CN101268863A - Method for preparing polymer brown reaction product, and produced products and application thereof - Google Patents
Method for preparing polymer brown reaction product, and produced products and application thereof Download PDFInfo
- Publication number
- CN101268863A CN101268863A CNA2008100496872A CN200810049687A CN101268863A CN 101268863 A CN101268863 A CN 101268863A CN A2008100496872 A CNA2008100496872 A CN A2008100496872A CN 200810049687 A CN200810049687 A CN 200810049687A CN 101268863 A CN101268863 A CN 101268863A
- Authority
- CN
- China
- Prior art keywords
- preparation
- reaction product
- molecular
- molecular weight
- brown reaction
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of high molecular browny resultant of reaction, sugar, amino acid and catalyzer react at a certain temperature. The preparation method is characterized in that reaction liquid separates the resultant with different molecular weights obtained by reaction through a membrane separation technique, then trapped fluid obtained by membrane separation is performed with membrane concentration, finally the resultant of the invention is obtained by spraying and drying a concentrated solution. The preparation method has the advantages that the browny resultant of reaction is separated and concentrated by utilizing the membrane technique, compared with an ethanol analysis method and a pH value adjusting method, the trashing effect is good, the technique condition is moderate, the processing time of the reaction liquid is short, the temperature is low, and the continuous reaction cannot happen. The membrane with different molecular weights is utilized to separate the browny resultant with different molecular weight sections in the reaction liquid, which is hard to live up to by the ethanol analysis method. In the membrane separation process, a little de-ionized water is added for leaching, thereby avoiding the use of a plurality of ethanol in the ethanol analysis method, and obviously lowering the production cost of products. The spraying and drying method has the advantages of short heating time, high efficiency and good quality of resultant.
Description
Technical field
The present invention relates to the cigarette perfume material, especially a kind of preparation method who can be used as the high-molecular brown reaction product that tobacco aromatics using uses and products thereof uses.This method is to react at a certain temperature with sugar and amino acid and catalyst, and product is carried out the film separation, gets rid of the small-molecule substance in the product.The trapped fluid (macromolecule product) that film is separated carries out spray-drying then, obtains powdery, water-soluble macromolecule browning reaction product.
Background technology
Maillard reaction is the browning reaction (Non-enzymatic browning) of the non-enzymatic catalysis that takes place between amino-compound and the reduced sugar, reaction is through complicated course, the final generation contains various little molecules and high molecular brown mixture, and wherein macromolecule product is also referred to as melanoid (Melanoidins).Maillard reaction is to produce one of main path of fragrance matter in tobacco modulation, the ageing process, and the organoleptic quality of raw tobacco material and cigarette product is had material impact.By model M aillard prepared in reaction cigarette perfume material, carried out a large amount of research both at home and abroad, but for maintaining secrecy of core technology, abroad concrete preparation method and the application technology to the Maillard tobacco aromatics using rarely has report, domestic research to it mainly is synthetic method, the analysis of product and the effect in cigarette thereof about low brownization of the non-enzyme of molecule product, and very few to the research of the non-enzyme brown reaction product of macromolecule.
In the preparation process of the non-enzyme brown reaction product of macromolecule, the separation of product is the sport technique segment of most critical, directly influences the yield and the perfuming cigarette effect of product.At present, separating out alcohol method and pH value adjusting method are the most frequently used separation methods of the non-enzyme brown reaction product of macromolecule.But separating out alcohol method and pH value adjusting method will effectively be removed small molecule by-product needs cyclic washing, and product also needs long-time dry, and whole separation process operation is numerous and diverse, and product will be because the long-time heating drying will continue reaction, water-soluble variation.In addition, the dialysis freeze-drying also is the separation method commonly used of the non-enzyme brown reaction product of prepared in laboratory macromolecule.The dialysis freeze-drying can effectively be removed small molecule by-product, and macromolecule product is also very stable in freezing dry process, but the freeze-drying of dialysing can only prepare the chamber of experimentizing in a small amount, is difficult in the suitability for industrialized production and is used.
Summary of the invention
The objective of the invention is to utilize membrane separation technique that the different molecular weight product in the brown reaction product is separated, obtain the browning reaction product of different molecular weight, again reactant liquor is carried out spray-drying, can obtain the Powdered macromolecule browning reaction product of different molecular weight.
The objective of the invention is to be achieved through the following technical solutions: the preparation method of high-molecular brown reaction product of the present invention, be to be to react under 80～100 ℃ in temperature with sugar and amino acid and catalyst, wherein: reactant liquor separates the different molecular weight product that reaction obtains by membrane separation technique by first filter earlier again, it is concentrated that the trapped fluid that the film separation is obtained carries out film then, at last concentrate is carried out spray-drying, obtain powdery, water-soluble high-molecular brown product.
