CN101586056A - Method for preparing rehmanniae flavor for cigarette by using membrane separation technique - Google Patents
Method for preparing rehmanniae flavor for cigarette by using membrane separation technique Download PDFInfo
- Publication number
- CN101586056A CN101586056A CNA2008100477477A CN200810047747A CN101586056A CN 101586056 A CN101586056 A CN 101586056A CN A2008100477477 A CNA2008100477477 A CN A2008100477477A CN 200810047747 A CN200810047747 A CN 200810047747A CN 101586056 A CN101586056 A CN 101586056A
- Authority
- CN
- China
- Prior art keywords
- cigarette
- film
- rehmanniae
- liquor
- flavor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 48
- 239000012528 membrane Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000000796 flavoring agent Substances 0.000 title claims abstract description 35
- 235000019634 flavors Nutrition 0.000 title claims abstract description 28
- 238000000926 separation method Methods 0.000 title claims abstract description 24
- 239000000706 filtrate Substances 0.000 claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 238000010992 reflux Methods 0.000 claims abstract description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 241000405414 Rehmannia Species 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 23
- 238000005516 engineering process Methods 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 3
- 206010013911 Dysgeusia Diseases 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- 235000013599 spices Nutrition 0.000 description 10
- 235000009508 confectionery Nutrition 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000003546 flue gas Substances 0.000 description 8
- 239000012716 precipitator Substances 0.000 description 8
- 239000003814 drug Substances 0.000 description 7
- 235000013355 food flavoring agent Nutrition 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 230000000391 smoking effect Effects 0.000 description 5
- 210000001124 body fluid Anatomy 0.000 description 4
- 239000010839 body fluid Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 239000002304 perfume Substances 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 241000208125 Nicotiana Species 0.000 description 3
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 3
- 239000008280 blood Substances 0.000 description 3
- 210000004369 blood Anatomy 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 235000019633 pungent taste Nutrition 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000003203 everyday effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001471 micro-filtration Methods 0.000 description 2
- 238000001728 nano-filtration Methods 0.000 description 2
- 235000010987 pectin Nutrition 0.000 description 2
- 229920001277 pectin Polymers 0.000 description 2
- 239000001814 pectin Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 description 1
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 description 1
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 description 1
- QIIDATRCGITYRZ-UHFFFAOYSA-N Catalpol Natural products OCC1OC(OC2OC=CC3C(O)C(=C(CO)C23)O)C(O)C(O)C1O QIIDATRCGITYRZ-UHFFFAOYSA-N 0.000 description 1
- 241000721047 Danaus plexippus Species 0.000 description 1
- 244000167230 Lonicera japonica Species 0.000 description 1
- 235000017617 Lonicera japonica Nutrition 0.000 description 1
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 description 1
- 241000013557 Plantaginaceae Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- BLUAFEHZUWYNDE-NNWCWBAJSA-N artemisinin Chemical compound C([C@](OO1)(C)O2)C[C@H]3[C@H](C)CC[C@@H]4[C@@]31[C@@H]2OC(=O)[C@@H]4C BLUAFEHZUWYNDE-NNWCWBAJSA-N 0.000 description 1
- 229960004191 artemisinin Drugs 0.000 description 1
- 229930101531 artemisinin Natural products 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- LHDWRKICQLTVDL-PZYDOOQISA-N catalpol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@H]1[C@@H]2[C@@]3(CO)O[C@H]3[C@@H](O)[C@@H]2C=CO1 LHDWRKICQLTVDL-PZYDOOQISA-N 0.000 description 1
- UXSACQOOWZMGSE-UHFFFAOYSA-N catalposide Natural products OC1C(O)C(O)C(CO)OC1OC1C2C3(CO)OC3C(OC(=O)C=3C=CC(O)=CC=3)C2C=CO1 UXSACQOOWZMGSE-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 1
- 229940074393 chlorogenic acid Drugs 0.000 description 1
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 description 1
- 235000001368 chlorogenic acid Nutrition 0.000 description 1
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- LHDWRKICQLTVDL-UHFFFAOYSA-N methyl iridoid glycoside Natural products OC1C(O)C(O)C(CO)OC1OC1C2C3(CO)OC3C(O)C2C=CO1 LHDWRKICQLTVDL-UHFFFAOYSA-N 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000011146 sterile filtration Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
Abstract
The invention discloses a method for preparing rehmanniae flavor for cigarette by using the membrane separation technique, belonging to the technical field of cigarette flavor preparation. The method is carried out according to the following steps: carrying out reflux extraction twice, obtaining the filtrate of rehmanniae extract A; filtering by a ceramic membrane with the aperture of 100nm, and obtaining the solution passing through the membrane called a filtrate B; and filtering the filtrate B through an organic spiral-wound membrane with the trapping molecular weight of 25 thousand, obtaining a filtrate C which is the rehmanniae flavor for cigarette. The method is simple, is easily implemented, and uses membrane separation technique to replace the original precipitation remelting method. The invention has the advantages of simple technology, short production period, low cost, remarkable economic benefits, improvement of automazation degree and enhancement of controllability of production technology, and solves the problems of aftertaste and remaining of cigarettes in mouths.
