CN108095187B - Method for enriching tobacco glucoside - Google Patents
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- CN108095187B CN108095187B CN201711194257.5A CN201711194257A CN108095187B CN 108095187 B CN108095187 B CN 108095187B CN 201711194257 A CN201711194257 A CN 201711194257A CN 108095187 B CN108095187 B CN 108095187B
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- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
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Abstract
The invention relates to a method for enriching tobacco glucoside, and belongs to the technical field of cigarette production. According to the invention, according to the difference of physicochemical properties of different chemical components of tobacco, the non-glycoside substances in the tobacco are removed and the tobacco glycoside is enriched by utilizing the combined application of membranes with the aperture of 100nm, 10nm and 3-5 nm. Removing impurities from water extract of tobacco raw material by centrifugation or chemical sedimentation, removing solid matters such as silt, tobacco powder and fiber with 100nm pore membrane to obtain true solution of tobacco extract, filtering the true solution with 10nm pore membrane to remove soluble high molecular substances, filtering the 10nm pore membrane permeate with 3-5nm pore membrane to remove impurities such as sugar and salt, and collecting the 3-5nm pore membrane retentate to obtain solution enriched with tobacco glucoside. The technical method does not need to use an organic solvent, is environment-friendly, and has the advantages of good economy, high enrichment yield of the tobacco glycoside, suitability for large-scale production and the like.
Description
Technical Field
The invention belongs to the technical field of cigarette production, and particularly relates to a process method for enriching tobacco glucoside by treating tobacco extract by a membrane separation technology according to the difference of physicochemical properties of different chemical components of tobacco.
Background
The glycoside is also called glycoside, and is a compound formed by dehydration of hemiacetal hydroxyl of monosaccharide or oligosaccharide and functional groups such as hydroxyl, sulfydryl and the like in the molecule of the compound. The glucoside in the tobacco is an important latent fragrant substance of the tobacco, and has important effects on the fragrance characteristics and smoking quality of the cigarette.
The nicotiana glycosides can be obtained by isolating the chemical constituents of tobacco or by synthetic methods. The general method for preparing glucoside by separating chemical components from tobacco is to firstly extract the tobacco with water, then extract water solution with n-butyl alcohol to enrich glucoside, and obtain the glucoside by column chromatography purification. When the glucoside is prepared by a synthetic method, generally, aglycone and bromide of sugar are prepared by substitution reaction. The former method has high cost and is not suitable for large-scale production; although the latter method can obtain some tobacco glycoside substances with high purity, it is difficult to obtain a glycoside mixture which has the same or similar composition with tobacco glycoside, and the application of cigarettes is limited, and the preparation cost is high.
At present, no article and patent report for enriching glucoside from tobacco by using membrane separation technology is found.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provide the method for enriching the tobacco glycoside, and the technical method does not need to use an organic solvent, is environment-friendly, and has the advantages of good economy, high enrichment yield of the tobacco glycoside, suitability for large-scale production and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for enriching tobacco glucoside comprises the following steps:
step (1), preparing a tobacco suspension turbid solution: centrifuging or chemically settling the tobacco raw material water extract with dry matter content not higher than 25%, and removing the precipitate to obtain tobacco suspension;
the tobacco raw material is at least one of tobacco stems, tobacco powder and tobacco leaves;
the chemical sedimentation takes chitosan with the mass concentration of 0.2% as a sedimentation agent;
step (2), primary filtration: filtering the tobacco suspension turbid solution obtained in the step (1) through a membrane with the aperture of 100nm, and when the volume ratio of the trapped fluid to the permeation solution is 1: 19, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped fluid, uniformly mixing, continuing to pass through a 100nm pore size membrane until the volume of the trapped fluid is 5% of the volume of the tobacco suspension turbid liquid, and finishing filtration;
and (3) secondary filtration: filtering the permeation solution obtained in the step (2) by a membrane with the aperture of 10nm, adding water with the volume of 1/10 of the tobacco suspension turbid solution into the trapped solution when the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution, uniformly mixing, continuously passing through a ceramic membrane with the aperture of 10nm until the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution finally, and finishing the filtration;
step (4), filtering for three times: filtering the permeate obtained in the step (3) by using a membrane with the aperture of 3-5nm, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid when the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, then adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid again, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the final trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, wherein the obtained final trapped liquid is the solution enriched with the tobacco glucoside, and the trapped liquid is evaporated and concentrated to obtain viscous tobacco glucoside.
