CN101891774A - Production process of rhamnose - Google Patents
Production process of rhamnose Download PDFInfo
- Publication number
- CN101891774A CN101891774A CN 201010247300 CN201010247300A CN101891774A CN 101891774 A CN101891774 A CN 101891774A CN 201010247300 CN201010247300 CN 201010247300 CN 201010247300 A CN201010247300 A CN 201010247300A CN 101891774 A CN101891774 A CN 101891774A
- Authority
- CN
- China
- Prior art keywords
- rhamnosyl
- production technique
- yeast
- primary crystal
- rhamnose
- 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
Abstract
The invention belongs to the field of plant extraction, in particular to a process for producing rhamnose by adopting waste liquid produced by using flos sophorae immaturus to prepare quercetin. The technical problem to be solved by the invention is to provide a new process for producing the rhamnose, and the production process can effectively utilize the waste liquid, reduce the emissions of waste residue and waste water and be environment-friendly. The production process is completed by adopting the following steps: A) adding alkaline matters into the waste liquid, adjusting the pH value to 5-7 and standing; B) adopting edible yeast to ferment supernatant liquor obtained by standing in the step A), removing impurities, and collecting zymotic fluid; and C) concentrating the zymotic fluid, obtaining a primary crystal, refining the primary crystal and obtaining the rhamnose. The production process has the advantages of fully utilizing the waste liquid produced by using the flos sophorae immaturus to prepare the quercetin, saving resources, simplifying the production process, having no emission of waste matters, being green and environment-friendly and having low cost; and the purity of the obtained rhamnose can achieve 99%.
Description
Technical field
The invention belongs to field of plant extraction, be specifically related to adopt the sophora bud to prepare the technology of the discarded liquid production rhamnosyl of Quercetin.
Background technology
Rhamnosyl is the 6-deoxymannose, natural distributed be the L type, be 6-deoxy-L-mannose (6-de-oxy-L-mannose), claim methylpentose again.CAS number is 10030-85-0, molecular formula: C
6H
12O
5Extensively be present in polysaccharide, glucosides, vegetable jelly and the bacterial polysaccharides of plant, sugariness is 33% of a sucrose.As a kind of sweeting agent, it also has anti-inflammatory action to rhamnosyl by widely; The effect of vitamin P sample has cough-relieving apophlegmatic, relieving dyspepsia, promoting blood circulation to remove blood stasis.Be used for maldigestion, abdominal pain due to retention of food, fall pounce on that the stasis of blood is swollen, hemostasis is through closing.
At present, less at the technology report of preparation rhamnosyl, the production method that the contriver once attempted rhamnosyl is as follows:
The sophora bud obtains the sophora flower flavones through purification processing, and further separation and purification Quercetin wherein, comprises three kinds of materials in the sophora flower flavones liquid: Quercetin, rhamnosyl, glucose.In the discarded liquid that separating purifies obtains being left behind the Quercetin, rhamnosyl, glucose respectively account for half ratio, the contriver adopts ethanol to extract, separate, obtain rhamnosyl, but this method solvent usage quantity is big, cost is very high, and production cycle long (about 15 days) and the recovery and the processing of solvent have greater environmental impacts; And because impurity wherein---glucose is difficult to remove, so purity is difficult to reach 98%.Usually, most of enterprises all can simply dispose its discarded liquid, and this not only causes a large amount of fund human input, environmental pollution, also will cause the wasting of resources.
The invention human desires is sought a kind of new method and is used to produce rhamnosyl.
Summary of the invention
Technical problem solved by the invention provides a kind of brand-new technology and is used to produce rhamnosyl, and production technique can effectively utilize the sophora bud to extract the discarded liquid that produces behind the Quercetin, reduces waste residue, discharge of wastewater, and is environmentally friendly.
The production technique of rhamnosyl of the present invention is to utilize the sophora bud to extract the discarded liquid that produces behind the Quercetin, adopts following steps to finish:
A, in discarded liquid, add the alkaline matter adjust pH, leave standstill to 5-7;
B, steps A is left standstill the supernatant liquor that obtains, adopt the food-yeast fermentation, remove impurity, collect fermented liquid;
C, fermented liquid is concentrated gets the primary crystal thing, and refining primary crystal thing promptly gets rhamnosyl.
In order to improve the purity of rhamnosyl, after step B fermentation, remove impurity, add gac in the fermented liquid, decolouring is stirred, and can realize removing the part residual impurity, and guarantees the pure purpose of color and luster of rhamnosyl.