Description
Technical field
The invention belongs to the cigarette flavors preparing technical field, is a kind of method with membrane separation technique preparation and production rehmanniae flavor for cigarette specifically.
Background technology
Glutinous rehmannia is the piece root of scrophulariaceae Scrophulariaceae plant glutinous rehmannia Rehmanniae glutinosa (Gaertn.) Libosch.ex.Fisch.et Mey, is divided into Rehmannia Root, Radix Rehmanniae and Radix Rehmanniae Preparata according to the concocting method difference.Catalpol is as the index substance of Rehmannia Root and Radix Rehmanniae at present, and 5-HMF is widely used as the index substance of Radix Rehmanniae Preparata.Radix Rehmanniae has nourishing Yin and clearing heat effect, and Radix Rehmanniae Preparata has the effect that marrow is filled out in the enriching yin of enriching blood, beneficial essence, is good nourishing YIN and supplementing blood medicine, be described as " strengthening renal yin to inhibit predominant yang, the monarch who enriches blood ", glutinous rehmannia contains the number of chemical composition, clinical application is more and more wider, is a rising multifunctional drug.
Response State Bureau's " 11th Five-Year development in science and technology outline ", the low harm of exploitation Chinese style cigarette, glutinous rehmannia has been used for suitability for industrialized production as essence spice for cigarette.Present production technique is that Radix Rehmanniae extract is further extracted purifying with precipitating back molten method, prepares to be fit to the glutinous rehmannia essence and flavoring agent that cigarette is used.Yet this production technique is comparatively complicated, and length consuming time, and the production cycle is long, and the people consumes greatly, and production cost is higher accordingly, the more important thing is that single precipitation returns molten method and can't solve the glutinous rehmannia essence and flavoring agent to the residual bigger negative impact of cigarette pleasant impression.
Summary of the invention
At the above-mentioned deficiency of prior art, the technical problem to be solved in the present invention provides and a kind ofly prepares the method for rehmanniae flavor for cigarette with membrane separation technique, shortens the production cycle, solves the negative impact of rehmanniae flavor for cigarette to the cigarette pleasant impression simultaneously.
The method for preparing rehmanniae flavor for cigarette with membrane separation technique is carried out according to the following steps:
(1) glutinous rehmannia is clayed into power after, 1 part of weight glutinous rehmannia adds the ethanolic soln of 6-10 part weight, refluxing extraction 3-5 hour after-filtration under 100-135 ℃ temperature keeps filtrate, filter residue is used for next step;
(2) filter residue that previous step is rapid adds the ethanolic soln of step (1) equivalent, and refluxing extraction 3-5 hour after-filtration merges filtrate twice under 100-135 ℃ temperature, and gained filtrate is Radix Rehmanniae extract A;
(3) Radix Rehmanniae extract A is crossed the ceramic membrane that pore size is 100nm (one-level film), when beginning to bubble in the glutinous rehmannia extract A system, the water that adds Radix Rehmanniae extract A gross weight 10%-20%, the solution by film is called liquor B, and the solution by film is not called concentrated solution B; When not having liquor B to flow out, stopper film is handled operation;
(4) liquor B being crossed molecular weight cut-off is organic rolled film (secondary film) of 2.5 ten thousand, when beginning to bubble in the liquor B system, the water that adds the 10%-20% of liquor B gross weight, solution by film is called liquor C, the solution by film is not called concentrated solution C, when not having liquor C to flow out, stopper film is handled operation;
The gained liquor C is rehmanniae flavor for cigarette.