In the present invention, the concrete steps of separation, concentration process are as follows:
A, elder generation utilize filter press to filter browning reaction liquid, remove the insoluble particles thing in the reactant liquor;
The milipore filter of b, the different molecular weight that dam of selection carries out film with filtered fluid and separates, and on purpose holds back the macromolecule brown product of target molecular weight;
C, be that the milipore filter of 80-500Da carries out film and concentrates with the molecular weight that dams once more, trapped fluid is concentrated into the concentrate that solid content is 10-30% trapped fluid.
In the present invention, described sugar can be any one of fructose, wood sugar or glucose; Described amino acid can be alanine or glycine; Described catalyst is a sodium acid carbonate.
The film separation process is to adopt the milipore filter of the molecular weight 10000Da～3000Da that dams to carry out film under 0.3～0.7MPa pressure condition to separate.
The film concentration process is that to adopt the molecular weight that dams be that the milipore filter of 80Da～500Da carries out film and concentrates trapped fluid is concentrated into the concentrate that solid content is 10-30%.
Spray-drying process of the present invention is to use Highspeedcentrifugingandsprayingdrier to finish, and the EAT of device therefor is that 180～250 ℃, leaving air temp are 90～120 ℃, centrifuge speed 30～45Hz, charging rate 8L～15Lh
-1
Product of the present invention adds in the tobacco as tobacco spice, has tangible perfuming cigarette effect.Adding proportion joins in the tobacco by 50ppm～500ppm.
It is concentrated that this invention advantage is to utilize membrane technology that the browning reaction product is separated, compare with pH value adjusting method with separating out alcohol method, and good impurity removing effect, the process conditions gentleness, the reactant liquor processing time is short, and temperature is low, can not continue to react.Utilize the film of different molecular weight the brown product of different molecular weight section in the reactant liquor can be separated, this is that separating out alcohol method is difficult to accomplish.In the film separation process, only need to add small quantity of deionized water and carry out drip washing, avoided a large amount of ethanol in the separating out alcohol method to use, obviously reduced production cost of products.It is short that spray drying process has heat time heating time, efficient height, shortcoming such as the advantage of product quality better has avoided common oven drying method long heat time heating time, and efficient is low.
The specific embodiment
The present invention is further described below in conjunction with embodiment, but is not restriction the present invention.
Embodiment 1:
Glucose, alanine and sodium acid carbonate are added in the reactor, add a certain amount of deionized water then, fully after the dissolving, reaction is 24 hours under 95 ℃ of temperature conditions.Reaction finishes, and adopts filter press that reactant liquor is carried out filter just, removes the insoluble accessory substance in the system.Just the dam milipore filter of molecular weight 10000Da of the filtrate after filter employing carries out film and separates under the 0.3MPa pressure condition, in the separation process, adds the continuous drip washing of the 20L deionized water liquid that dams.After film separate to finish, be that the milipore filter of 80Da carries out film and concentrates trapped fluid is concentrated into the concentrate that solid content is 10-30% with the molecular weight that dams once more.Is that 200 ℃, leaving air temp are 90 ℃, centrifuge speed 35Hz, charging rate 14Lh with concentrate at EAT
-1Carry out spray-drying under the condition, promptly get powdery, water-soluble macromolecule browning reaction product, yield about 26%.
The efficient liquid phase chromatographic analysis of concentrate shows that the milipore filter that adopts the molecular weight 10000Da that dams carries out the film separation and can effectively remove little molecular product.It is not obvious that gel osmoticing chromatogram analysis shows that the molecular weight of macromolecule product before and after spray-drying changes, and the weight average molecular weight of product reaches 20000Da, and this illustrates that spray-dired short time heating process can not cause the further variation of product.
This high-molecular brown reaction product is joined blank by different amounts examine cigarette reference cigarette, thought by the smoke panel test committee evaluation of Zhengzhou tobacco research institute: this product has tangible perfuming cigarette effect, and the flue gas characteristic of cigarette, mouthfeel characteristic also all have improvement in various degree.
Embodiment 2:
Fructose, glycine and sodium acid carbonate are added in the reactor, add a certain amount of deionized water then, fully after the dissolving, reaction is 24 hours under 95 ℃ of temperature conditions.Reaction finishes, and adopts filter press that reactant liquor is carried out filter just, removes the insoluble accessory substance in the system.Just the dam milipore filter of molecular weight 10000Da of the filtrate after filter employing carries out film and separates under the 0.5MPa pressure condition, in the separation process, adds the continuous drip washing of the 30L deionized water liquid that dams.After film separate to finish, be that the milipore filter of 150Da carries out film and concentrates trapped fluid is concentrated into the concentrate that solid content is 10-30% with the molecular weight that dams once more.Is that 220 ℃, outlet temperature are 100 ℃, centrifuge speed 40Hz, charging rate 11Lh with concentrate in inlet temperature
-1Carry out spray-drying under the condition, promptly get powdery, water-soluble macromolecule browning reaction product, yield about 25%.