Further, in the step (1), the dry matter content of the water extract of the tobacco raw material is preferably 6 to 15%.
Further, in the step (1), the weight ratio of the tobacco raw material to water in the tobacco raw material water extract is preferably less than 1: 3.
Further, it is preferable that the weight ratio of the tobacco raw material to water is 1:5 to 1: 7.
Further, in the step (2), the membrane with the aperture of 100nm is preferably an organic membrane or an inorganic membrane, and the working pressure is less than 0.5 MPa; when the inorganic membrane is adopted, the working temperature range is 0-100 ℃; in the case of organic films, the working temperature ranges from 0 to 70 ℃.
Further, it is preferable that, in the step (3), the working pressure of the 10nm pore diameter membrane is 0.2 to 0.8 MPa.
Further, in the step (4), it is preferable that the membrane with a pore diameter of 3-5nm is an organic membrane or an inorganic membrane, and the working pressure is 0.4-1.5 MPa; when the inorganic membrane is adopted, the working temperature range is 0-100 ℃; in the case of organic films, the working temperature ranges from 0 to 70 ℃.
As an alternative technical scheme, the chemical sedimentation can also be implemented by taking diatomite as a sedimentation agent.
The invention has the following technical characteristics
(1) The enrichment of the tobacco glucoside is that other substances are removed by selecting a membrane with a proper pore size, and the method is independent of the manufacturing material of the membrane and the operation mode of the membrane.
(2) The nicotiana glycosides are relatively stable in nature and thus the temperature can be run under conditions that the membrane can tolerate.
(3) The operating pressure at which the membrane operates is well within the design of the apparatus.
(4) The running concentration (dry matter content of the extractive solution) of tobacco extractive solution is not higher than 25%, and the suitable concentration is 6-15%.
In the invention, the tobacco suspension turbid liquid obtained by centrifugation or chemical sedimentation also contains a small amount of solid matters such as silt, tobacco powder, fiber and the like;
the invention aims to retain and remove silt, tobacco powder and fiber remained in tobacco suspension, and protein, pectin and other substances which are re-aggregated and separated out.
The purpose of the secondary filtration of the present invention is to remove and retain soluble proteins and soluble pectins (which may be referred to as a soluble polymer A).
The purpose of the three-time filtration is to remove sugar, organic acid salt and inorganic acid salt, the permeate liquid is a solution containing sugar, organic acid salt and inorganic acid salt, and the retentate liquid is a solution rich in tobacco glycoside (which can be called as component B tobacco glycoside).
With respect to the film: the membrane used in the invention is not related to the material for preparing the membrane, but only related to the aperture; the temperature during membrane filtration is related to the membrane material, the inorganic membrane can be between 0 and 100 ℃, the organic membrane can be between 0 and 70 ℃ (most organic membranes are between 0 and 50 ℃), and the operating pressure: relative to the membrane pore diameter, the membrane pore diameter is generally less than 0.3MPa at 100 nm; at 10nm, generally between 0.2 and 0.5 MPa; the flow rate is not generally said to be a problem because the flow rate may be unstable due to membrane fouling in membrane filtration, which is generally between 0.2 and 1MPa at 3 to 5 nm.
Preparation of tobacco extract: the water is used as solvent, and the extraction can be carried out when the water amount and the raw material amount are more than 3:1 in weight ratio, preferably 5:1-7:1, and the extraction is carried out twice in batch mode, wherein the continuous mode has no fixed water amount and raw material amount ratio, and the extraction can be carried out under normal pressure, reduced pressure and pressurized. The temperature is 0-120 deg.C, extraction is not critical, and aqueous solution can be used for enriching glycoside.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a method for enriching glucoside substances in tobacco by utilizing the difference of molecular particle sizes of different chemical components in the tobacco and adopting the combination of membranes with the aperture of 100nm, 10nm and 3-5nm, belonging to a physical separation method. Compared with the n-butyl alcohol extraction method utilizing the polarity difference of different chemical components of tobacco, the method avoids the use of an organic solvent, the content of enriched glucoside can reach more than 85 percent, the separation yield of glucoside substances can reach more than 95 percent and is far higher than 80 percent of the separation yield of obvious n-butyl alcohol extraction method, and the method has the remarkable advantage in cost, is environment-friendly and is suitable for large-scale production.