Described ethanolic soln is that volumn concentration is the ethanolic soln of 30%-60%.
Described pore size excessively is the ceramic membrane of 100nm, and flow velocity is 50-70L/h, and temperature is controlled at below 45 ℃, and intake pressure is 1.8-2.2MPa, and top hole pressure is 1.0-1.4MPa.
Described molecular weight cut-off excessively is organic rolled film of 2.5 ten thousand, and flow velocity is 15-25L/h, and temperature is controlled at below 45 ℃, and intake pressure is 0.6-1.0MPa, and top hole pressure is 0.5-0.7MPa.
The fineness of described glutinous rehmannia is the 80-100 order.
Described glutinous rehmannia is meant Rehmannia Root or Radix Rehmanniae or Radix Rehmanniae Preparata or the mixture among them.
Method of the present invention is simple, implements easily, substitutes original precipitation with membrane separation technique and returns molten method, and have the following advantages: 1. technology is simple.2. with short production cycle, cost is low, has remarkable economic efficiency.3. level of automation improves, and the controllability of production technique strengthens.4. the oral cavity pleasant impression and the residue problem of cigarette have been solved.
Embodiment
Below relevant technical problem of the present invention is described in further detail.Membrane separation technique is to utilize film that each component of mixture is selected diactinic difference, realizes separation, purification, spissated new separation technology.Size according to membrane pore size is divided, and film commonly used has four kinds of microfiltration membrane, ultra-filtration membrane, nanofiltration membrane and reverse osmosis membranes.The particle that with film is 0.05-10 μ m to diameter is a microfiltration membrane with the film that other solution or other lower-molecular-weight components separate; Being used for macromole or diameter are not more than the film that the particulate of 0.10 μ m separates is ultra-filtration membrane; And to be used for the isolated molecule amount be hundreds of to the film of several thousand mixture solution be nanofiltration membrane.The aperture of film is more little, and the material that is trapped is many more, and the material that penetrates film is few more, and then the purity of resulting filtrate is just high more.The present invention controls the required purity of filtrate, thereby prepares the rehmanniae flavor for cigarette with different flavor feature by selecting the film of different sorts and aperture/molecular weight cut-off size.
The application of membrane separation technique in Chinese medicine preparation starts from late 1980s to the beginning of the nineties, and up to now, relevant bibliographical information is many.Wherein, the main effect of membrane technique is to extract a certain monomeric compound of preparation from the mixture of complexity, and the target product of its technological line is single compound, and is pure more good more.As from hay, extract hay acid, from Japanese Honeysuckle chlorogenic acid extracting, from Herba Artemisiae annuae, extract Artemisinin or the like.Yet cigarette product itself is exactly a complicated system, and combustion processes has more been deepened its complicacy.Essence and flavoring agent in the tobacco through the comfortable flavor characteristic of pleasant of the burning back cigarette of giving be many-sided factor comprehensively, the effect of balance and coordination.Therefore sometimes single pure product are added to as essence and flavoring agent and go in the cigarette that effect is bad on the contrary, and several or multiple mixture with certain flavour characteristic compound joins and has good effect in the cigarette on the contrary.Therefore, the needed target product of essence spice for cigarette is not pure more good more.On the other hand, if the composition that is contained in the essence and flavoring agent is too many, contingent chemical reaction increases in the cigarette burning process so, also may produce more other cigarette is had the compound of negative impact, cause cigarette pleasant impression, residual etc. negative effect arranged.Therefore, essence spice for cigarette is too pure bad, and contained material is also bad too much, and it needs one " suitable purity ".Simultaneously, well-known, target product is pure more, and preparation technology is complicated more, and production cost is also high more.Therefore, the application of membrane separation technique in essence spice for cigarette compared with the application in the Chinese medicine preparation of having reported, no matter is that the both is completely different on starting point or technical thought.
The one-level film of technical scheme of the present invention in (3) step selected the ceramic membrane of 100nm, mainly is separation and the sterile filtration that is used for the solution suspended substance, removes macromolecular cpds such as a part of protein, pectin simultaneously.Owing to contain certain density ethanol among the Radix Rehmanniae extract A, therefore select ceramic membrane.And the secondary film in (4) step to select molecular weight cut-off be organic rolled film of 2.5 ten thousand, mainly be that only to keep molecular weight be 2.5 ten thousand and following compound, organic rolled film helps to improve membrane flux, and follow-up easy to clean, simple.
