CN109232487A - One kind extracting ascorbic method from Rosa roxburghii Tratt - Google Patents
One kind extracting ascorbic method from Rosa roxburghii Tratt Download PDFInfo
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- CN109232487A CN109232487A CN201811124432.8A CN201811124432A CN109232487A CN 109232487 A CN109232487 A CN 109232487A CN 201811124432 A CN201811124432 A CN 201811124432A CN 109232487 A CN109232487 A CN 109232487A
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- rosa roxburghii
- roxburghii tratt
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- ascorbic
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/62—Three oxygen atoms, e.g. ascorbic acid
Abstract
The present invention relates to Rosa roxburghii Tratt manufacture fields, in particular to one kind, and ascorbic method is extracted from Rosa roxburghii Tratt, the described method comprises the following steps (1) grinding, enzymatic hydrolysis；(2) it extracts；(3) it separates, be concentrated；In the process of lapping of raw material, with alcohol vapour, CO2Gas is as protective gas, it is suppressed that the activity of enzyme in grinding raw material prevents the substances oxidation stain such as phenols, reduces the coloring of the oxidation material of vitamin C finished product.
Description
Technical field
The present invention relates to Rosa roxburghii Tratt manufacture fields, in particular to one kind, and ascorbic method is extracted from Rosa roxburghii Tratt.
Background technique
Rosa roxburghii Tratt is the fruit of rosaceae rose rosa roxburghii, also known as the spring is sent to return, and is distributed mainly on Southwestern China area,
It is the abundantest with Guizhou resource-saving, it is ethnic group's medication, there is the effect of digestion-promoting spleen-invigorating, astringing to arrest diarrhea, be mainly used for treating
Having indigestion abdominal distension, the diseases such as diarrhea.Through modern research shows that Fructus Rosae Normalis extract and its Triterpenoid (such as Euscaphicoside, roxburic acid, open country
Multiflorin etc.) adjust body's immunity, anti-aging, removing toxic substances, antiatherosclerosis, resisting stress, it is antitumor, anti-inflammatory,
Analgesia, the mononuclear cell proliferation for inhibiting immune response inhibit the sides such as B cell, T cell and macrophage in peripheral blood, inhibition HIV
Face shows certain pharmacological activity, in addition, the chemical components such as triterpene, flavones, polysaccharide, vitamin are mainly contained in Rosa roxburghii Tratt, because
It is referred to as " three chloroazotic acid fruits " rich in vitamin C, citrin and superoxide dismutase (SOD), Vitamin C content is macaque
10 times of peach.Wherein vitamin C is a kind of important water soluble vitamin, hypovitaminosis related with the multiple metabolism of human body
It can lead to the symptoms such as bleeding, skeleton change and poor wound healing, it is huge for the demand of vitamin.
There is following manner: 1, supercritical extract for ascorbic extraction at present, extracts safety, temperature is room temperature, yield
Height, but the device is complicated, investment is big；2, historrhexis's extraction method, safety, energy conservation, efficiently, do not destroy ingredient, scalable, preferably
Various solvents, but which is leachable to the various composition in raw material, further increases each component separation complexity；
3, continuous backflow method；Save solvent, high-efficient, but heated length, small scale, ingredient destructible, 4, infusion method, it is simple, investment is small,
Safety, but low efficiency, time-consuming, perishable low efficiency, time-consuming, perishable, 5, circumfluence method, the good, high income of selectivity, but
That poor selectivity, ingredient destructible, post-processing are difficult, it is seen that with upper type time consumption, efficiency, component preservation on
There is certain defect.
Application No. is CN201610860071.8 disclose it is a kind of ascorbic method is extracted from Chinese ephedra fruit, pass through by
Chinese ephedra fruit raw material is crushed, is digested, is ultrasonically treated, and filter residue and filtrate are separately extracted, gelatin is added, chitosan, leads to
Cross microfiltration membranes and carry out purification process, finally by purified product by polyamide column chromatography successively by washing, ethanol elution, dense
After contracting, drying, it is extracted vitamin C, improves ascorbic content, but the invention is in ascorbic extraction process
Vitamin C is not protected, the vitamin C of dissolution can be oxidized when contacting with air, lead to ascorbic contain
It measures low, causes wastage of material.