Drawings
FIG. 1 is a process flow diagram of the tobacco glycoside enrichment method of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available by purchase.
The percentage numbers are percentages by mass unless otherwise indicated.
Example 1
A method for enriching tobacco glucoside comprises the following steps:
step (1), preparing a tobacco suspension turbid solution: centrifuging a tobacco raw material water extracting solution with the dry matter content of 15%, and removing the precipitate to obtain a tobacco suspension turbid solution;
the tobacco raw material is tobacco stems;
the chemical sedimentation takes chitosan with the mass concentration of 0.2% as a sedimentation agent;
step (2), primary filtration: filtering the tobacco suspension turbid solution obtained in the step (1) through a membrane with the aperture of 100nm, and when the volume ratio of the trapped fluid to the permeation solution is 1: 19, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped fluid, uniformly mixing, continuing to pass through a 100nm pore size membrane until the volume of the trapped fluid is 5% of the volume of the tobacco suspension turbid liquid, and finishing filtration;
and (3) secondary filtration: filtering the permeation solution obtained in the step (2) by a membrane with the aperture of 10nm, adding water with the volume of 1/10 of the tobacco suspension turbid solution into the trapped solution when the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution, uniformly mixing, continuously passing through a ceramic membrane with the aperture of 10nm until the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution finally, and finishing the filtration;
step (4), filtering for three times: filtering the permeate obtained in the step (3) by using a membrane with the aperture of 3-5nm, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid when the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, then adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid again, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the final trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, wherein the obtained final trapped liquid is the solution enriched with the tobacco glucoside, and the trapped liquid is evaporated and concentrated to obtain viscous tobacco glucoside.
In the step (1), the weight ratio of the tobacco raw material to water in the preparation process of the tobacco raw material water extracting solution is 1: 4.
In the step (2), the 100nm pore diameter membrane is an organic membrane, the working pressure is less than 0.5MPa, and the working temperature range is 0-70 ℃.
In the step (3), the working pressure of the membrane with the aperture of 10nm is 0.2-0.8 MPa.
In the step (4), the membrane with the aperture of 3-5nm is an inorganic membrane, the working pressure is 0.4-1.5MPa, and the working temperature range is 0-100 ℃.
Example 2
A method for enriching tobacco glucoside comprises the following steps:
step (1), preparing a tobacco suspension turbid solution: centrifuging a tobacco raw material water extracting solution with the dry matter content of 6%, and removing precipitates to obtain a tobacco suspension turbid solution;
the tobacco raw material is tobacco powder;
the chemical sedimentation takes chitosan with the mass concentration of 0.2% as a sedimentation agent;
step (2), primary filtration: filtering the tobacco suspension turbid solution obtained in the step (1) through a membrane with the aperture of 100nm, and when the volume ratio of the trapped fluid to the permeation solution is 1: 19, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped fluid, uniformly mixing, continuing to pass through a 100nm pore size membrane until the volume of the trapped fluid is 5% of the volume of the tobacco suspension turbid liquid, and finishing filtration;
and (3) secondary filtration: filtering the permeation solution obtained in the step (2) by a membrane with the aperture of 10nm, adding water with the volume of 1/10 of the tobacco suspension turbid solution into the trapped solution when the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution, uniformly mixing, continuously passing through a ceramic membrane with the aperture of 10nm until the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution finally, and finishing the filtration;
step (4), filtering for three times: filtering the permeate obtained in the step (3) by using a membrane with the aperture of 3-5nm, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid when the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, then adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid again, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the final trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, wherein the obtained final trapped liquid is the solution enriched with the tobacco glucoside, and the trapped liquid is evaporated and concentrated to obtain viscous tobacco glucoside.
Wherein in the step (1), the weight ratio of the tobacco raw material to the water is 1:5 in the preparation process of the tobacco raw material water extracting solution.
In the step (2), the 100nm aperture membrane is an inorganic membrane, the working pressure is less than 0.5MPa, and the working temperature range is 0-100 ℃.
In the step (3), the working pressure of the membrane with the aperture of 10nm is 0.2-0.8 MPa.
