CN104561188A - Process for preparing tagatose through cottonseed meal - Google Patents
Process for preparing tagatose through cottonseed meal Download PDFInfo
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- CN104561188A CN104561188A CN201410825940.4A CN201410825940A CN104561188A CN 104561188 A CN104561188 A CN 104561188A CN 201410825940 A CN201410825940 A CN 201410825940A CN 104561188 A CN104561188 A CN 104561188A
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- tagatose
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- raffinose
- lactosi
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Abstract
The invention particularly relates to a process for preparing tagatose through cottonseed meal. The process is characterized by comprising the following steps: 1) extracting the cottonseed meal with an alcoholic solution, removing the alcohol, performing ultrafiltration to remove macromolecular substance, and obtaining raffinose crude extracting liquid; 2) adding alpha-galactosidase to the raffinose crude extracting liquid obtained in the step 1), hydrolyzing the solution, performing decoloration by activated carbon, ion exchange and condensation on the hydrolysate, and utilizing a ternary sequential simulant moving bed to separate, so as to respectively obtain a sucrose component, a D-galactose component and a raffinose component; 3) regulating the concentration of the separated D-galactose solution, adding calcium oxide, performing reaction for a period of time, regulating the pH value of the solution, filtering, so as to obtain the mixed liquid containing tagatose and D-galactose; 4) decoloring the mixed liquid obtained in the step 3), then performing ion exchange to desalt, further carrying out evaporation and concentration, separating by the simulant moving bed to obtain tagatose syrup, and finally concentrating the tagatose syrup to obtain the tagatose product. The process disclosed by the invention has the advantages of reasonable process, high safety and reliability in production and low production cost.
Description
Technical field
The present invention is specifically related to the technique that a kind of cottonseed meal prepares tagatose.
Background technology
Cottonseed meal be cottonseed after lint, shelling, Kernel-hull separation, the byproduct obtained after oil is got in precompressed lixiviate or direct solvent lixiviate.At present, for the exploitation of cottonseed meal, domestic being confined to produces feed, and as produced feed protein, low gossypol cotton albumen, added value is low.
Tagatose (tagatose) belongs to the one of rare sugar, and six-carbon ketone sugar is the epimer of fructose.White odorless crystalline powder, taste is sweet, and sugariness is 92% of equivalent sucrose, and the heat produced is only 1/3 (1.5kcal/g) of sucrose, fusing point 132 ~ 135 DEG C, and water-soluble, in water, solubleness is 62% (30 DEG C).To thermally-stabilised, second-order transition temperature 15 DEG C, easy crystallization, water absorbability is low.Acid resistance is strong, stable in the scope of pH2 ~ 7.Easy generation caramelization and Maillaid braun reaction.Natural tagatose is mainly present in the milk-product such as yogurt, milk powder.
Tagatose product has obtained the food sanitation department approvals such as the U.S., Australia, Japan, Korea S, New Zealand at present and has used.In China, within 2014, national health State Family Planning Commission approved tagatose is new food raw material, but does not obtain industrialization at home.Much more external adopt chemical method and process for producing tagatose through bio-enzymatic, chemical method needs to use an alkali metal salt or alkaline-earth metal as isomery agent, and environmental pollution is serious; Take lactose as raw material, produce glucose sugar after hydrolysis, glucose and semi-lactosi are difficult to be separated, and yield is low.
Chinese patent " a kind of preparation method of functional sweetener D-tatai sugar " (application number: CN200610085922) and Chinese patent " use the galactose isomerization of high yield to manufacture the method for tagatose " (application number: CN200780045683), two patents are all direct take semi-lactosi as raw material production tagatose, raw materials cost is very high, can not carry out suitability for industrialized production.
Chinese patent " uses soy oligosaccharide to produce the method for tagatose " (application number: CN200980103383), and application chromatography carries out separation semi-lactosi and tagatose, and separation efficiency is low, is not suitable for Industry Promotion.
Chinese patent " a kind of fermentation lactobacillus and utilize it to prepare the method for D-Tag " (application number: CN200910025982), D-Tag is 50% to the transformation efficiency of substrate, transformation efficiency is lower, and the sterility requirements of strain culturing to production facility is higher, and front-end investment is more.
Summary of the invention
The object of the invention is to solve and produce the high defect of tagatose raw materials cost at present, a kind of rational technology is provided, production safety is reliable, the cottonseed meal that production cost is low prepares the technique of tagatose, with cheap cottonseed meal for raw material, through extracting raffinose, enzymolysis, the operations such as isomery obtain tagatose and D-semi-lactosi, and application simulation moving-bed carries out separation and purification, the D-semi-lactosi of obtained high yield, then D-semi-lactosi is utilized to continue to produce tagatose, raw material sources are extensive and with low cost, thus it is more single to solve current tagatose raw materials, and the problem that raw materials cost is high.