For the ease of comparative analysis, the chosen process of the applicant to described " suitable purity " also is described, the applicant has carried out following test.After carrying out 1,2,3 steps with technical scheme of the present invention, to cross molecular weight cut-off once more be organic rolled film of 1.5 ten thousand (molecular weight cut-off is that 2.5 ten thousand secondary film parameter is identical in other parameter and the technical scheme) with having crossed liquor B behind the one-level film, and the filtrate that obtains is called filtrate D; The Radix Rehmanniae extract A that step 1 of the present invention, 2 is obtained separates purification with traditional precipitator method, and the rehmanniae flavor for cigarette of preparation is called extracting solution E.
The Radix Rehmanniae extract A that step 1 of the present invention, 2 is obtained, liquor B, C, D, and separate the extracting solution E of purification with traditional precipitator method with different membrane sepn preparations, join respectively in the middle-grade blank pipe tobacco of flavoring and casing not, and to the sample cigarette contrast experiment that smokes panel test, smoking result sees Table 1.From smoking result as can be seen, handle through film and the effect of smokeing panel test of the Radix Rehmanniae extract A that the precipitator method are handled the not poorest, it is big to show that mainly throat stimulates, residual seriously; And effective through the sample after the film processing than the sample of precipitator method processing, show that mainly the former flue gas matter is better, and sweet sense is arranged and the sense of promoting the production of body fluid, inhale the flavor pleasant; And between the sample through the film processing difference being arranged also, the quality of smoking result is: the film (liquor B) of film (filtrate the D)＞100nm of the film of 2.5 ten thousand molecular weight (liquor C)＞1.5 ten thousand molecular weight.The pore size of three kinds of films is: the film of the film of the film of 100nm＞2.5 ten thousand molecular weight＞1.5 ten thousand molecular weight, and the aperture of film is more little, and the material that is trapped is many more, and the material that permeates come (being filtrate) is few more, and then the purity of filtrate is high more, and vice versa.Therefore, the purity through the filtrate after three kinds of films processing is: filtrate D＞liquor C＞liquor B＞sample E＞Radix Rehmanniae extract A.From smoking result as can be seen, the filtrate that obtains by membrane separation technique is not pure more good more during as essence and flavoring agent, and the material that is contained is few more good more; The material that neither be contained is The more the better.This also is the singularity that membrane separation technique is used in the tobacco flavour fragrance industry.
Table 1, smoking result
| Sample | Smell perfume (or spice) | Odour characteristics | The flue gas feature | Inhale the flavor feature |
| A | Do not have | Perfume quantity has increase slightly, and outer perfuming is coordinated | Flue gas changes little | Pungency is bigger, and pleasant impression is residual serious, and puckery sense is arranged. |
| Liquor B | A little less than in fragrant and sweet | Perfume quantity increases, the obvious and coordination of outer perfuming | The soft sophistication of flue gas increases, and concentration increases | The sweet sense and the sense of promoting the production of body fluid slightly increase, and pungency slightly reduces |
| Liquor C | Fragrant and sweet strong | Fragrance enriches plentiful, and is strong, obvious, the coordination of outer perfuming | Flue gas concentration increases, the soft exquisiteness of flue gas, and conglobation property is good | The sweet sense and the sense of promoting the production of body fluid obviously increase, and be non-stimulated and residual, and pleasant impression is clean comfortable joyful, and sweet sense is arranged back |
| Filtrate D | Fragrant and sweet strong | Fragrance enriches plentiful, and outer perfuming is obviously coordinated | Flue gas concentration increases, and conglobation property is good, exquisiteness | The sweet sense and the sense of promoting the production of body fluid obviously increase, and excitement reduces, and is slightly residual, and sweet sense is arranged back |
| E | Do not have | Perfume quantity increases, and outer perfuming is obviously coordinated | Flue gas concentration increases, | Pungency slightly reduces, and has residual |
Cause cigarette odor-absorbing, especially one of residual factor of excitement, pleasant impression is that macromolecular cpd burning in the additive causes, and the class material that protein and pectin come to this.The Radix Rehmanniae extract A that the applicant obtains step 1 of the present invention, 2, measure with liquor B, C and the D of membrane separation technique preparation and the protein content that separates with traditional precipitator method among the extracting solution E of purification, protein content in every kind of sample all with Radix Rehmanniae extract A in compare, show the characteristic (seeing Table 2) of each sample with the reduced rate of protein content.