In the step (4), the working pressure of the organic membrane with the aperture of 3-5nm is 0.4-1.5MPa, and the working temperature range is 0-70 ℃.
Example 3
A method for enriching tobacco glucoside comprises the following steps:
step (1), preparing a tobacco suspension turbid solution: chemically settling a tobacco raw material water extract with the dry matter content of 25%, and then discarding the precipitate to obtain a tobacco suspension turbid solution;
the tobacco raw material is tobacco leaves;
the chemical sedimentation takes diatomite as a sedimentation agent;
step (2), primary filtration: filtering the tobacco suspension turbid solution obtained in the step (1) through a membrane with the aperture of 100nm, and when the volume ratio of the trapped fluid to the permeation solution is 1: 19, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped fluid, uniformly mixing, continuing to pass through a 100nm pore size membrane until the volume of the trapped fluid is 5% of the volume of the tobacco suspension turbid liquid, and finishing filtration;
and (3) secondary filtration: filtering the permeation solution obtained in the step (2) by a membrane with the aperture of 10nm, adding water with the volume of 1/10 of the tobacco suspension turbid solution into the trapped solution when the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution, uniformly mixing, continuously passing through a ceramic membrane with the aperture of 10nm until the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution finally, and finishing the filtration;
step (4), filtering for three times: filtering the permeate obtained in the step (3) by using a membrane with the aperture of 3-5nm, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid when the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, then adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid again, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the final trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, wherein the obtained final trapped liquid is the solution enriched with the tobacco glucoside, and the trapped liquid is evaporated and concentrated to obtain viscous tobacco glucoside.
In the step (1), the weight ratio of the tobacco raw material to water in the preparation process of the tobacco raw material water extracting solution is 1: 7.
In the step (2), the 100nm aperture membrane is an inorganic membrane, the working pressure is less than 0.5MPa, and the working temperature range is 0-100 ℃.
In the step (3), the working pressure of the membrane with the aperture of 10nm is 0.2-0.8 MPa.
In the step (4), the membrane with the aperture of 3-5nm is an inorganic membrane, the working pressure is 0.4-1.5MPa, and the working temperature range is 0-100 ℃.
Example 4
A method for enriching tobacco glucoside comprises the following steps:
step (1), preparing a tobacco suspension turbid solution: chemically settling a tobacco raw material water extracting solution with the dry matter content of 20%, and then discarding the precipitate to obtain a tobacco suspension turbid solution;
the tobacco raw materials are tobacco stems and tobacco powder; (mass ratio is 1: 1)
The chemical sedimentation takes chitosan with the mass concentration of 0.2% as a sedimentation agent;
step (2), primary filtration: filtering the tobacco suspension turbid solution obtained in the step (1) through a membrane with the aperture of 100nm, and when the volume ratio of the trapped fluid to the permeation solution is 1: 19, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped fluid, uniformly mixing, continuing to pass through a 100nm pore size membrane until the volume of the trapped fluid is 5% of the volume of the tobacco suspension turbid liquid, and finishing filtration;
and (3) secondary filtration: filtering the permeation solution obtained in the step (2) by a membrane with the aperture of 10nm, adding water with the volume of 1/10 of the tobacco suspension turbid solution into the trapped solution when the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution, uniformly mixing, continuously passing through a ceramic membrane with the aperture of 10nm until the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution finally, and finishing the filtration;
step (4), filtering for three times: filtering the permeate obtained in the step (3) by using a membrane with the aperture of 3-5nm, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid when the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, then adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid again, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the final trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, wherein the obtained final trapped liquid is the solution enriched with the tobacco glucoside, and the trapped liquid is evaporated and concentrated to obtain viscous tobacco glucoside.
In the step (1), the weight ratio of the tobacco raw material to water in the preparation process of the tobacco raw material water extracting solution is 1: 6.
In the step (2), the 100nm aperture membrane is an organic membrane or an inorganic membrane, and the working pressure is less than 0.5 MPa; when the inorganic membrane is adopted, the working temperature range is 0-100 ℃; in the case of organic films, the working temperature ranges from 0 to 70 ℃.
In the step (3), the working pressure of the membrane with the aperture of 10nm is 0.2-0.8 MPa.
In the step (4), the working pressure of the organic membrane with the aperture of 3-5nm is 0.4-1.5MPa, and the working temperature range is 0-70 ℃.