The present invention is achieved by the following technical solution:
Namely cottonseed meal prepares a technique for tagatose, it is characterized in that step is as follows:
1) cottonseed meal is by after alcoholic solution lixiviate dealcoholysis, removes macromolecular substance, obtain raffinose crude extract through ultrafiltration;
2) by step 1) in raffinose crude extract add alpha-galactosidase and be hydrolyzed, hydrolyzed solution through activated carbon decolorizing, from friendship, concentrated after, utilize the sequential simulated moving bed separation of ternary, obtain sucrose component, D-semi-lactosi component and raffinose component respectively;
3) after isolated D-galactose solution being regulated concentration, add calcium oxide, reaction for some time, regulator solution pH, filter, obtain the mixed solution containing tagatose and D-semi-lactosi;
4) by step 3) in the decolouring of gained mixed solution, ion-exchange desalination, after evaporation concentration, through simulation moving-bed separation, obtaining tagatose slurry, obtaining tagatose product finally by concentrating.
Step 1) in, alcoholic solution is ethanol, and concentration is 60% ~ 90%, and during lixiviate, solid-liquid ratio is 1: 8 ~ 1: 12, and Extracting temperature is 0 DEG C ~ 70 DEG C, extraction time 0.5h ~ 3.5h.
Step 2) in, alpha-galactosidase addition is 0.02g/g ~ 0.04g/g, hydrolysis time is 150 ~ 300min, in hydrolyzed solution, the content of sucrose is 45 ~ 55%, the content of D-semi-lactosi is 42 ~ 45%, the content of residue raffinose is 1-5%, and after hydrolysis, solution boiling 10min at 80 DEG C goes out enzyme.
Step 2) in, the sequential simulated moving bed separation condition of ternary is, ternary is entered sequential simulated moving bed with the speed of 2.0L/h-4.0L/h, 60 DEG C-80 DEG C, switching time be 10min-20min condition under be separated, obtaining D-galactose content in D-semi-lactosi component is 87.3% ~ 95.2%.
Step 3) in, be after 15 ~ 25% by D-galactose solution quality of regulation concentration, add the calcium oxide that mol ratio is 1:1, in less than 20 DEG C reaction 30 ~ 150min, then regulator solution pH is 5.8, filter, obtain the mixed solution containing tagatose and D-semi-lactosi, in mixed solution, the content of tagatose is 70 ~ 80%.
Step 4) in the concentration > 95% of tagatose product.
The sequential simulated moving bed product for Nanjing Kaitong Grain Biochemical Research & Design Co., Ltd.'s production of ternary of the present invention, model is SSMB-200L, and separating medium is the positive resin of calcium type, 8 rod structures.
Sequential simulated moving bed technology is called for short SSMB technology, the simulation moving-bed of a kind of batch sequence operation, compared with common simulation moving bed technique, its many switch-valve that circular flow can be cut off on circulation line device can be used for one the outlet being separated intermediate component outflow, it adopts intermittent feeding and the different order of intermittent take-off, the operational mode of distinct program simultaneously, the mixture separation of ternary component can be three independent cuts by the operation scheme of the conversion program of order more than this, is applicable to the separation of ternary component.