Table 2 protein content reduced rate
| Sample | The protein reduced rate |
| Radix Rehmanniae extract A | 0％ |
| Liquor B | 70％ |
| Liquor C | 88％ |
| Filtrate D | 90％ |
| Extracting solution E | 40％ |
Protein content all reduces greatly than the content that tradition precipitate back among the extracting solution E that molten method obtains in the filtrate after handling through film shown in the last table, so the essence and flavoring agent after the film processing is aspect the pleasant impression of cigarette and mouthfeel far better (seeing Table 1).And through different film treating processess, Protein content is also different in the filtrate: liquor B＞liquor C＞filtrate D's, but liquor C but is more suitable for doing essence spice for cigarette than filtrate D.This mainly is that and the protein content difference is little among liquor C and the D because protein also just influences one of factor of cigarette mouthfeel, so neither protein content in essence spice for cigarette low more good more, material purity be high more good more.This also is the example that extract of the present invention will have suitable purity.
Because membrane separation technique is used for suitability for industrialized production, so the production cycle of this technology is the problem that must consider.The applicant is than the production cycle of right membrane technique method and two kinds of methods production of traditional precipitator method rehmanniae flavor for cigarette.Experiment is found, use the weak point of the production cycle of membrane technique method than traditional precipitator method, and the amount of the rehmanniae flavor for cigarette of preparation is many more, and the production cycle difference of two kinds of methods is big more, and particular case sees Table 3.
Table 3, two kinds of method production cycle comparisons
From people's consumption aspect, traditional precipitator method need 5 of operator every day, and the average operation time be 8 hours at least, and the membrane separating method after improving only needs 2 of operator every day, and only 6 hours average operation time, the employee also has certain time of having a rest.Therefore the technology after improving has tangible economic benefit than traditional technology.
Be several embodiment below.
Embodiment 1:
(1) Radix Rehmanniae Preparata is clayed into power after, get the glutinous rehmannia of 1 times of weight, add the ethanolic soln of 40% (volumn concentration) of 6 times of weight, under 120 ℃ temperature refluxing extraction 3-5 hour, filter.
(2) will step (1) filter the ethanolic soln that adds 40% (volumn concentration) of 6 times of crude drug weight in the remaining filter residue in back, under 120 ℃ temperature, continued refluxing extraction 4 hours, filter and merge filtrate twice, obtain Radix Rehmanniae extract A.
(3) Radix Rehmanniae extract A is at first crossed the ceramic membrane (one-level film) that pore size is 100nm, flow velocity is 65L/h, and temperature is controlled at below 45 ℃, and intake pressure is 2.0MPa, and top hole pressure is 1.2MPa.When beginning to bubble in the glutinous rehmannia extract A system, add 10% water of Radix Rehmanniae extract gross weight, be used to improve the yield of target product.To be designated as liquor B by the solution of film, the solution by film is not designated as concentrated solution B.When not having liquor B to flow out, stopper film is handled operation.
(4) liquor B being crossed once more a molecular weight cut-off is organic rolled film (secondary film) of 2.5 ten thousand, and flow velocity is 20L/h, and temperature is controlled at below 45 ℃, and intake pressure is 0.8MPa, and top hole pressure is 0.6MPa.When beginning to bubble in the liquor B system, add 10% water of liquor B gross weight, be used to improve the yield of target product.To be designated as liquor C by the solution of film, the solution by film is not designated as concentrated solution C.When not having liquor C to flow out, stopper film is handled operation.
Liquor C is essence spice for cigarette, stores for future use.
Embodiment 2:
(1) Radix Rehmanniae is clayed into power after, get the glutinous rehmannia of 1 times of weight, add the ethanolic soln of 50% (volumn concentration) of 8 times of weight, refluxing extraction is 4 hours under 120 ℃ temperature, filters.