Example 5
A method for enriching tobacco glucoside comprises the following steps:
step (1), preparing a tobacco suspension turbid solution: chemically settling a tobacco raw material water extracting solution with the dry matter content of 10%, and then discarding the precipitate to obtain a tobacco suspension turbid solution;
the tobacco raw materials are tobacco stems, tobacco powder and tobacco leaves; (mass ratio is 1: 1: 2)
The chemical sedimentation takes chitosan with the mass concentration of 0.2% as a sedimentation agent;
step (2), primary filtration: filtering the tobacco suspension turbid solution obtained in the step (1) through a membrane with the aperture of 100nm, and when the volume ratio of the trapped fluid to the permeation solution is 1: 19, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped fluid, uniformly mixing, continuing to pass through a 100nm pore size membrane until the volume of the trapped fluid is 5% of the volume of the tobacco suspension turbid liquid, and finishing filtration;
and (3) secondary filtration: filtering the permeation solution obtained in the step (2) by a membrane with the aperture of 10nm, adding water with the volume of 1/10 of the tobacco suspension turbid solution into the trapped solution when the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution, uniformly mixing, continuously passing through a ceramic membrane with the aperture of 10nm until the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution finally, and finishing the filtration;
step (4), filtering for three times: filtering the permeate obtained in the step (3) by using a membrane with the aperture of 3-5nm, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid when the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, then adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid again, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the final trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, wherein the obtained final trapped liquid is the solution enriched with the tobacco glucoside, and the trapped liquid is evaporated and concentrated to obtain viscous tobacco glucoside.
In the step (1), the weight ratio of the tobacco raw material to water in the preparation process of the tobacco raw material water extracting solution is 1: 8.
In the step (2), the 100nm pore diameter membrane is an organic membrane, the working pressure is less than 0.5MPa, and the working temperature range is 0-70 ℃.
In the step (3), the working pressure of the membrane with the aperture of 10nm is 0.2-0.8 MPa.
In the step (4), the working pressure of the organic membrane with the aperture of 3-5nm is 0.4-1.5MPa, and the working temperature range is 0-70 ℃.
Comparative example 1
Comparative example 1 differs from example 5 in that: and (3) when the volume ratio of the trapped fluid to the permeated fluid in the step (2) is 1: 19, the modification is that when the volume ratio of the trapped liquid to the permeated liquid is 1: and (15) hours.
Comparative example 2
Comparative example 2 differs from example 5 in that: the dry matter content of the tobacco raw material water extract was 35%.
Comparative example 3
Comparative example 3 differs from example 5 in that: the step (4) is modified as follows: and (3) filtering for three times: filtering the permeate obtained in the step (3) by using a membrane with the aperture of 3-5nm, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the retentate when the volume of the retentate is 5% of the volume of the tobacco suspension turbid liquid, uniformly mixing, continuously passing through the membrane with the aperture of 3-5nm until the volume of the retentate is 5% of the volume of the tobacco suspension turbid liquid, obtaining the retentate which is the solution enriched with the tobacco glucoside, and evaporating and concentrating the retentate to obtain the tobacco glucoside.
Evaluation of technical Effect
The inventive examples, comparative examples and n-butanol extraction method were compared, and the results are shown in table 1.
