CN108095187B - Method for enriching tobacco glucoside - Google Patents
Method for enriching tobacco glucoside Download PDFInfo
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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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- 241000208125 Nicotiana Species 0.000 title claims abstract description 208
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 206
- 238000000034 method Methods 0.000 title claims abstract description 31
- 229930182478 glucoside Natural products 0.000 title description 33
- 150000008131 glucosides Chemical class 0.000 title description 33
- 239000012528 membrane Substances 0.000 claims abstract description 116
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000002994 raw material Substances 0.000 claims abstract description 36
- 239000011148 porous material Substances 0.000 claims abstract description 28
- 229930182470 glycoside Natural products 0.000 claims abstract description 26
- 150000002338 glycosides Chemical class 0.000 claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 26
- 238000004062 sedimentation Methods 0.000 claims abstract description 21
- 239000012465 retentate Substances 0.000 claims abstract description 20
- 239000012466 permeate Substances 0.000 claims abstract description 12
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 239000000725 suspension Substances 0.000 claims description 96
- 239000007788 liquid Substances 0.000 claims description 95
- 238000001914 filtration Methods 0.000 claims description 57
- 238000002156 mixing Methods 0.000 claims description 29
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 229920001661 Chitosan Polymers 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 235000019504 cigarettes Nutrition 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000013049 sediment Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 86
- 239000012530 fluid Substances 0.000 description 20
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 8
- 238000000605 extraction Methods 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 6
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- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 239000001814 pectin Substances 0.000 description 2
- 235000010987 pectin Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- TWCMVXMQHSVIOJ-UHFFFAOYSA-N Aglycone of yadanzioside D Natural products COC(=O)C12OCC34C(CC5C(=CC(O)C(O)C5(C)C3C(O)C1O)C)OC(=O)C(OC(=O)C)C24 TWCMVXMQHSVIOJ-UHFFFAOYSA-N 0.000 description 1
- PLMKQQMDOMTZGG-UHFFFAOYSA-N Astrantiagenin E-methylester Natural products CC12CCC(O)C(C)(CO)C1CCC1(C)C2CC=C2C3CC(C)(C)CCC3(C(=O)OC)CCC21C PLMKQQMDOMTZGG-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
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- PFOARMALXZGCHY-UHFFFAOYSA-N homoegonol Natural products C1=C(OC)C(OC)=CC=C1C1=CC2=CC(CCCO)=CC(OC)=C2O1 PFOARMALXZGCHY-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
本发明涉及一种烟草糖苷的富集方法，属于卷烟生产技术领域。本发明根据烟草不同化学成分的理化性质差异，利用100nm、10nm、3‑5nm孔径膜的组合运用，除去烟草中的非糖苷物质富集烟草糖苷。烟草原料的水提取物经离心或化学沉降除杂后，采用100nm孔径膜除去泥沙、烟草碎末、纤维等固形物制备成烟草提取液的真溶液，该真溶液经10nm孔径膜过滤处理，除去溶液中的可溶性高分子物质，10nm孔径膜的透过液再经3‑5nm孔径膜过滤处理除去糖、盐等杂质，3‑5nm孔径膜的截留液即为富集了烟草糖苷的溶液。该技术方法不需要使用有机溶剂，环境友好，具有经济性好，烟草糖苷富集收率高，适用规模化生产等优点。
The invention relates to a method for enriching tobacco glycosides, belonging to the technical field of cigarette production. According to the difference in physical and chemical properties of different chemical components of tobacco, the invention utilizes the combined application of 100nm, 10nm and 3-5nm pore membranes to remove non-glycoside substances in tobacco and enrich tobacco glycosides. After the water extract of the tobacco raw material is removed by centrifugation or chemical sedimentation, a 100nm pore size membrane is used to remove solids such as sediment, tobacco fines and fibers to prepare a true solution of the tobacco extract, and the true solution is filtered through a 10nm pore size membrane, The soluble macromolecular substances in the solution are removed, the permeate of the 10nm pore membrane is filtered through a 3-5nm pore membrane to remove impurities such as sugar and salt, and the retentate of the 3-5nm pore membrane is a solution enriched with tobacco glycosides. The technical method does not need to use an organic solvent, is environmentally friendly, has the advantages of good economy, high enrichment yield of tobacco glycosides, and is suitable for large-scale production.
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)
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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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