The efficient liquid phase chromatographic analysis of concentrate shows better than embodiment one of impurity-eliminating effect that the film that carries out with this understanding separates, but the product yield under this condition is a little less than embodiment 1.It is not obvious that gel osmoticing chromatogram analysis shows that the molecular weight of macromolecule product before and after spray-drying changes, about product weight average molecular weight 21000Da.
This high-molecular brown reaction product is joined blank by different amounts examine cigarette reference cigarette, thought by the smoke panel test committee evaluation of Zhengzhou tobacco research institute: this product has tangible perfuming cigarette effect, can enrich cigarette perfume (or spice), reduces to stimulate, covers assorted gas, improve pleasant impression.
Embodiment 3:
Wood sugar, alanine and sodium acid carbonate are added in the reactor, add a certain amount of deionized water then, fully after the dissolving, reaction is 24 hours under 95 ℃ of temperature conditions.Reaction finishes, and adopts filter press that reactant liquor is carried out filter just, removes the insoluble accessory substance in the system.Just the dam milipore filter of molecular weight 3000Da of the filtrate after filter employing carries out film and separates under the 0.7MPa pressure condition, in the separation process, adds the continuous drip washing of the 50L deionized water liquid that dams.After film separate to finish, be that the milipore filter of 500Da carries out film and concentrates trapped fluid is concentrated into the concentrate that solid content is 10-30% with the molecular weight that dams once more.Is that 240 ℃, outlet temperature are 120 ℃, centrifuge speed 45Hz, charging rate 9Lh with concentrate in inlet temperature
-1Carry out spray-drying under the condition, promptly get powdery, water-soluble macromolecule browning reaction product, yield about 28%.
The efficient liquid phase chromatographic analysis of concentrate shows that the milipore filter that adopts the molecular weight 3000Da that dams carries out the film separation and can effectively remove little molecular product.It is not obvious that gel osmoticing chromatogram analysis shows that the molecular weight of macromolecule product before and after spray-drying changes, about product weight average molecular weight 6000Da.
This high-molecular brown reaction product is joined blank by different amounts examine cigarette reference cigarette, thought by the smoke panel test committee evaluation of Zhengzhou tobacco research institute: this product has tangible perfuming cigarette effect, can increase cigarette perfume (or spice), soft flue gas, improve pleasant impression, improve the whole smooth degree of flue gas.
Claims (9)
1, a kind of preparation method of high-molecular brown reaction product, be to be to react under 80～100 ℃ in temperature with sugar and amino acid and catalyst, it is characterized in that: reactant liquor separates the different molecular weight product that reaction obtains by membrane separation technique by first filter earlier again, it is concentrated that the trapped fluid that the film separation is obtained carries out film then, at last concentrate is carried out spray-drying, obtain powdery, water-soluble high-molecular brown product.
2, the preparation method of high-molecular brown reaction product according to claim 1 is characterized in that: the concrete steps of separation, concentration process are as follows:
A, elder generation utilize filter press to filter browning reaction liquid, remove the insoluble particles thing in the reactant liquor;
The milipore filter of b, the different molecular weight that dam of selection carries out film with filtered fluid and separates, and on purpose holds back the macromolecule brown product of target molecular weight;
C, be that the milipore filter of 80-500Da carries out film and concentrates with the molecular weight that dams once more, trapped fluid is concentrated into the concentrate that solid content is 10-30% trapped fluid.
3, the preparation method of high-molecular brown reaction product according to claim 1 is characterized in that: sugar is any one of fructose, wood sugar or glucose.
4, the preparation method of high-molecular brown reaction product according to claim 1 is characterized in that: amino acid is alanine, glycine.
5, the preparation method of high-molecular brown reaction product according to claim 1 is characterized in that: catalyst is a sodium acid carbonate.
6, the preparation method of high-molecular brown reaction product according to claim 1, it is characterized in that: spray-drying uses spray dryer to finish, and the EAT of device therefor is that 180～250 ℃, leaving air temp are 90～120 ℃, centrifuge speed 30～45Hz, charging rate 8L～15Lh
-1
7, the preparation method of high-molecular brown reaction product according to claim 1 is characterized in that: the film separation process is to adopt the milipore filter of the molecular weight 10000Da～3000Da that dams to carry out film under 0.3～0.7MPa pressure condition to separate.