Do description below with regard to noun and parameter that the present invention occurs:
Raw material " sophora bud extracts the discarded liquid that produces behind the Quercetin ": be by the sophora bud → extractions rutin → hydrolysis reaction → filtrations → filter cake → washing filter cake to the process of neutral → refining → Quercetin, filtered liquid that obtains after filtration behind the hydrolysis reaction and washing filter cake to the waste water of neutrality generation has constituted raw material of the present invention and has discarded liquid.But the waste water that produces during owing to the washing filter cake is more, and rhamnosyl content wherein is lower, if in actual production, use this part waste water, in subsequent technique, can add too much alkaline matter, yeast, also can increase the energy consumption and the time cost of concentrated broth, actual efficiency is not high, so the discarded liquid of raw material of the present invention has following three kinds of situations: 1, filtered liquid+water lotion; 2, filtered liquid; 3, filtered liquid+portion water washing lotion.The purity that different material is formed rhamnosyl does not constitute influence, just influences the rate of recovery of rhamnosyl and energy consumption cost, the time cost of production.During practical application, reach the angle that as far as possible reduces the rhamnosyl loss from the rate of recovery, cost, the mode of preferred filtered liquid+portion water washing lotion, the part that water lotion is chosen is good with the washing leading portion.
Alkaline matter is meant alkaline matters such as sodium hydroxide, potassium hydroxide, calcium hydroxide, copper hydroxide, ironic hydroxide, ammoniacal liquor, hydrated barta.Acid in the discarded liquid is mainly sulfuric acid, and the pH value is approximately 1, and the purpose that adds alkaline matter is a neutralizing acid, and (wherein, residue is a barium sulfate, and extract is the mixture of rhamnosyl and glucose to isolate residue and extract.)
But find in the use: ammoniacal liquor is liquid, adds and uses inconvenience; Adopt sodium hydroxide, potassium hydroxide, calcium hydroxide can be brought other insoluble impuritiess into, and then cause the rhamnosyl purity drop, so in order to guarantee the rhamnosyl product purity, the preferred hydrated barta of production technique of the present invention, sulfuric acid reaction in hydrated barta and the discarded liquid generates the barium sulfate precipitate thing, the vitriol that water-fast excellent forms in other alkaline matters, in production technique of the present invention, the invention human desires makes rhamnosyl soluble in water fully, go out product by low temperature crystallization again, if there is other water-soluble impurity to bring into wherein, final impurity can enter the rhamnosyl product along with crystallization, not only reduced rhamnosyl content, removing impurity also can become technological difficulties, so preferred hydrated barta adjust pH.
Adjusting pH value to the reason of 5-7 is: surpass this scope, fermentation step is difficult to carry out, and influences the yeast effect, so can influence removal glucose, reduces rhamnosyl purity in the product.
Yeast product has several sorting techniques.The various objectives that eats and do the animal feed with the mankind can be divided into food-yeast and fodder yeast.Be divided into bread yeast, food yeast and bakers' yeast etc. in the food-yeast again.The food-yeast that the present invention adopts is selected bread yeast.
Adoptable bread yeast has yeast cake, active dry yeast and quick active dry yeast.
Wherein, yeast cake are the bulk product that contain moisture 70～73% that adopt yeast saccharomyces cerevisiae production.Be faint yellow, have structure and easily pulverizing closely, strong baking strength is arranged.But 4 ℃ of preservations about 1 month, 0 ℃ of energy preservation 2～3 months.Product is with plate-and-frame filter press the yeast-lactic press dewatering after centrifugal to be obtained at first, thereby is called as yeast cake, is commonly called as fresh yeast.
Active dry yeast: adopt containing moisture about 8%, particulate state, having the dried yeast products of baking strength of yeast saccharomyces cerevisiae production.Employing has anti-drying power, the stable alcohol mother of fermenting power obtains fresh yeast through cultivation, makes with drying through extrusion molding again.Ferment effect and yeast cake are close.
Quick active dry yeast: a kind of novel fine particle shape (diameter is less than 1mm) product of fermenting power rapidly and efficiently that has.Moisture content is 4～6%.It is on the basis of active dry yeast, adopts gene engineering to obtain highly siccostabile Wine brewing yeast strain, through special nutrition-allocated proportion and strict multiplication culture condition and adopt fluidized bed drying equipment dry and get.Compare with active dry yeast, particle is less, the fermenting power height.
The ratio of food-yeast and supernatant liquor is: food-yeast 2.5-3.5kg (yeast cake, active dry yeast and quick active dry yeast consumption are all in this scope), supernatant liquor 1000L.Yeast can not effectively be removed glucose less, thereby can not improve the purity of rhamnosyl; Yeast too much can increase cost, and can influence the follow-up filtration process in back, so this scope of selection.