(2) will step (1) filter the ethanolic soln that adds 50% (volumn concentration) of 8 times of crude drug weight in the remaining filter residue in back, under 120 ℃ temperature, continued refluxing extraction 4 hours, filter and merge filtrate twice, obtain Radix Rehmanniae extract A.
(3) Radix Rehmanniae extract A is at first crossed the ceramic membrane (one-level film) that pore size is 100nm, flow velocity is 65L/h, and temperature is controlled at below 45 ℃, and intake pressure is 2.0MPa, and top hole pressure is 1.2MPa.When beginning to bubble in the glutinous rehmannia extract A system, add 15% water of Radix Rehmanniae extract gross weight, be used to improve the yield of target product.To be designated as liquor B by the solution of film, the solution by film is not designated as concentrated solution B.When not having liquor B to flow out, stopper film is handled operation.
(4) liquor B being crossed once more a molecular weight cut-off is organic rolled film (secondary film) of 2.5 ten thousand, and flow velocity is 20L/h, and temperature is controlled at below 45 ℃, and intake pressure is 0.8MPa, and top hole pressure is 0.6MPa.When beginning to bubble in the liquor B system, add 15% water of liquor B gross weight, be used to improve the yield of target product.To be designated as liquor C by the solution of film, the solution by film is not designated as concentrated solution C.When not having liquor C to flow out, stopper film is handled operation.
Liquor C is essence spice for cigarette, stores for future use.
Embodiment 3:
(1) mixture of Radix Rehmanniae Preparata and Rehmannia Root is clayed into power after, get the glutinous rehmannia of 1 times of weight, add the ethanolic soln of 60% (volumn concentration) of 10 times of weight, refluxing extraction is 4 hours under 120 ℃ temperature, filters.
(2) will step (1) filter the ethanolic soln that adds 60% (volumn concentration) of 10 times of crude drug weight in the remaining filter residue in back, under 120 ℃ temperature, continued refluxing extraction 4 hours, filter and merge filtrate twice, obtain Radix Rehmanniae extract A.
(3) Radix Rehmanniae extract A is at first crossed the ceramic membrane (one-level film) that pore size is 100nm, flow velocity is 65L/h, and temperature is controlled at below 45 ℃, and intake pressure is 2.0MPa, and top hole pressure is 1.2MPa.When beginning to bubble in the glutinous rehmannia extract A system, add 20% water of Radix Rehmanniae extract gross weight, be used to improve the yield of target product.To be designated as liquor B by the solution of film, the solution by film is not designated as concentrated solution B.When not having liquor B to flow out, stopper film is handled operation.
(4) liquor B being crossed once more a molecular weight cut-off is organic rolled film (secondary film) of 2.5 ten thousand, and flow velocity is 20L/h, and temperature is controlled at below 45 ℃, and intake pressure is 0.8MPa, and top hole pressure is 0.6MPa.When beginning to bubble in the liquor B system, add 20% water of liquor B gross weight, be used to improve the yield of target product.To be designated as liquor C by the solution of film, the solution by film is not designated as concentrated solution C.When not having liquor C to flow out, stopper film is handled operation.
Liquor C is essence spice for cigarette, stores for future use.
Claims (6)
1, a kind ofly prepare the method for rehmanniae flavor for cigarette, it is characterized in that described method carries out according to the following steps with membrane separation technique:
(1) glutinous rehmannia is clayed into power after, 1 part of weight glutinous rehmannia adds the ethanolic soln of 6-10 part weight, refluxing extraction 3-5 hour after-filtration under 100-135 ℃ temperature keeps filtrate, filter residue is used for next step;
(2) filter residue that previous step is rapid adds the ethanolic soln of step (1) equivalent, and refluxing extraction 3-5 hour after-filtration merges filtrate twice under 100-135 ℃ temperature, and gained filtrate is Radix Rehmanniae extract A;
(3) Radix Rehmanniae extract A is crossed the ceramic membrane that pore size is 100nm (one-level film), when beginning to bubble in the glutinous rehmannia extract A system, the water that adds Radix Rehmanniae extract A gross weight 10%-20%, the solution by film is called liquor B, and the solution by film is not called concentrated solution B; When not having liquor B to flow out, stopper film is handled operation;
(4) liquor B being crossed molecular weight cut-off is organic rolled film (secondary film) of 2.5 ten thousand, when beginning to bubble in the liquor B system, the water that adds the 10%-20% of liquor B gross weight, solution by film is called liquor C, the solution by film is not called concentrated solution C, when not having liquor C to flow out, stopper film is handled operation;
The gained liquor C is rehmanniae flavor for cigarette.