TABLE 1
From the aspect of enrichment yield and purity of the table 1, the method has significant advantages over the traditional n-butanol extraction method. The examples of the invention and the comparative examples have excellent effects, which shows that the upper step and the lower step of the invention have good synergistic effect.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The method for enriching the tobacco glucoside is characterized by comprising the following steps of:
step (1), preparing a tobacco suspension turbid solution: centrifuging or chemically settling the tobacco raw material water extract with dry matter content not higher than 25%, and removing the precipitate to obtain tobacco suspension;
the tobacco raw material is at least one of tobacco stems, tobacco powder and tobacco leaves;
the chemical sedimentation takes chitosan with the mass concentration of 0.2% as a sedimentation agent;
step (2), primary filtration: filtering the tobacco suspension turbid solution obtained in the step (1) through a membrane with the aperture of 100nm, and when the volume ratio of the trapped fluid to the permeation solution is 1: 19, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped fluid, uniformly mixing, continuing to pass through a 100nm pore size membrane until the volume of the trapped fluid is 5% of the volume of the tobacco suspension turbid liquid, and finishing filtration;
and (3) secondary filtration: filtering the permeation solution obtained in the step (2) by a membrane with the aperture of 10nm, adding water with the volume of 1/10 of the tobacco suspension turbid solution into the trapped solution when the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution, uniformly mixing, continuously passing through a ceramic membrane with the aperture of 10nm until the volume of the trapped solution is 5 percent of the volume of the tobacco suspension turbid solution finally, and finishing the filtration;
step (4), filtering for three times: filtering the permeate obtained in the step (3) by using a membrane with the aperture of 3-5nm, adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid when the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, then adding water with the volume of 1/10 of the tobacco suspension turbid liquid into the trapped liquid again, continuously passing through the membrane with the aperture of 3-5nm after uniformly mixing until the volume of the final trapped liquid is 5% of the volume of the tobacco suspension turbid liquid, wherein the obtained final trapped liquid is the solution enriched with the tobacco glucoside, and the trapped liquid is evaporated and concentrated to obtain the tobacco glucoside;
in the step (1), the dry matter content of the water extract of the tobacco raw material is 6-15%;
in the step (2), the 100nm aperture membrane is an organic membrane or an inorganic membrane, and the working pressure is less than 0.5 MPa; when the inorganic membrane is adopted, the working temperature range is 0-100 ℃; in the case of organic films, the working temperature ranges from 0 to 70 ℃.
2. The method for enriching a nicotiana glycosides as claimed in claim 1, wherein in step (1), the weight ratio of the tobacco material to water in the aqueous extract of tobacco material is less than 1: 3.
3. The method of enriching a nicotiana glycosides as claimed in claim 2, wherein the weight ratio of the tobacco material to the water is 1:5-1: 7.
4. The method for enriching nicotiana glycosides as claimed in claim 1, wherein the operating pressure of the membrane having a pore size of 10nm in the step (3) is 0.2 to 0.8 MPa.
5. The method for enriching nicotiana glycosides according to claim 1, wherein in step (4), the membrane having a pore size of 3 to 5nm is an organic membrane or an inorganic membrane, and the operating pressure is 0.4 to 1.5 MPa; when the inorganic membrane is adopted, the working temperature range is 0-100 ℃; in the case of organic films, the working temperature ranges from 0 to 70 ℃.
6. The method of claim 1, wherein the chemical sedimentation is performed using diatomaceous earth as a sedimentation agent.
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| US3883425A (en) * | 1973-12-10 | 1975-05-13 | Wadley Res Inst & Blood Bank | Detoxification of saponins |
| JPS591717B2 (en) * | 1981-06-20 | 1984-01-13 | 日本たばこ産業株式会社 | Loliolide-β-D-glucoside and a tobacco flavor improver comprising the compound |
| CN1058971C (en) * | 1995-02-11 | 2000-11-29 | 国内贸易部西安油脂科学研究设计院 | Prodn. technology for extracting fine sasanquasaponin by super filtration film method |
| CN101407537A (en) * | 2008-10-28 | 2009-04-15 | 姜涛 | Method for cleanly producing saponin by comprehensively utilizing turmeric |
| CN101401897A (en) * | 2008-11-06 | 2009-04-08 | 云南白药集团股份有限公司 | Edulcoration purification process for rhizoma paris saponin extract solution |
| CN102127121A (en) * | 2010-12-29 | 2011-07-20 | 华宝食用香精香料（上海）有限公司 | Method for extracting glucoside compound from tobacco leaves |
| CN103497987B (en) * | 2013-09-16 | 2015-02-25 | 陕西科技大学 | Clean production method of yam diosgenin |
| CN104849393A (en) * | 2015-06-09 | 2015-08-19 | 安徽中烟工业有限责任公司 | Method for determining glucosidic bonded fragrance component in tobacco |
| CN105112482A (en) * | 2015-08-20 | 2015-12-02 | 大连润伟海参研发科技有限公司 | Method for extracting peptides, polysaccharides, saponin and lipid from viscera of sea cucumber |
| CN106565813B (en) * | 2016-09-26 | 2018-06-19 | 中国林业科学研究院亚热带林业研究所 | The processing method that a kind of Tea Saponin continuously purifies |
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