Fermentation time is: 28～32h.This time range can make yeast fully remove glucose, guarantees product purity.
For abundant fermentation, ferment and appropriate to the occasionly stirred once every 2-6 hour.Stirring is in order to allow yeast fully touch liquid, so that fermentation fully can make yeast fully remove glucose, to guarantee product purity.
Among the step C, add activated carbon decolorizing and can remove the part residual impurity, and guarantee that the color and luster of rhamnosyl is pure.
Among the step D, the method for refining primary crystal thing is as follows:
(1) adds methyl alcohol and the gac that 3-4.2 doubly measures in the primary crystal thing, stir (preferably the being heated to boiling) dissolving of heating;
(2) with (1) gained material filtering, the filtrate crystallisation by cooling;
(3) the crystallisation by cooling after-filtration, be drying to obtain rhamnosyl.
Wherein, adopting the purpose of refining crystallization step (1) processing mode is for rhamnosyl is fully dissolved in the methyl alcohol, by the filtration in the step (2), removes the impurity that is insoluble in the methyl alcohol, to reach the purpose of purified product.
Further, the methyl alcohol of the preferred purity of methyl alcohol more than 99.5% (v/v).Heating can promote that rhamnosyl fully is dissolved in the methyl alcohol, and can reduce the usage quantity of methyl alcohol, and guarantees the yield of product.Adding gac is in order to decolour, to adsorb impurity, in order to avoid impurity enters crystalline product.
Because the rhamnosyl that also has not crystallization to separate out in the mother liquor that obtains after step (3) is filtered is to guarantee product yield, so filtrate filtered is concentrated, crystallisation by cooling, filters, is drying to obtain rhamnosyl.
Beneficial effect of the present invention:
1, the rhamnosyl that adopts production technique of the present invention to obtain, purity can reach 99%.
2, production technique of the present invention is easy, does not have the waste material discharging, environmental protection.
3, the sophora bud prepares the discarded liquid that Quercetin produces and is fully used, and has saved resource.
4, greatly reduce production costs: production technique of the present invention need not to use ethanol, can reduce production costs greatly than alcohol extraction technology, estimates one kilogram of rhamnosyl saving of every production cost 50-80.00 unit; And for the processing again and the recycle of mother liquor, it is about 5% to improve yield, estimates that one kilogram of rhamnosyl of every production saves cost 15-20.00 unit.
5, with short production cycle, about 5-6 days.
Embodiment
Below by specific description of embodiments of the present invention the explanation but do not limit the present invention.
Embodiment 1 utilizes the discarded liquid that produces behind the sophora bud extraction Quercetin to prepare rhamnosyl.
A, in discarded liquid, add the hydrated barta adjust pH, leave standstill to 5-7;
B, steps A is left standstill the supernatant liquor that obtains, adopt the food-yeast fermentation, the ratio of yeast and supernatant liquor is 2.5-3.5 (kg): 1000 (L); Fermentation 28-32h should ferment while stirring;
C, get and remove sedimentary fermented liquid, add gac, decolouring stir about 60min;
D, the fermented liquid that step C decolouring is obtained concentrate, and crystallization promptly gets rhamnosyl.
Concrete, adopt three primary yeasts to be prepared respectively at present embodiment:
When (1) food-yeast adopted yeast cake in the above-mentioned example: the ratio of yeast and supernatant liquor was 3.5kg: 1000L; The content of the rhamnosyl of primary crystal about about 94%.
When (2) food-yeast adopted active dry yeast in the above-mentioned example: the ratio of yeast and supernatant liquor was 3kg: 1000L; The content of the rhamnosyl of primary crystal about about 95%.
(3) in above-mentioned example food-yeast if adopt quick active dry yeast: the ratio of yeast and supernatant liquor is 2.5kg: 1000L; The content of the rhamnosyl of primary crystal about about 96%.
Embodiment 2 refining crystallizations: embodiment 1 is concentrated the crystallization that obtains adopt following method to make with extra care, promptly get rhamnosyl.
(1) the primary crystal product is adopted the refined methanol (refined methanol is that the nail determining alcohol is greater than 99.5%v/v) of 3 times of amounts and 3% gac, stir (to the boiling) dissolving of heating;
(2) (1) gained lysate is filtered the filtered liquid crystallisation by cooling;
(3) suction filtration, drying crystalline thing are rhamnosyl;
(4) suction filtration liquid concentrates, crystallisation by cooling, and suction filtration, the drying crystalline thing is rhamnosyl.
Rhamnosyl content is all more than 99% in the crystallisate.