2, according to claim 1ly prepare the method for rehmanniae flavor for cigarette with membrane separation technique, it is characterized in that: described ethanolic soln is that volumn concentration is the ethanolic soln of 30%-60%.
3, the method for preparing rehmanniae flavor for cigarette with membrane separation technique according to claim 1, it is characterized in that: described pore size excessively is the ceramic membrane of 100nm, flow velocity is 50-70L/h, temperature is controlled at below 45 ℃, intake pressure is 1.8-2.2MPa, and top hole pressure is 1.0-1.4MPa.
4, the method for preparing rehmanniae flavor for cigarette with membrane separation technique according to claim 1, it is characterized in that: described molecular weight cut-off excessively is organic rolled film of 2.5 ten thousand, flow velocity is 15-25L/h, temperature is controlled at below 45 ℃, intake pressure is 0.6-1.0MPa, and top hole pressure is 0.5-0.7MPa.
5, according to claim 1ly prepare the method for rehmanniae flavor for cigarette with membrane separation technique, it is characterized in that: the fineness of described glutinous rehmannia is the 80-100 order.
6, according to claim 1ly prepare the method for rehmanniae flavor for cigarette with membrane separation technique, it is characterized in that: described glutinous rehmannia is meant Rehmannia Root or Radix Rehmanniae or Radix Rehmanniae Preparata or the mixture among them.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100477477A CN101586056B (en) | 2008-05-19 | 2008-05-19 | Method for preparing rehmanniae flavor for cigarette by using membrane separation technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100477477A CN101586056B (en) | 2008-05-19 | 2008-05-19 | Method for preparing rehmanniae flavor for cigarette by using membrane separation technique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101586056A true CN101586056A (en) | 2009-11-25 |
| CN101586056B CN101586056B (en) | 2011-11-23 |
Family
ID=41370487
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100477477A Expired - Fee Related CN101586056B (en) | 2008-05-19 | 2008-05-19 | Method for preparing rehmanniae flavor for cigarette by using membrane separation technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101586056B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818119A (en) * | 2015-04-27 | 2015-08-05 | 湖北中烟工业有限责任公司 | Cigarette alfalfa extract and preparation method thereof |
| CN104839885A (en) * | 2015-05-31 | 2015-08-19 | 中国烟草总公司郑州烟草研究院 | Improved method for manufacturing electronic cigarette liquid |
| CN105132178A (en) * | 2015-07-24 | 2015-12-09 | 湖北中烟工业有限责任公司 | Preparation method of broad bean flower extract liquid for tobacco |
| CN105132180A (en) * | 2015-07-31 | 2015-12-09 | 湖北中烟工业有限责任公司 | Preparation method of beet juice for cigarette production |
| CN106010797A (en) * | 2016-07-25 | 2016-10-12 | 中国烟草总公司郑州烟草研究院 | Malt coke-sweet flavor prepared from coked malt and application thereof in electronic cigarettes |
| CN106617273A (en) * | 2016-10-12 | 2017-05-10 | 湖北中烟工业有限责任公司 | Clove mouth tobacco product and preparation method of clove mouth tobacco product |
| CN114836261A (en) * | 2022-05-06 | 2022-08-02 | 云南中烟新材料科技有限公司 | Method for extracting old medicine orange spice and application of old medicine orange spice in cigarette filter tip |
| CN115462552A (en) * | 2022-09-16 | 2022-12-13 | 湖南中烟工业有限责任公司 | Spice with fruit sweet fragrance, preparation method thereof and application thereof in cigarettes |
-
2008
- 2008-05-19 CN CN2008100477477A patent/CN101586056B/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818119A (en) * | 2015-04-27 | 2015-08-05 | 湖北中烟工业有限责任公司 | Cigarette alfalfa extract and preparation method thereof |
| CN104839885A (en) * | 2015-05-31 | 2015-08-19 | 中国烟草总公司郑州烟草研究院 | Improved method for manufacturing electronic cigarette liquid |
| CN104839885B (en) * | 2015-05-31 | 2016-08-24 | 中国烟草总公司郑州烟草研究院 | A kind of electronic cigarette liquid and preparation method thereof of improvement |
