy component chicory sweet aroma product
The content of the relevant ingredients of the sweet and spicy flavor in P2 was measured by the same GC-MS analysis method as in example 1, and the specific results are shown in Table 7, and the chromatogram is shown in FIG. 4.
TABLE 7 analysis results of major aroma components of P2
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(3) Sweet component analysis of a recombinant chicory sweet flavor product
The HPLC-ELSD analysis method similar to that of example 1 was used to determine the content of small molecule saccharide in P2, and the specific results are shown in Table 8, and the chromatogram is shown in FIG. 5. As can be seen from the analysis results, P2 is rich in glucose, fructose and sucrose, and also contains a small amount of D-sorbitol, maltose and maltotriose. The small molecular sugar components can be added into the tobacco pipe to increase the sweet feeling of the tobacco pipe, reduce the stimulation and improve the comfort of suction; meanwhile, reducing sugar such as glucose, fructose and the like can also generate Maillard reaction with inherent amino acid of tobacco leaves during combustion and absorption, so that various sweet flavor substances are generated, and the sweet and fragrant characteristics of smoke are improved.
Table 8 results of analysis of saccharide compositions in P2
(4) Sensory evaluation of a high-component chicory sweet aroma flavor product in a tube tobacco
The prepared product P2 is diluted by water and is applied to the tobacco shreds of the tobacco in a feeding procedure in a spraying mode, and the dosage of the product P2 is 0.02% of the mass of the tobacco shreds of the tobacco after being converted into dry matters. The control sample is prepared by diluting herba Cichorii extract (Sakuda GmbH, carnis Corvus, chebulae.) of equal dry matter quality with water to the same concentration, adding into tobacco shred, and balancing under constant temperature and humidity for a period of time. The results of the comprehensive evaluation by 7 or more panelists (table 9) are shown: compared with a control sample, when the pipe tobacco shred added with P2 is sucked, the smoke is more fragrant and sweet, is coordinated with the smoke, has the advantages of sweet aftertaste and comfort, smaller stimulation to the oral cavity and the throat, better overall sensory quality and better accords with the taste preference of domestic consumers.
TABLE 9 sensory quality comparison and smoking results of control and test cut tobacco
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and are not limiting; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may be modified or some technical features may be replaced with others, which may not depart from the spirit and scope of the technical solutions of the embodiments of the present application.
Claims (9)
1. A method for preparing a chicory sweet flavor product with a heavy component, which is characterized by comprising the following steps:
s1, raw material treatment:
selecting a set solvent to dissolve chicory extract into a solution with a set concentration, then carrying out solid-liquid separation, and collecting liquid obtained by the solid-liquid separation;
s2, multistage membrane separation:
selecting a set membrane to carry out multistage membrane separation on the chicory extract solution treated in the step S1, and carrying out step-by-step separation according to the pore diameter of the membrane from large to small; the method comprises the following specific steps: the chicory extract solution is firstly passed through a membrane with the aperture of 200nm, the trapped fluid A is discarded, the permeate A is further passed through a membrane with the aperture of 50nm, the trapped fluid B is collected, the permeate B is then passed through a membrane with the molecular weight of 80KD or the aperture of 15nm, the trapped fluid C is discarded, the permeate C is further passed through a membrane with the molecular weight of 1KD or the aperture of 2nm, and the trapped fluid D and the permeate D are collected;
s3, recombination of effective components:
uniformly mixing the trapped fluid B, the trapped fluid D and the penetrating fluid D according to a set proportion to obtain the chicory sweet aroma flavor product with the recombinant components.
2. A process for the preparation of a recombinant chicory sweet aroma product according to claim 1, characterized in that the solvent in step S1 is water, a mixture of water and ethanol and/or propylene glycol.
3. A process for the preparation of a recombinant chicory sweet aroma product according to claim 1, characterized in that the solvent is added in step S1 in an amount of 1-30 times the mass of dry matter in the chicory extract.
4. A process for the preparation of a recombinant chicory sweet aroma product according to claim 3, characterized in that the solvent is added in step S1 in an amount of 2-15 times the mass of dry matter in the chicory extract.
5. The method for preparing a recombinant chicory sweet flavor product according to claim 1, wherein in step S1, the chicory extract is diluted into a solution with a set concentration, and the solution is left for a set time at a low temperature, and then subjected to solid-liquid separation to remove insoluble matters, thereby more effectively removing plant waxes.
6. A process for the preparation of a recombinant chicory sweet aroma product according to claim 1, characterized in that the membrane in step S2 is an organic membrane or a ceramic membrane.
7. The preparation method of the chicory sweet flavor product with the recombinant component according to claim 1, wherein in the step S3, the contents of water, ethanol, 1, 2-propylene glycol and glycerin in the trapped liquid B, the trapped liquid D and the permeate D are respectively measured, the dry matter mass fractions of the solutions are calculated, and according to the dry matter mass ratios of the solutions, the amount of the trapped liquid B is 2-8 times that of the permeate D based on the permeate D, and the amount of the trapped liquid D is 2-5 times that of the permeate D.
8. Use of a heavy component chicory sweet flavor product according to any of the preceding claims 1 to 7 as additive for flavoring tobacco cut filler.
9. Use of the recombinant chicory sweet flavor product according to claim 8, characterized in that the recombinant chicory sweet flavor product is added in an amount of 0.005-0.5% of the mass of the tobacco cut filler.
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