Embodiment 3
(1) the primary crystal product is adopted the refined methanol of 4.2 times of amounts and 3% gac, stir (to the boiling) dissolving of heating;
(2) (1) gained lysate is filtered the filtered liquid crystallisation by cooling;
(3) suction filtration, drying crystalline thing are rhamnosyl;
(4) suction filtration liquid concentrates, crystallisation by cooling, and suction filtration, the drying crystalline thing is rhamnosyl.
Rhamnosyl content is all more than 99.5% in the crystallisate.
Embodiment 4
(1) the primary crystal product is adopted the refined methanol of 3.5 times of amounts and 3% gac, stir (to the boiling) dissolving of heating;
(2) (1) gained lysate is filtered the filtered liquid crystallisation by cooling;
(3) suction filtration, drying crystalline thing are rhamnosyl;
(4) suction filtration liquid concentrates, crystallisation by cooling, and suction filtration, the drying crystalline thing is rhamnosyl.
Rhamnosyl content is all more than 99.5% in the crystallisate.
Production technology of the present invention is simple, and the rhamnose that obtains is more than the purity to 99%; The site technique workflow reengineering is convenient, and feasibility is strong, does not have the waste material discharging, environmental protection; The waste liquid that the sophora bud prepares the Quercetin generation is fully used, and has saved resource; Greatly reduce production cost; Application prospect is wide.
Claims (10)
1. the production technique of rhamnosyl is characterized in that: it is that to extract the discarded liquid that produces behind the Quercetin with the sophora bud be raw material, finishes through following steps:
A, in discarded liquid, add the alkaline matter adjust pH, leave standstill to 5-7;
B, steps A is left standstill the supernatant liquor that obtains, adopt the food-yeast fermentation, remove impurity, collect fermented liquid;
C, fermented liquid is concentrated gets the primary crystal thing, and refining primary crystal thing promptly gets rhamnosyl.
2. the production technique of rhamnosyl according to claim 1 is characterized in that: after step B ferments, remove impurity, add gac in the fermented liquid, decolouring stirring, the fermented liquid employing step C processing after will decolouring again.
3. the production technique of rhamnosyl according to claim 1, it is characterized in that: the described alkaline matter of steps A is sodium hydroxide, potassium hydroxide, calcium hydroxide, copper hydroxide, ironic hydroxide, ammoniacal liquor or hydrated barta.
4. the production technique of rhamnosyl according to claim 3, it is characterized in that: the described alkaline matter of steps A is a hydrated barta.
5. the production technique of rhamnosyl according to claim 1, it is characterized in that: the ratio of yeast and supernatant liquor is 2.5-3.5kg: 1000L; Fermentation time is 28～32h.
6. the production technique of rhamnosyl according to claim 1 is characterized in that: among the step C, the method for refining primary crystal thing is as follows:
(1) methyl alcohol and the gac that primary crystal thing and 3-4.2 are doubly measured mixes;
(2) with step (1) gained material filtering, filtrate crystallisation by cooling;
(3) the crystallisation by cooling after-filtration, be drying to obtain rhamnosyl.
7. the production technique of rhamnosyl according to claim 6, it is characterized in that: methanol concentration is greater than 99.5% described in the step (1).
8. the production technique of rhamnosyl according to claim 6 is characterized in that: heat behind step (1) mixing primary crystal thing, methyl alcohol, the gac.
9. the production technique of rhamnosyl according to claim 8 is characterized in that: heat to boiling.