8, the preparation method of high-molecular brown reaction product according to claim 1 is characterized in that: the film concentration process is that to adopt the molecular weight that dams be that the milipore filter of 80Da～500Da carries out film and concentrates trapped fluid is concentrated into the concentrate that solid content is 10-30%.
9, the application of the described high-molecular brown reaction product of a kind of claim 1, it is characterized in that: this product adds in the tobacco as tobacco spice, has tangible perfuming cigarette effect.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100496872A CN101268863B (en) | 2008-05-05 | 2008-05-05 | Method for preparing polymer brown reaction product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100496872A CN101268863B (en) | 2008-05-05 | 2008-05-05 | Method for preparing polymer brown reaction product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101268863A true CN101268863A (en) | 2008-09-24 |
| CN101268863B CN101268863B (en) | 2010-06-09 |
Family
ID=40003284
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100496872A Active CN101268863B (en) | 2008-05-05 | 2008-05-05 | Method for preparing polymer brown reaction product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101268863B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633866B (en) * | 2009-06-02 | 2011-11-02 | 华宝食用香精香料（上海）有限公司 | Cigarette siraitia grosvenorii additive and preparation method and application thereof |
| CN112675705A (en) * | 2020-12-14 | 2021-04-20 | 湖北中烟工业有限责任公司 | Method for carrying out fractional purification on Maillard reaction intermediate |
| CN112931923A (en) * | 2021-02-02 | 2021-06-11 | 云南中烟工业有限责任公司 | Preparation method of specific molecular weight peptide Maillard intermediate and application of intermediate in tobacco flavor |
-
2008
- 2008-05-05 CN CN2008100496872A patent/CN101268863B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633866B (en) * | 2009-06-02 | 2011-11-02 | 华宝食用香精香料（上海）有限公司 | Cigarette siraitia grosvenorii additive and preparation method and application thereof |
| CN112675705A (en) * | 2020-12-14 | 2021-04-20 | 湖北中烟工业有限责任公司 | Method for carrying out fractional purification on Maillard reaction intermediate |
| CN112931923A (en) * | 2021-02-02 | 2021-06-11 | 云南中烟工业有限责任公司 | Preparation method of specific molecular weight peptide Maillard intermediate and application of intermediate in tobacco flavor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101268863B (en) | 2010-06-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101704850A (en) | Method for separating and extracting compound of Amadori of Maillard reaction midbody | |
| CN105212262A (en) | A kind of preparation method of tobacco flavor material | |
| CN104262413B (en) | Preparation method of trehalose anhydrous | |
| CN101268863B (en) | Method for preparing polymer brown reaction product | |
| CN103059163B (en) | Method for preparing alginate oligosaccharide monomers by using microwave radiation | |
| CN102870954B (en) | Preparation method for antioxidant peptide | |
| CN102952266A (en) | Separation and purification method of gamma-polyglutamic acid | |
| CN115260334B (en) | Compound extraction process of mulberry leaf polysaccharide | |
| CN1962875B (en) | Method for preparing uridine diphosphate | |
| CN104357518A (en) | Method for preparing nucleotide from waste beer yeast | |
| CN107760750A (en) | A kind of method that high F value oligopeptide and starch sugar are synchronously prepared using corn protein powder as raw material | |
| CN107418897A (en) | A kind of technique for effectively discarding mycoprotein using glutamic acid fermentation | |
| CN104072636B (en) | The preparation technology of heparin sodium | |
| CN105062675A (en) | Preparation method of beta vulgaris Maillard reactant for tobacco | |
| CN101849605A (en) | Preparation method of silkworm pupa high zinc protein powder | |
| CN103194518A (en) | Preparation method of fish collagen peptides with narrow molecular weight ranges | |
| EP3194132B1 (en) | Heat insulation material based on aerogel | |
| CN101974151B (en) | Method for preparing bio-based nylon polybutyrolactam | |
| CN110042129B (en) | Preparation method of agricultural gamma-polyglutamic acid | |
| CN101429529B (en) | Ester zymoid method production process of azeotropy water elimination coupling simulated moving bed | |
| CN110038524A (en) | It is a kind of for isolating and purifying the preparation method of the affinity chromatography medium of chitosan enzyme | |
| CN101914599B (en) | Nucleotide mixture extracted from edible fungi as well as preparation method and application thereof | |
| RU2316592C1 (en) | Method for preparing chitosan oligomers | |
| CN108441535A (en) | The production method of three enzymes, one ferment silkworm peptide | |
| CN114847467B (en) | Yeast extract rich in cysteine and preparation method thereof |
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 |