| CN105132178A (en) * | 2015-07-24 | 2015-12-09 | 湖北中烟工业有限责任公司 | Preparation method of broad bean flower extract liquid for tobacco |
| CN105132180A (en) * | 2015-07-31 | 2015-12-09 | 湖北中烟工业有限责任公司 | Preparation method of beet juice for cigarette production |
| CN106010797A (en) * | 2016-07-25 | 2016-10-12 | 中国烟草总公司郑州烟草研究院 | Malt coke-sweet flavor prepared from coked malt and application thereof in electronic cigarettes |
| CN106617273A (en) * | 2016-10-12 | 2017-05-10 | 湖北中烟工业有限责任公司 | Clove mouth tobacco product and preparation method of clove mouth tobacco product |
| CN114836261A (en) * | 2022-05-06 | 2022-08-02 | 云南中烟新材料科技有限公司 | Method for extracting old medicine orange spice and application of old medicine orange spice in cigarette filter tip |
| CN114836261B (en) * | 2022-05-06 | 2023-05-12 | 云南中烟新材料科技有限公司 | Extraction method of old medicine orange spice and application of old medicine orange spice in cigarette filter tips |
| CN115462552A (en) * | 2022-09-16 | 2022-12-13 | 湖南中烟工业有限责任公司 | Spice with fruit sweet fragrance, preparation method thereof and application thereof in cigarettes |
| CN115462552B (en) * | 2022-09-16 | 2023-09-05 | 湖南中烟工业有限责任公司 | Spice with fruit fragrance, preparation method thereof and application thereof in cigarettes |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101586056B (en) | 2011-11-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101586056B (en) | Method for preparing rehmanniae flavor for cigarette by using membrane separation technique | |
| CN101357949B (en) | Extraction method of polysaccharides from morinda officinalis how and application thereof in cigarette | |
| CN101768514B (en) | Alhagi sparsifolia extract and preparation method and application thereof | |
| CN102191130A (en) | Preparation method of fermented cigarette fructus momordicae extractum | |
| CN106037012B (en) | A kind of tobacco juice for electronic smoke | |
| CN103432193A (en) | Microwave-assisted aqueous two-phase extraction and separation method of kudzu root total flavones | |
| CN102796615B (en) | Method for preparing cigarette strawberry extract by using pectinase | |
| CN104479869A (en) | Casing essence for quietly elegant fragrance style cigarette | |
| CN102499434B (en) | Preparation method for litchi pericarp extract and application of same in production of cigarette | |
| CN1401751A (en) | Method for preparing pure tobacco oil | |
| CN109852479A (en) | A kind of floating oil method prepares the method and its application of flue-cured tobacco absolute oil | |
| CN102703217A (en) | Noni extract and application thereof | |
| CN102423116A (en) | Preparation method for pineapple spice for cigarette | |
| CN1476892A (en) | Method for separating effertive components of Chinese medicine by adopting membrane technique | |
| CN102408944A (en) | Tobacco additive capable of reducing irritation and increasing tobacco fragrance and preparation method thereof | |
| CN101357950A (en) | Extraction method of polysaccharides from morinda officinalis how and application thereof in cigarette | |
| CN1319477C (en) | Chinese medicine cigarette for reducing toxin | |
| CN102488320B (en) | Application of paper mulberry fruit essential oil in cigarette flavoring and material feeding | |
| CN101422518B (en) | Preparation method of loquat flower extract | |
| CN114836261B (en) | Extraction method of old medicine orange spice and application of old medicine orange spice in cigarette filter tips | |
| CN115386428B (en) | Multistage extraction-based Maillard reaction essence of drug-flavor mixed system | |
| CN115537268B (en) | Mixed system Maillard reaction essence based on multistage extraction and batch stability control method thereof | |
| CN109700068A (en) | A kind of floating oil method prepares the method and its application of sun-cured tobacco absolute oil | |
| KR100334325B1 (en) | Green tea leaf make use of manufacture method of soju | |
| CN104447969B (en) | Alkali extraction and acid precipitation isolates and purifies albumen in larch pine needle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111123 Termination date: 20140519 |