Relative to the production technique of prior art tagatose, tool of the present invention has the following advantages:
1) raw material of the present invention is the wide material sources of cottonseed meal, cottonseed meal, cheap;
2) raffinose crude extract alpha-galactosidase carries out decomposing obtained D-semi-lactosi, and enzyme digestion reaction is thorough, and D-semi-lactosi transformation efficiency is high;
3) apply chromatographic separation to be separated enzymolysis solution, D-semi-lactosi and other two kinds of sugar are easily separated, and D-semi-lactosi yield is high, and purity is high;
4) D-semi-lactosi adopts calcium oxide to carry out isomery, and transformation efficiency is high, and impurity calcium ion is easily separated.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is further described:
Embodiment 1
In the present embodiment, the extraction process of raffinose crude extract is:
1) detoxification degreased cottonseed meal is through alcoholic solution lixiviate, filters, gets filtrate, after dealcoholysis, remove macromolecular substance through ultrafiltration, obtain raffinose crude extract, add ethanol (concentration is 70%), solid-liquid ratio is 1: 10, Extracting temperature is 30 DEG C, and under water-bath, condensing reflux extracts 3h, after cooling, collect and filter, obtain raffinose crude extract;
2) get appropriate raffinose crude extract, add alpha-galactosidase (addition is 0.02g/g), hydrolysis 150min, after hydrolysis, solution boiling 10min at 80 DEG C goes out enzyme; Get quantitative enzyme hydrolysis and carry out liquid-phase chromatographic analysis, result is: in hydrolyzed solution, sucrose content is 51.8%, D-galactose content is 42.6%, and the content of raffinose is 4.6%; Hydrolyzed solution, through activated carbon decolorizing, from friendship, after concentrated, enters ternary with the speed of 2.0L/h sequential simulated moving bed, 60 DEG C, switching time be 15min condition under be separated, obtaining D-galactose content in D-semi-lactosi component is 95.2%;
3) be after 15% by isolated D-galactose solution quality of regulation concentration, add the calcium oxide that mol ratio is 1:1,60min is reacted in less than 20 DEG C, then regulator solution pH is 5.8, filter, obtain the mixed solution containing tagatose and D-semi-lactosi, in the mixed solution obtained, the content of tagatose is 74.7%;
4) mixed solution is decoloured again, ion-exchange desalination, after evaporation concentration, through simulation moving-bed separation, obtain tagatose slurry, obtain tagatose product finally by concentrated, purity is 92.8%.
Embodiment 2
In the present embodiment, the extraction process of raffinose crude extract is:
1) detoxification degreased cottonseed meal is through alcoholic solution lixiviate, filters, gets filtrate, after dealcoholysis, remove macromolecular substance through ultrafiltration, obtain raffinose crude extract, add ethanol (concentration is 75%), solid-liquid ratio is 1: 8, Extracting temperature is 50 DEG C, and under water-bath, condensing reflux extracts 2h, after cooling, collect and filter, obtain raffinose crude extract;
2) get appropriate raffinose crude extract, add alpha-galactosidase (addition is 0.03g/g), hydrolysis 200min, after hydrolysis, solution boiling 10min at 80 DEG C goes out enzyme; Get quantitative enzyme hydrolysis and carry out liquid-phase chromatographic analysis, result is: in hydrolyzed solution, sucrose content is 52.2%, D-galactose content is 43.2%, and raffinose content is 3.6%; Hydrolyzed solution, through activated carbon decolorizing, from friendship, after concentrated, enters ternary with the speed of 3.0L/h sequential simulated moving bed, 70 DEG C, switching time be 13min condition under be separated, obtaining D-galactose content in D-semi-lactosi component is 87.9%;
3) be after 20% by isolated D-galactose solution quality of regulation concentration, add the calcium oxide that mol ratio is 1:1,120min is reacted in less than 20 DEG C, then regulator solution pH is 5.8, filter, obtain the mixed solution containing tagatose and D-semi-lactosi, in the mixed solution obtained, the content of tagatose is 80.0%;
4) mixed solution is decoloured again, ion-exchange desalination, after evaporation concentration, through simulation moving-bed separation, obtain tagatose slurry, obtain tagatose product finally by concentrated, purity is 98.7%.
Embodiment 3
In the present embodiment, the extraction process of raffinose crude extract is:
1) detoxification degreased cottonseed meal is through alcoholic solution lixiviate, filters, gets filtrate, after dealcoholysis, remove macromolecular substance through ultrafiltration, obtain raffinose crude extract, add ethanol (concentration is 80%), solid-liquid ratio is 1: 12, Extracting temperature is 70 DEG C, and under water-bath, condensing reflux extracts 3h, after cooling, collect and filter, obtain raffinose crude extract;
2) get appropriate raffinose crude extract, add alpha-galactosidase (addition is 0.04g/g), hydrolysis 300min, after hydrolysis, solution boiling 10min at 80 DEG C goes out enzyme; Get quantitative enzyme hydrolysis and carry out liquid-phase chromatographic analysis, result is sucrose content be 52.0%, D-galactose content is 45.2%, and raffinose content is 1.8%; Hydrolyzed solution, through activated carbon decolorizing, from friendship, after concentrated, enters ternary with the speed of 4.0L/h sequential simulated moving bed, 80 DEG C, switching time be 10min condition under be separated, obtaining D-galactose content in D-semi-lactosi component is 89.7%;
3) be after 25% by isolated D-galactose solution quality of regulation concentration, add the calcium oxide that mol ratio is 1:1,150min is reacted in less than 20 DEG C, then regulator solution pH is 5.8, filter, obtain the mixed solution containing tagatose and D-semi-lactosi, in the mixed solution obtained, the content of tagatose is 78.8%;
4) mixed solution is decoloured again, ion-exchange desalination, after evaporation concentration, through simulation moving-bed separation, obtain tagatose slurry, obtain tagatose product finally by concentrated, purity is 95.6%.