10. the production technique of rhamnosyl according to claim 6 is characterized in that: step (3) filtrate filtered is concentrated, crystallisation by cooling, filters, is drying to obtain rhamnosyl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102473001A CN101891774B (en) | 2010-08-06 | 2010-08-06 | Production process of rhamnose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102473001A CN101891774B (en) | 2010-08-06 | 2010-08-06 | Production process of rhamnose |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101891774A true CN101891774A (en) | 2010-11-24 |
| CN101891774B CN101891774B (en) | 2012-07-04 |
Family
ID=43101145
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102473001A Active CN101891774B (en) | 2010-08-06 | 2010-08-06 | Production process of rhamnose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101891774B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145669A (en) * | 2013-01-21 | 2013-06-12 | 李玉山 | Process of clean production of quercetin |
| CN103159725A (en) * | 2013-02-27 | 2013-06-19 | 李玉山 | Clean preparation process of high-purity hesperetin |
| CN105315317A (en) * | 2015-10-29 | 2016-02-10 | 南京中医药大学 | Product prepared by heating quercetin and rhamnose as well as preparation method and application thereof |
| CN110200255A (en) * | 2019-06-01 | 2019-09-06 | 苏州禾研生物技术有限公司 | A kind of preparation method and its usage of compound rhamnose syrup fragrance |
-
2010
- 2010-08-06 CN CN2010102473001A patent/CN101891774B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 《华南理工大学学报（自然科学版）》 20000430 浦跃武，等 5L 发酵罐生产鼠李糖的试验研究 26-29 1-10 第28卷, 第4期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145669A (en) * | 2013-01-21 | 2013-06-12 | 李玉山 | Process of clean production of quercetin |
| CN103159725A (en) * | 2013-02-27 | 2013-06-19 | 李玉山 | Clean preparation process of high-purity hesperetin |
| CN105315317A (en) * | 2015-10-29 | 2016-02-10 | 南京中医药大学 | Product prepared by heating quercetin and rhamnose as well as preparation method and application thereof |
| CN110200255A (en) * | 2019-06-01 | 2019-09-06 | 苏州禾研生物技术有限公司 | A kind of preparation method and its usage of compound rhamnose syrup fragrance |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101891774B (en) | 2012-07-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101736045B (en) | Method for continuously extracting functional components of chlorella vulgaris | |
| CN102268490B (en) | Clean technique for co-producing xylose, xylitol and arabinose from agricultural waste and forest waste | |
| CN102732585B (en) | New method for purifying fructo oligosaccharide in chicory | |
| CN103704462B (en) | Extraction and purification method for sesame proteins | |
| CN106977582A (en) | A kind of method of Hydrolysis kinetics phytosterol in deodorization distillate | |
| CN101775417A (en) | Method for extracting anthocyanin from blueberry pomace | |
| CN103087143A (en) | Method for extracting tigogenin from squeezed juice of sisal residue | |
| CN101698860A (en) | Method for producing citric acid by carrying out slag removal and fermentation on cassava | |
| CN101891774B (en) | Production process of rhamnose | |
| CN102584571A (en) | Extraction process for shikimic acid in fermentation liquor | |
| CN102040579A (en) | Method for extracting luteolin from peanut roots, stems, leaves and shells | |
| CN102250964B (en) | Production technology of starchiness raw material alcohol | |
| CN102676605A (en) | Method for producing xylose and L-arabinose using xylose mother liquor | |
| CN106146686A (en) | A kind of technique utilizing Receptaculum Helianthi industrialized production pectin | |
| CN104928341A (en) | Preparation method for ferulic acid combining ultrasonic-assisted enzymolysis and microbial-fermented bran | |
| CN102766671B (en) | Method for extracting proteins from vitamin C fermented mash | |
| CN102746366B (en) | Method for extracting tea saponin from camellia oleifera cake | |
| CN101816372B (en) | Clean production method of coproduced biologic protein feed of diosgenin | |
| CN102086149A (en) | Novel method for extracting sodium gluconate | |
| CN105039486A (en) | Method for extracting ferulic acid from wheat straw by biotechnology | |
| CN106674360A (en) | Purifying method of resistant dextrin | |
| CN104928331A (en) | Technology for preparing functional xylo-oligosaccharide by comprehensively utilizing wheat straw | |
| CN102021218B (en) | Dioscin degradation catalyst | |
| CN104892554B (en) | The preparation method of a kind of gibberic acid GA3 | |
| CN102286594A (en) | Method for producing carotenoids by fermenting high-fiber subsidiary agricultural products |
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 | ||
| C56 | Change in the name or address of the patentee |
Owner name: CHENGDU EUROPEAN PHARMACEUTICAL CO., LTD. Free format text: FORMER NAME: CHENGDU OUKANG PHARMACEUTICAL CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 611530 Sichuan city of Chengdu province Qionglai city Linchiung Industrial Park Management Committee two floor Patentee after: Chengdu Okay Pharmaceutical Co., Ltd. Address before: 611530 Sichuan city of Chengdu province Qionglai city Linchiung Industrial Park Management Committee two floor Patentee before: Chengdu Oukang Pharmaceutical Co., Ltd. |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Production process of rhamnose Effective date of registration: 20181129 Granted publication date: 20120704 Pledgee: Qionglai City branch of the Agricultural Bank of China Limited by Share Ltd Pledgor: Chengdu Okay Pharmaceutical Co., Ltd. Registration number: 2018510000131 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20211220 Granted publication date: 20120704 Pledgee: Qionglai City branch of the Agricultural Bank of China Limited by Share Ltd. Pledgor: CHENGDU OKAY PHARMACEUTICAL Co.,Ltd. Registration number: 2018510000131 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |