CN103478896A - Tea flower oligosaccharide or polysaccharide, preparation method thereof and application thereof in cigarettes - Google Patents
Tea flower oligosaccharide or polysaccharide, preparation method thereof and application thereof in cigarettes Download PDFInfo
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- CN103478896A CN103478896A CN201310446757.9A CN201310446757A CN103478896A CN 103478896 A CN103478896 A CN 103478896A CN 201310446757 A CN201310446757 A CN 201310446757A CN 103478896 A CN103478896 A CN 103478896A
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Abstract
The invention belongs to the field of spices and tobacco and relates to tea flower oligosaccharide or polysaccharide, a preparation method thereof and application thereof in cigarettes. The tea flower oligosaccharide or polysaccharide obtained by extracting is high in purity and high in extraction rate, and the preparation method is simple and convenient in operation, easy to implement, high in efficiency and low in solvent consumption. By applying the tea flower oligosaccharide or polysaccharide in the cigarettes, original processing techniques are unchanged, smoking quality of the cigarettes is obviously improved, and sensory comfortableness of the cigarettes is improved, so that the tea flower oligosaccharide or polysaccharide has significance and value of actual production.
Description
Technical field
The invention belongs to spices and Field of Tobacco, relate to a kind of Tea Flower compound sugar or polysaccharide, its preparation method and the application in cigarette thereof.
Background technology
Carbohydrate distributes very wide at nature, no matter the animal kingdom or plant kingdom, all exist carbohydrate.Press the construction unit number and divide, sugar can be divided into monose, compound sugar and polysaccharide.Monose is to be hydrolyzed into more micromolecular sugar, and compound sugar refers to and contains the compound that 2-10 glycosidic bond is polymerized, claims again oligosaccharides.Polysaccharide is to be formed by the condensation of monose molecule, the dehydration that surpass more than 10, is molecule mechanism complexity and huge glucide.
Compound sugar is the constituent of many plants, has micro-ecological environment in the human body of improvement, improves blood lipid metabolism, strengthens the significantly pharmacologically active such as immunologic function.
Polysaccharide is extremely wide in distributed in nature, also very important, has plenty of the constituent that forms the animals and plants skeleton structure, as cellulose; Has plenty of the nutrient as the animals and plants storage, as glycogen and starch; What also have has a special biologically active, as the heparin in human body, blood coagulation resisting function is arranged, and for example the polysaccharide in the pneumococcus cell membrane has antigenic action.
The extraction of natural plant polyose is the focus of studying at present, and the acquisition of polysaccharide generally need be passed through the water extraction process, contains polysaccharide and compound sugar in water extraction liquid simultaneously, and traditional aqueous extraction-alcohol precipitation technology is often given it up compound sugar, causes great waste.
It is to occur in 20 beginnings of the century that film separates, the separation technology emerged rapidly after the sixties in 20th century.Membrane separation technique is owing to having separation, concentrated, purifying and refining function concurrently, efficient, energy-saving and environmental protection arranged again, molecular level filters and filter process is simple, be easy to the feature such as control.The aperture of film is generally micron order, and the difference (or being called molecular cut off) according to its aperture, can be divided into film micro-filtration membrane (MF), milipore filter (UF), NF membrane (NF) and reverse osmosis membrane (RO) etc.Mainly milipore filter is used for to separation and the purifying of polysaccharide in the research field of plant polyose, as lentinan (Li Zhizhou, 2001; Read to protect justice, 2003), soyabean oligosaccharides (Gao Weixing, 2005), Tea Polysaccharides (Liu Junhai, 2007).
Tea Flower is the flower of Theaceae Camellia Plants tea tree (Camellia sinensis), Tea Flower is wide at China's distributed pole, be September to next year 1, February tea tree florescence in most of tea district, Tea Flower is a kind of without plantation cultivation, abundant and reproducible natural resources, for a long time, the tea grower only plucks the fresh and tender bud-leaf of tea tree, for Tea Flower, lets alone to run its course, and seldom is used.Tea Flower is rich in multiple beneficial composition and the active materials such as protein, Tea Polyphenols, tea polysaccharide, Tea Saponin, flavonoids, amino acid, vitamin, trace element and superoxide dismutase (SOD), theobromine.
2013 No. 1 file approval Tea Flower of the Ministry of Public Health is as a kind of new resource food.The research of Tea Flower carbohydrate concentrates on the aspects such as the extracting method, separating and purifying technology, content detection, structure calibrating, bioactivity research of Tea Flower macromolecular polysaccharide at present.Wherein the extracting method of Tea Flower macromolecular polysaccharide has ultrasonic wave extraction, Microwave Extraction etc., and the separation and purification of polysaccharide generally adopts macroreticular resin absorbing method, anion exchange, gel chromatography etc.
Still need at present and want new technique, to prepare Tea Flower compound sugar or polysaccharide, and it can be used as the particularly additive of cigarette of good tobacco product.
Summary of the invention
The inventor, through deep research and performing creative labour, has obtained a kind of preparation technology of Tea Flower polysaccharide and has correspondingly obtained a kind of Tea Flower compound sugar or polysaccharide.The inventor is surprised to find, and the Tea Flower compound sugar or the polysaccharide that make are put in cigarette, can significantly improve sucking quality and the sense organ comfort level of cigarette, and does not change the existing processing technology of cigarette.Following invention is provided thus:
One aspect of the present invention relates to a kind of preparation method of Tea Flower compound sugar, comprises the step of water extraction, Separation of Solid and Liquid, micro-filtration, ultrafiltration; Particularly, it also comprises counter-infiltration, concentrated, dry step.
The invention still further relates to a kind of preparation method of Tea Flower compound sugar, comprise the steps:
1) water extraction: take a certain amount of fresh Tea Flower or dry Tea Flower, use hot water lixiviate, ultrasonic extraction or microwave extract method to carry out the one or many extraction;
2) liquid-solid separation: extract is separated with Tea Flower, obtain extract; Preferably, merge and repeatedly extract the extract obtained;
3) micro-filtration: adopt micro-filtration membrane to remove solid content and the suspension in extract, obtain micro-filtration and see through liquid;
4) ultrafiltration: adopt milipore filter to be separated, obtain ultrafiltration and see through liquid;
5) counter-infiltration: adopt reverse osmosis membrane that ultrafiltration is seen through to liquid and concentrated, obtain reverse osmosis concentrated liquid;
6) concentrated: as further to concentrate, obtain concentrate;
7) drying: concentrate is carried out to drying, obtain the Tea Flower compound sugar.
The preparation method of the described Tea Flower compound sugar of any one according to the present invention is characterized in that any one in following (1)-(7) or multinomial:
(1) mass ratio of solvent described in step 1) (water) and Tea Flower is 5-25, is preferably 5-15, more preferably 10;
(2) be separated into centrifugal step 2) or filter;
(3) aperture of micro-filtration membrane described in step 3) is 50-1200nm, is preferably 100-300nm, more preferably 200nm; System pressure is 1-6Bar, is preferably 2-4Bar, more preferably 3Bar;
(4) molecular cut off of milipore filter described in step 4) is 5000-300000Dal, is preferably 10000-50000Dal, more preferably 30000Dal; System pressure is that 5-35Bar is preferably 10-30Bar, more preferably 20Bar;
(5) to the rejection of sodium chloride, more than 98%, system pressure is 10-40Bar to the reverse osmosis membrane described in step 5), is preferably 20-35Bar, is preferably 32Bar;
(6) reduced pressure concentration of simmer down to described in step 6);
(7) drying mode in step 7) is spray-drying.
Another aspect of the present invention relates to a kind of preparation method of Tea Flower polysaccharide, comprises the step of water extraction, Separation of Solid and Liquid, micro-filtration, ultrafiltration; Particularly, it also comprises that de-albumen, alcohol are analysed, dry step.
The invention still further relates to a kind of preparation method of Tea Flower polysaccharide, comprise the steps:
1) water extraction: take a certain amount of fresh Tea Flower or dry Tea Flower, use hot water lixiviate, ultrasonic extraction or microwave extract method to carry out the one or many extraction;
2) liquid-solid separation: extract is separated with Tea Flower, obtain extract; Preferably, merge and repeatedly extract the extract obtained;
3) micro-filtration: adopt micro-filtration membrane to remove solid content and the suspension in extract, obtain micro-filtration and see through liquid;
4) ultrafiltration: adopt milipore filter to be separated, obtain the ultrafiltration trapped fluid;
5) de-albumen: the ultrafiltration trapped fluid carries out the deproteinization processing, obtains the deproteinization product;
6) alcohol is analysed: will take off protein product and use ethanol to carry out alcohol to analyse, obtain alcohol and analyse thing;
7) drying: alcohol is analysed to thing and carry out drying, obtain the Tea Flower polysaccharide.
The preparation method of the described Tea Flower polysaccharide of any one according to the present invention is characterized in that any one in following (1)-(7) or multinomial:
(1) mass ratio of solvent described in step 1) and Tea Flower is 5-25, is preferably 5-15, more preferably 10;
(2) be separated into centrifugal step 2) or filter;
(3) aperture of micro-filtration membrane described in step 3) is 50-800nm, is preferably 100-300nm, more preferably 200nm; System pressure is 1-6Bar, is preferably 2-4Bar, more preferably 3Bar;
(4) molecular cut off of milipore filter described in step 4) is 5000-300000Dal, is preferably 10000-50000Dal, more preferably 30000Dal; System pressure is that 5-35Bar is preferably 10-30Bar, more preferably 20Bar;
(5) described in step 5), Deproteinated method is Sevage method, enzyme process or trichloroacetic acid method, is preferably the Sevage method;
(6) alcohol described in step 6) is analysed working concentration at 80% above ethanol, and for example 80%-95%, 80%-85%, 80%-90%, 85%-95%, be preferably 85%, and the alcohol time of analysing is 24-48 hour, is preferably 36 hours;
(7) drying mode in step 7) is spray-drying.