Claims (6)
1. cottonseed meal prepares a technique for tagatose, it is characterized in that step is as follows:
1) cottonseed meal is by after alcoholic solution lixiviate dealcoholysis, removes macromolecular substance, obtain raffinose crude extract through ultrafiltration;
2) by step 1) in raffinose crude extract add alpha-galactosidase and be hydrolyzed, hydrolyzed solution through activated carbon decolorizing, from friendship, concentrated after, utilize the sequential simulated moving bed separation of ternary, obtain sucrose component, D-semi-lactosi component and raffinose component respectively;
3) after isolated D-galactose solution being regulated concentration, add calcium oxide, reaction for some time, regulator solution pH, filter, obtain the mixed solution containing tagatose and D-semi-lactosi;
4) by step 3) in the decolouring of gained mixed solution, ion-exchange desalination, after evaporation concentration, through simulation moving-bed separation, obtaining tagatose slurry, obtaining tagatose product finally by concentrating.
2. a kind of cottonseed meal according to claim 1 prepares the technique of tagatose, it is characterized in that step 1) in, alcoholic solution is ethanol, concentration is 60% ~ 90%, during lixiviate, solid-liquid ratio is 1: 8 ~ 1: 12, and Extracting temperature is 0 DEG C ~ 70 DEG C, extraction time 0.5h ~ 3.5h.
3. a kind of cottonseed meal according to claim 1 prepares the technique of tagatose, it is characterized in that step 2) in, alpha-galactosidase addition is 0.02g/g ~ 0.04g/g, hydrolysis time is 150 ~ 300min, in hydrolyzed solution, the content of sucrose is 45 ~ 55%, the content of D-semi-lactosi is 42 ~ 45%, and the content of residue raffinose is 1-5%, and after hydrolysis, solution boiling 10min at 80 DEG C goes out enzyme.
4. a kind of cottonseed meal according to claim 1 prepares the technique of tagatose, it is characterized in that step 2) in, the sequential simulated moving bed separation condition of ternary is, ternary is entered sequential simulated moving bed with the speed of 2.0L/h-4.0L/h, 60 DEG C-80 DEG C, switching time be 10min-20min condition under be separated, obtaining D-galactose content in D-semi-lactosi component is 87.3% ~ 95.2%.
5. a kind of cottonseed meal according to claim 1 prepares the technique of tagatose, it is characterized in that step 3) in, be after 15 ~ 25% by D-galactose solution quality of regulation concentration, add the calcium oxide that mol ratio is 1:1, in less than 20 DEG C reaction 30 ~ 150min, then regulator solution pH is 5.8, filters, obtain the mixed solution containing tagatose and D-semi-lactosi, in mixed solution, the content of tagatose is 70 ~ 80%.
6. a kind of cottonseed meal according to claim 1 prepares the technique of tagatose, it is characterized in that step 4) in the concentration > 95% of tagatose product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410825940.4A CN104561188A (en) | 2014-12-26 | 2014-12-26 | Process for preparing tagatose through cottonseed meal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315920A (en) * | 2021-12-29 | 2022-04-12 | 山东百龙创园生物科技股份有限公司 | Preparation method of isomerized lactose |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948500A (en) * | 2006-05-26 | 2007-04-18 | 江南大学 | Preparation method of functional sweetener D-tatai sugar |
| CN104140988A (en) * | 2013-05-07 | 2014-11-12 | 南京中医药大学 | Process of preparing D-galactose by extracting cottonseed meal |
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- 2014-12-26 CN CN201410825940.4A patent/CN104561188A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948500A (en) * | 2006-05-26 | 2007-04-18 | 江南大学 | Preparation method of functional sweetener D-tatai sugar |
| CN104140988A (en) * | 2013-05-07 | 2014-11-12 | 南京中医药大学 | Process of preparing D-galactose by extracting cottonseed meal |
Non-Patent Citations (1)
| Title |
|---|
| 信成夫等: "化学异构法生产塔格糖的研究", 《中国食品添加剂》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315920A (en) * | 2021-12-29 | 2022-04-12 | 山东百龙创园生物科技股份有限公司 | Preparation method of isomerized lactose |
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Application publication date: 20150429 |