In one embodiment of the invention, the preparation method of Tea Flower compound sugar and/or Tea Flower polysaccharide as shown in Figure 1.
Of the present inventionly relate in one aspect to a kind of Tea Flower compound sugar, the preparation method of the described Tea Flower compound sugar of its any one in the present invention makes again.
Of the present inventionly relate in one aspect to a kind of Tea Flower polysaccharide, the preparation method of the described Tea Flower polysaccharide of its any one in the present invention makes again.
The tobacco articles that relates in one aspect to again of the present invention, it contains Tea Flower compound sugar and/or Tea Flower polysaccharide; Particularly, described tobacco product is cigarette; Particularly, described Tea Flower compound sugar is Tea Flower compound sugar of the present invention; Particularly, described Tea Flower polysaccharide is Tea Flower polysaccharide of the present invention; Particularly, the 0.001-1% that the content of described Tea Flower compound sugar and/or Tea Flower polysaccharide is tobacco quality; Be preferably 0.01-0.1%; 0.01-0.05% more preferably; Particularly, be 0.01-0.03%, 0.03-0.05%, 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09% or 0.1%.
In a preferred embodiment of the present invention, described tobacco product contains Tea Flower compound sugar of the present invention and Tea Flower polysaccharide.The inventor also is surprised to find, for being applied to tobacco product, Tea Flower compound sugar and Tea Flower polysaccharide share (being preferably 1:1) than alone effective separately, and the extraordinary writs inventor is impressive is to have increased the elegant fragrance of tobacco product (for example cigarette).Preferably, the ratio of Tea Flower compound sugar and Tea Flower polysaccharide is (1:1)-(1:3), for example (1:1)-(1:2), (1:2)-(1:3), 1:1,1:2,1:3; Particularly preferably, be 1:1.
The source of Tea Flower compound sugar or Tea Flower polysaccharide comprises the methods such as extraction, ultrasonic wave extraction, Microwave Extraction, enzyme extraction, means of supercritical extraction; Preferably, be Tea Flower compound sugar of the present invention or polysaccharide.Be mixed with even its addition manner water dissolves the reinforced solution that concentration is 1-10%, evenly be sprayed onto in pipe tobacco, by normal cigarette process, roll into cigarette, the 0.01-0.1% that concrete usage ratio is tobacco quality.
Described Tea Flower compound sugar and/the Tea Flower polysaccharide can be used as the additive of cigarette, the result of adding the cigarette sensory evaluating smoking of Tea Flower compound sugar and/or Tea Flower polysaccharide shows: after adding Tea Flower compound sugar and/or Tea Flower polysaccharide, the sucking quality of cigarette, sense organ comfort level are improved significantly.
Of the present invention relate in one aspect to again the Tea Flower compound sugar and/purposes of Tea Flower polysaccharide in preparing tobacco product; Particularly, described tobacco product is cigarette; Particularly, described Tea Flower compound sugar is Tea Flower compound sugar of the present invention; Particularly, described Tea Flower polysaccharide is Tea Flower polysaccharide of the present invention; Particularly, the 0.001-1% that the content of described Tea Flower compound sugar and/or Tea Flower polysaccharide is tobacco quality; Be preferably 0.01-0.1%; 0.01-0.05% more preferably; Particularly, be 0.01-0.03%, 0.03-0.05%, 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09% or 0.1%.
Of the present inventionly relate in one aspect to a kind of composition, it contains Tea Flower compound sugar of the present invention and/or Tea Flower polysaccharide of the present invention again; Preferably, the ratio of Tea Flower compound sugar and Tea Flower polysaccharide is (1:1)-(1:3); Particularly, described composition is food, beverage or health products.
Tea Flower compound sugar of the present invention and/or the purposes of Tea Flower polysaccharide of the present invention in preparing food, beverage or health products of relating in one aspect to again of the present invention.
In the present invention,
" tea tree " in described " Tea Flower ", if not otherwise specified, refer to the plant of Theales (Theales), Theaceae (Theaceae) or Camellia (Camellis);
In one aspect of the invention, " flower " in described " Tea Flower " comprising: perianth, oecium, gynoecium.Perianth comprises: calyx (being comprised of sepal), corolla (being comprised of petal).The color of flower and fragrance are from corolla.Stamen comprises: filigree and flower pesticide.Gynoecium comprises: column cap, style and ovary.
In one aspect of the invention, term " Tea Flower ", can be fresh flower, can be also dry flower; If there is no specified otherwise, it refers to the part of complete Tea Flower or Tea Flower; It at least comprises petal; Alternatively, also comprise and be selected from one or more in sepal, stamen and gynoecium.
In the present invention, if not otherwise specified, " Tea Flower compound sugar " of the present invention comprises pure Tea Flower compound sugar; Also comprise the Tea Flower extract that is rich in the Tea Flower compound sugar, mean in extract, except the Tea Flower compound sugar, also can to comprise other material extracted from Tea Flower; Particularly, the content (purity) of the Tea Flower compound sugar in the described Tea Flower extract that is rich in the Tea Flower compound sugar for >=30%, >=40%, >=50%, >=60%, >=70%, >=75%, >=80%, >=85%, >=90% or >=95%, the described content content that is weight percentage.
In the present invention, if not otherwise specified, " Tea Flower polysaccharide " of the present invention comprises pure Tea Flower polysaccharide; Also comprise the Tea Flower extract that is rich in the Tea Flower polysaccharide, mean in extract, except the Tea Flower polysaccharide, also can to comprise other material extracted from Tea Flower; Particularly, the content (purity) of the Tea Flower polysaccharide in the described Tea Flower extract that is rich in the Tea Flower polysaccharide for >=30%, >=40%, >=50%, >=60%, >=70%, >=75%, >=80%, >=85%, >=90% or >=95%, the described content content that is weight percentage.
Adopt recovery rate and the purity of phenolsulfuric acid colorimetric method for determining compound sugar, polysaccharide, the recovery rate of compound sugar is more than 2.5%, and purity is more than 90%, and polysaccharide extract rate is more than 3%, and purity is more than 90%.
The concentration of described ethanol, if not otherwise specified, all refer to volumetric concentration.
In the present invention, particularly, the tobacco product of described tobacco product for sucking, be preferably cigarette.
The beneficial effect of the invention
The present invention extracts the Tea Flower compound sugar of acquisition or purity of polysaccharide is high, recovery rate is high, and row easy and simple to handle, easy, efficient, and the solvent use amount is few.Tea Flower compound sugar, polysaccharide are applied in cigarette not change the original processing technology of cigarette, and obviously improve the sucking quality of cigarette, have improved the sense organ comfort level of cigarette, therefore have more the meaning and value of actual production.
The accompanying drawing explanation
Fig. 1: the schematic flow sheet for preparing Tea Flower compound sugar and polysaccharide.
The specific embodiment
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but it will be understood to those of skill in the art that the following example is only for the present invention is described, and should not be considered as limiting scope of the present invention.Unreceipted actual conditions person in embodiment, carry out according to the condition of normal condition or manufacturer's suggestion.The unreceipted person of production firm of agents useful for same or instrument, being can be by the conventional products of commercial acquisition.
embodiment 1:1# Tea Flower compound sugar, 2# Tea Flower polysaccharide and 1# cigarette and 2#
the preparation of cigarette
1. experiment material
The Dragon Well tea Tea Flower dried flower of Tea Flower for buying.
2. the preparation of Tea Flower compound sugar and polysaccharide
Step is as follows:
(1) water extraction: take a certain amount of Dragon Well tea Tea Flower dried flower, use the hot water lixiviate to carry out 3 times and extract, solvent and Tea Flower mass ratio are 5;
(2) liquid-solid separation: adopt 200 order filter clothes that extract is separated and obtains extract with Tea Flower, merge 3 times and extract the extract obtained;
(3) micro-filtration: use the micro-filtration membrane that aperture is 50nm, system pressure is 6Bar;
(4) ultrafiltration: use the milipore filter that molecular cut off is 5000Dal to be separated, system pressure 35Bar, obtain and see through liquid and trapped fluid;
(5) compound sugar preparation: ultrafiltration sees through liquid and adopts reverse osmosis membrane to be concentrated, and system pressure 10Bar, further adopt reduced pressure concentration, and the concentrate of acquisition obtains low 1# glycan product after adopting spray-drying;
(6) polysaccharide preparation: after the ultrafiltration trapped fluid is used the de-albumen of Sevage method, use 80% ethanol to carry out alcohol and analyse, the alcohol time of analysing is 48 hours, obtains the 2# polyose after spray-drying.
Adopt recovery rate and the purity of phenolsulfuric acid colorimetric method for determining Dragon Well tea Tea Flower compound sugar, polysaccharide, the recovery rate of compound sugar is 2.6%, and polysaccharide extract rate is more than 3.5%, and purity is 90.5%.
Principle: polysaccharide or compound sugar first are hydrolyzed into monose under the effect of sulfuric acid, and dehydration generates the alditol derivative rapidly, then with phenol, generates orange-yellow compound.Again with colorimetric method for determining.
Computing formula:
3.1# and the preparation of 2# cigarette
Use water-soluble solution to be mixed with the reinforced solution that concentration is 1% the Dragon Well tea tea tree 1# Tea Flower compound sugar of acquisition, evenly be sprayed onto in pipe tobacco, roll into cigarette by normal cigarette process, 0.01%(Tea Flower compound sugar quality/tobacco quality that concrete usage ratio is tobacco quality, the following examples are identical).Obtain the 1# cigarette.
Use water-soluble solution to be mixed with the reinforced solution that concentration is 10% the Dragon Well tea tea tree 2# Tea Flower polysaccharide of acquisition, evenly be sprayed onto in pipe tobacco, roll into cigarette by normal cigarette process, 0.01%(Tea Flower polysaccharide quality/tobacco quality that concrete usage ratio is tobacco quality, the following examples are identical).Obtain the 2# cigarette.
the preparation of embodiment 2:3# Tea Flower compound sugar, 4# Tea Flower polysaccharide and 3# cigarette
1. experiment material
Tea Flower picks up from the Tie Guanyin tea plant in Anxi, Fujian.
2. the preparation of Tea Flower compound sugar and polysaccharide
Step is as follows:
(1) water extraction: take a certain amount of Iron Guanyin, use microwave extract method etc. carries out 2 times and extracts, and solvent and Tea Flower mass ratio are 15;
(2) liquid-solid separation: adopt centrifugal method that extract is separated and obtains extract with Tea Flower, centrifugation rate is 9000 rev/mins, 5 minutes time, merges 2 times and extracts the extract obtained;
(3) micro-filtration: use the micro-filtration membrane that aperture is 800nm, system pressure is 1Bar;
(4) ultrafiltration: use the milipore filter that molecular cut off is 300000Dal to be separated, system pressure 5Bar, obtain and see through liquid and trapped fluid;
(5) compound sugar preparation: ultrafiltration sees through liquid and adopts reverse osmosis membrane to be concentrated, and system pressure 40Bar, further adopt reduced pressure concentration, and the concentrate of acquisition obtains 3# compound sugar product after adopting spray-drying;
(6) polysaccharide preparation: after the ultrafiltration trapped fluid is used the de-albumen of enzyme process, use 85% ethanol to carry out alcohol and analyse, the alcohol time of analysing is 36 hours, obtains the 4# polyose after spray-drying.
Adopt recovery rate and the purity of phenolsulfuric acid colorimetric method for determining Tie Guanyin tea plant flower compound sugar, polysaccharide, the recovery rate of compound sugar is 2.8%, and polysaccharide extract rate is more than 3.9%, and purity is 92.5%.
3.3# the preparation of cigarette
Use water-soluble solution to be mixed with the reinforced solution of mixing that concentration is 10% Anxi Tieguanyin Tea tea tree 3# Tea Flower compound sugar, the 4# Tea Flower polysaccharide (both ratios are 1:1) obtained, evenly be sprayed onto in pipe tobacco, roll into cigarette by normal cigarette process, concrete usage ratio is tobacco quality 0.03%.Obtain the 3# cigarette.
embodiment 3:5# Tea Flower compound sugar, 6# Tea Flower polysaccharide and 4#-6# cigarette
preparation
1. experiment material
Tea Flower is bought the Keemun black tea tea tree from the Anhui Qimen County.
2. the preparation of Tea Flower compound sugar and polysaccharide
Step is as follows:
(1) water extraction: take a certain amount of Keemun black tea tea tree dried flower, use ultrasonic extracting method to carry out 3 times and extract, solvent and Tea Flower mass ratio are 25;
(2) liquid-solid separation: adopt the suction filtration method that extract is separated and obtains extract with Tea Flower,, merge 3 times and extract the extract obtained;
(3) micro-filtration: use the micro-filtration membrane that aperture is 200nm, system pressure is 3Bar;
(4) ultrafiltration: use the milipore filter that molecular cut off is 50000Dal to be separated, system pressure 15Bar, obtain and see through liquid and trapped fluid;
(5) compound sugar preparation: ultrafiltration sees through liquid and adopts reverse osmosis membrane to be concentrated, and system pressure 25Bar, further adopt reduced pressure concentration, and the concentrate of acquisition obtains 5# compound sugar product after adopting spray-drying;
(6) polysaccharide preparation: after the ultrafiltration trapped fluid is used the de-albumen of enzyme process, use 90% ethanol to carry out alcohol and analyse, the alcohol time of analysing is 24 hours, obtains the 6# polyose after spray-drying.
Adopt recovery rate and the purity of phenolsulfuric acid colorimetric method for determining Keemun black tea Tea Flower compound sugar, polysaccharide, the recovery rate of compound sugar is 2.5%, and polysaccharide extract rate is more than 3.2%, and purity is 92.5%.
3.4#-6# the preparation of cigarette
Use water-soluble solution to be mixed with the reinforced solution that concentration is 5% the Keemun black tea tea tree 4# Tea Flower compound sugar of acquisition, evenly be sprayed onto in pipe tobacco, by normal cigarette process, roll into cigarette, concrete usage ratio is tobacco quality 0.05%.Obtain the 4# cigarette.
Use water-soluble solution to be mixed with the reinforced solution that concentration is 5% the Keemun black tea tea tree 6# Tea Flower polysaccharide of acquisition, evenly be sprayed onto in pipe tobacco, by normal cigarette process, roll into cigarette, concrete usage ratio is tobacco quality 0.05%.Obtain the 5# cigarette.
Use water-soluble solution to be mixed with the reinforced solution that concentration is 5% the Keemun black tea tea tree 5# Tea Flower compound sugar, the 6# Tea Flower polysaccharide (both ratios are 1:3) that obtain, evenly be sprayed onto in pipe tobacco, roll into cigarette by normal cigarette process, concrete usage ratio is tobacco quality 0.05%.Obtain the 6# cigarette.
the preparation of embodiment 4:7# Tea Flower polysaccharide and 7# cigarette
1. experiment material
Tea Flower picks up from the Tie Guanyin tea plant in Anxi, Fujian.
2. the preparation of Tea Flower polysaccharide
Step is as follows:
(1) pretreatment: the Tea Flower taking-up is placed in 40 ℃ of baking ovens and is dried to moisture below 10%, with pulverizer, pulverize and obtain the Tea Flower powder;
(2) water extraction: take a certain amount of Tea Flower powder and use ultrasonic extraction to carry out 3 extractions, solvent and Tea Flower mass ratio are 10;
(3) alcohol precipitation: extract and the separation of Tea Flower powder are obtained to extract, merge and repeatedly extract the extract obtained, the reduced pressure concentration extract, to 1/5 of original volume, adds absolute ethyl alcohol to carry out alcohol precipitation 48h in concentrate, and filtration drying obtains the thick polysaccharide of Tea Flower;
(4) deproteination matter: the thick polysaccharide of Tea Flower is put into water and is redissolved, and uses the Sevage method to remove the protein in thick polysaccharide;
(5) alcohol precipitation: the polysaccharide solution after reduced pressure concentration deproteination matter, to 1/5 of original volume, adds absolute ethyl alcohol to carry out alcohol precipitation 48h in concentrate, filtration drying obtains the Tea Flower polysaccharide.
Adopt phenolsulfuric acid colorimetric determination polysaccharide extract rate and purity, the polysaccharide extract rate that the Tie Guanyin tea plant flower extracts is 1.5%, and purity is 86.5%.
3.7# the preparation of cigarette
Use water-soluble solution to be mixed with the reinforced solution of mixing that concentration is 10% the Anxi Tieguanyin Tea tea tree 7# Tea Flower polysaccharide of acquisition, evenly be sprayed onto in pipe tobacco, by normal cigarette process, roll into cigarette, concrete usage ratio is tobacco quality 0.03%.Obtain the 7# cigarette.
embodiment 5: sensory evaluating smoking's experiment
1. laboratory sample
The 1#-7# cigarette that embodiment 1-4 makes.The cigarette of 0# cigarette for making according to normal cigarette process, it does not add Tea Flower compound sugar or polysaccharide.
2. experimental technique
The sensory evaluating smoking committee of Fujian China Tobacco Industrial Co., Ltd. by GB5606.4-2005 to the comparison of being smoked panel test of 0# and 1#-7# cigarette sample.
3. experimental result
As shown in Table 1 below.
Table 1: Sensory Quality of Cigarette check original record
Smoking result shows: compare (0#) with blank cigarette, adding Tea Flower polysaccharide, the cigarette flavor matter of compound sugar, perfume quantity has lifting, can with the harmony of cigarette flavor phase, and can cover assorted gas, reduce excitant, promote pleasant impression.Polysaccharide, compound sugar are used the quality (3#, 6#) that more can promote cigarette simultaneously, especially add the 3# cigarette of Tie Guanyin tea plant flower polysaccharide, compound sugar, its indices all has lifting preferably, has increased the elegant fragrance of cigarette, promote mouthfeel, and improve smoke behavior simultaneously.The Tea Flower polysaccharide extracted according to a conventional method adds in cigarette, can promote the cigarette quality, but the Tea Flower polysaccharide that the amplitude promoted is extracted lower than the present invention.
embodiment 6: stability experiment (the sensory evaluating smoking's experiment after placement)
The 3# cigarette is placed after 5 days, 30 days, 60 days, 90 days and smoked panel test respectively, and result is as following table 2:
Table 2: aesthetic quality's inspection record of the cigarette after placement
Smoking result shows: the cigarette sample of placing 30 days is suitable with the quality of cigarette sample of placing 5 days, the cigarette sample of placing 60 days, 90 days slightly descends on perfume quantity, other indexs remain unchanged, and the sample of placing on the whole 90 days still can keep feature and the quality of cigarette.
Although the specific embodiment of the present invention has obtained detailed description, it will be understood to those of skill in the art that.According to disclosed all instructions, can carry out various modifications and replacement to those details, these change all within protection scope of the present invention.Four corner of the present invention is provided by claims and any equivalent thereof.
Claims (10)
1. the preparation method of a Tea Flower compound sugar, comprise the step of water extraction, Separation of Solid and Liquid, micro-filtration, ultrafiltration; Particularly, it also comprises counter-infiltration, concentrated, dry step;
More specifically, the preparation method of described Tea Flower compound sugar, comprise the steps:
1) water extraction: take a certain amount of fresh Tea Flower or dry Tea Flower, use hot water lixiviate, ultrasonic extraction or microwave extract method to carry out the one or many extraction;
2) liquid-solid separation: extract is separated with Tea Flower, obtain extract; Preferably, merge and repeatedly extract the extract obtained;
3) micro-filtration: adopt micro-filtration membrane to remove solid content and the suspension in extract, obtain micro-filtration and see through liquid;
4) ultrafiltration: adopt milipore filter to be separated, obtain ultrafiltration and see through liquid;
5) counter-infiltration: adopt reverse osmosis membrane that ultrafiltration is seen through to liquid and concentrated, obtain reverse osmosis concentrated liquid;
6) concentrated: as further to concentrate, obtain concentrate;
7) drying: concentrate is carried out to drying, obtain the Tea Flower compound sugar.
2. the preparation method of Tea Flower compound sugar according to claim 1 is characterized in that any one in following (1)-(7) or multinomial:
(1) mass ratio of solvent described in step 1) and Tea Flower is 5-25;
(2) be separated into centrifugal step 2) or filter;
(3) aperture of micro-filtration membrane described in step 3) is 50-800nm, and system pressure is 1-6Bar;
(4) molecular cut off of milipore filter described in step 4) is 5000-300000Dal, and system pressure is 5-35Bar;
(5) to the rejection of sodium chloride, more than 98%, system pressure is 10-40Bar to the reverse osmosis membrane described in step 5);
(6) reduced pressure concentration of simmer down to described in step 6);
(7) drying mode in step 7) is spray-drying.
3. the preparation method of a Tea Flower polysaccharide, comprise the step of water extraction, Separation of Solid and Liquid, micro-filtration, ultrafiltration; Particularly, it also comprises that de-albumen, alcohol are analysed, dry step;
More specifically, the preparation method of described Tea Flower polysaccharide, comprise the steps:
1) water extraction: take a certain amount of fresh Tea Flower or dry Tea Flower, use hot water lixiviate, ultrasonic extraction or microwave extract method to carry out the one or many extraction;
2) liquid-solid separation: extract is separated with Tea Flower, obtain extract; Preferably, merge and repeatedly extract the extract obtained;
3) micro-filtration: adopt micro-filtration membrane to remove solid content and the suspension in extract, obtain micro-filtration and see through liquid;
4) ultrafiltration: adopt milipore filter to be separated, obtain the ultrafiltration trapped fluid;
5) de-albumen: the ultrafiltration trapped fluid takes off albumen to be processed, and obtains de-protein product;
6) alcohol is analysed: will take off protein product and use ethanol to carry out alcohol to analyse, obtain alcohol and analyse thing;
7) drying: alcohol is analysed to thing and carry out drying, obtain the Tea Flower polysaccharide.
4. the preparation method of Tea Flower polysaccharide according to claim 3 is characterized in that any one in following (1)-(7) or multinomial:
(1) mass ratio of solvent described in step 1) and Tea Flower is 5-25;
(2) be separated into centrifugal step 2) or filter;
(3) aperture of micro-filtration membrane described in step 3) is 50-800nm, and system pressure is 1-6Bar;
(4) molecular cut off of milipore filter described in step 4) is 5000-300000Dal, and system pressure is 5-35Bar;
(5) Deproteinated method described in step 5) is Sevage method, enzyme process or trichloroacetic acid method;
(6) to analyse working concentration be 80% above ethanol to alcohol described in step 6), and the alcohol time of analysing is 24-48 hour;
(7) drying mode in step 7) is spray-drying.
5. a Tea Flower compound sugar, its preparation method by the described Tea Flower compound sugar of any one in claim 1 to 2 makes.
6. a Tea Flower polysaccharide, its preparation method by the described Tea Flower polysaccharide of any one in claim 3 to 4 makes.
7. a tobacco articles, it contains Tea Flower compound sugar and/or Tea Flower polysaccharide; Particularly, described tobacco product is cigarette; Particularly, described Tea Flower compound sugar is Tea Flower compound sugar claimed in claim 5; Particularly, described Tea Flower polysaccharide is Tea Flower polysaccharide claimed in claim 6; Preferably, the ratio of Tea Flower compound sugar and Tea Flower polysaccharide is (1:1)-(1:3); Particularly, the 0.001-1% that the content of described Tea Flower compound sugar and/or Tea Flower polysaccharide is tobacco quality; Be preferably 0.01-0.1%; 0.01-0.05% more preferably.
The Tea Flower compound sugar and/purposes of Tea Flower polysaccharide in preparing tobacco product; Particularly, described tobacco product is cigarette; Particularly, described Tea Flower compound sugar is Tea Flower compound sugar claimed in claim 5; Particularly, described Tea Flower polysaccharide is Tea Flower polysaccharide claimed in claim 6; Preferably, the ratio of Tea Flower compound sugar and Tea Flower polysaccharide is (1:1)-(1:3); Particularly, the 0.001-1% that the content of described Tea Flower compound sugar and/or Tea Flower polysaccharide is tobacco quality; Be preferably 0.01-0.1%; 0.01-0.05% more preferably.
9. a composition, it contains Tea Flower compound sugar claimed in claim 5 and/or Tea Flower polysaccharide claimed in claim 6; Preferably, the ratio of Tea Flower compound sugar and Tea Flower polysaccharide is (1:1)-(1:3); Particularly, described composition is food, beverage or health products.
10. Tea Flower compound sugar claimed in claim 5 and/or the purposes of Tea Flower polysaccharide claimed in claim 6 in preparing food, beverage or health products.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104186910A (en) * | 2014-08-28 | 2014-12-10 | 浙江大学 | Tea flower protein extract and application thereof |
| CN105062676A (en) * | 2015-07-29 | 2015-11-18 | 湖北中烟工业有限责任公司 | Acacia farnesiana perfume for tobacco and preparation method thereof |
| CN109393484A (en) * | 2018-12-11 | 2019-03-01 | 深圳前海金万鸿实业有限公司 | Tea flower processing technology and tea flower product |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106213577B (en) * | 2016-09-20 | 2019-01-04 | 福建中烟工业有限责任公司 | Prepare the method and Iron Guanyin water-removing tea extraction of Iron Guanyin water-removing tea extraction |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683362A (en) * | 2005-02-07 | 2005-10-19 | 黑龙江双河松嫩大豆生物工程有限责任公司 | Method for preparing soybean isoflavone, soybean spanin, oligosaccharide and soybean concentrated protein |
| CN1699586A (en) * | 2005-04-29 | 2005-11-23 | 西北大学 | Process for extracting tea polyphenol, caffeine as a byproduct thereof and tea polysaccharide from tea |
| CN1837201A (en) * | 2006-02-21 | 2006-09-27 | 张守政 | Process for extracting tea polyphenol, theanine, tea polysaccharide and tea pigment from tea |
| US20110048438A1 (en) * | 2009-08-31 | 2011-03-03 | Rodney Masri | Tea based smoking product |
| CN102675398A (en) * | 2012-05-27 | 2012-09-19 | 唐忠海 | Method for extracting momordica grosvenori glycoside V and farnesol from grosvenor momordica fruits |
| CN102702274A (en) * | 2012-06-12 | 2012-10-03 | 华东理工大学 | Method for preparing high-purity soybean oligosaccharide from soybean whey wastewater |
| CN102940074A (en) * | 2012-11-15 | 2013-02-27 | 戴群 | Tea extract for effectively retaining aroma and taste of original tea and preparation method and application thereof |
-
2013
- 2013-09-27 CN CN201310446757.9A patent/CN103478896B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683362A (en) * | 2005-02-07 | 2005-10-19 | 黑龙江双河松嫩大豆生物工程有限责任公司 | Method for preparing soybean isoflavone, soybean spanin, oligosaccharide and soybean concentrated protein |
| CN1699586A (en) * | 2005-04-29 | 2005-11-23 | 西北大学 | Process for extracting tea polyphenol, caffeine as a byproduct thereof and tea polysaccharide from tea |
| CN1837201A (en) * | 2006-02-21 | 2006-09-27 | 张守政 | Process for extracting tea polyphenol, theanine, tea polysaccharide and tea pigment from tea |
| US20110048438A1 (en) * | 2009-08-31 | 2011-03-03 | Rodney Masri | Tea based smoking product |
| CN102675398A (en) * | 2012-05-27 | 2012-09-19 | 唐忠海 | Method for extracting momordica grosvenori glycoside V and farnesol from grosvenor momordica fruits |
| CN102702274A (en) * | 2012-06-12 | 2012-10-03 | 华东理工大学 | Method for preparing high-purity soybean oligosaccharide from soybean whey wastewater |
| CN102940074A (en) * | 2012-11-15 | 2013-02-27 | 戴群 | Tea extract for effectively retaining aroma and taste of original tea and preparation method and application thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104186910A (en) * | 2014-08-28 | 2014-12-10 | 浙江大学 | Tea flower protein extract and application thereof |
| CN104186910B (en) * | 2014-08-28 | 2017-12-01 | 浙江大学 | A kind of Tea Flower protein extract and its application |
| CN105062676A (en) * | 2015-07-29 | 2015-11-18 | 湖北中烟工业有限责任公司 | Acacia farnesiana perfume for tobacco and preparation method thereof |
| CN105062676B (en) * | 2015-07-29 | 2018-11-23 | 湖北中烟工业有限责任公司 | A kind of Acacia tobacco aromaticss and preparation method thereof |
| CN109393484A (en) * | 2018-12-11 | 2019-03-01 | 深圳前海金万鸿实业有限公司 | Tea flower processing technology and tea flower product |
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|---|---|
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