Summary of the invention
The present invention extracts ascorbic method in order to solve the above technical problems, providing one kind from Rosa roxburghii Tratt.
Realize particular by following technical scheme: one kind extracting ascorbic method from Rosa roxburghii Tratt, including following
Step (1) grinding, enzymatic hydrolysis: it first by air-dried Rosa roxburghii Tratt, cleans, sterilize, being ground into 90-120 mesh, and fruit of Grossularia burejensis Berger volume 1- is added
2 times of water stirs 3-5min, and 5-6min is ground in the grinding pot for being equipped with protective gas, and addition quality is fruit of Grossularia burejensis Berger
0.04%-0.06% complex enzyme, constantly grinding 20-40min, sterilize 5-8min, obtains Rosa roxburghii Tratt mixed liquor；(2) it extracts: will go out
Tea Saponin mixed liquor is added in Rosa roxburghii Tratt mixed liquor after bacterium, constantly shakes, then sodium chloride is added in time 10min, from
The heart, filtering obtain Rosa roxburghii Tratt clarification permeate, for use；(3) it separates, be concentrated: step 2 gained Rosa roxburghii Tratt being clarified in permeate and is added
Nitration mixture is separated using separation film device, obtains seperation film permeate, seperation film is ultrafiltration membrane, reuses device for ultrafiltration membrane
Concentration is carried out to seperation film permeate, alkali is added, the nitration mixture in concentrate is neutralized, vitamin C concentrate is obtained, -20
It is freeze-dried, crystallizes at~-40 DEG C.
The raw material after smashing is ground under protective gas first, enzyme is added, the macromoleculars such as fiber, starch in process of lapping
Substance be first ground to the molecule of small level-one, the raw material after grinding mixes more equal with cellulase, amylase, protease
It is even, it is more easier to adhere to, at this time alcohol vapour and CO2As protection gas, in the case where protecting gas shielded, raw material continues to be ground, former
The substances such as phenols, vitamin in material further dissolve out, and organic matter evaporates thicker with alcohol vapour formation in the Rosa roxburghii Tratt of part
Isolation layer, prevent vitamin to be oxidized, CO2The activity for reducing core polyphenol oxidase, galactosidase, reduces raw material
The problem that darkens caused by middle phenols oxidation stain in vitamin C finished product, and another aspect complex enzyme B ultrasound oxide discrimination
Change enzyme removing and be oxidized free radical present in vitamin C, vitamin C is restored, Tea Saponin mixed liquor, mixed liquor is then added
In in addition to Tea Saponin is there are also chitosan, chitosan is surfactant, is beneficial to increase ascorbic dissolution rate, make dimension give birth to
Plain C is gradually accumulated, secondly, being 20-35 DEG C in temperature, part isomerism, the product of generation can occur between Tea Saponin molecule
That is the isomer of Tea Saponin contains the aldehyde radical for being also easy to be oxidized, glycosyl etc., than ascorbic originality in the isomers
It is stronger, vitamin C can be effectively prevent to be oxidized, ascorbic dissolution rate, Tea Saponin generation are increased by chitosan in this way
For vitamin C oxidation, ascorbic content is increased, the vitamin C of dissolution is between Tea Saponin mixed liquor and sodium chloride solution
Constantly flowing, is dissolved in sodium chloride solution, forms more stable vitamin C, is divided Rosa roxburghii Tratt clarification permeate
From concentration, primarily to the further vitamin C in purification sodium chloride, is to big point in Rosa roxburghii Tratt clarification permeate first
Sub- substance and pigment are separated, and the nitration mixture added in separation process can aoxidize to avoid vitamin C, and nitration mixture is oxalic acid, phosphorus
Acid, hydrochloric acid, two or three in acetic acid, the nitration mixture according to same volume than mixing, concentration 3-9%, under the concentration
Nitration mixture will not be aoxidized with the product after concentration.
Further, the nitration mixture includes oxalic acid, phosphoric acid, hydrochloric acid, two or three in acetic acid.
Further, mixed volume sour in the nitration mixture is identical, and the concentration for mixing acid later is 3-9%.
Further, molecular cut off is 20000- when ultrafiltration membrane progress separating treatment used in the step (3)
27000, molecular cut off is 7000-10000 when being concentrated.
Further, the protection gas is alcohol vapour, CO2According to volume by for (1-2): 3 mixing, temperature are 3-6 DEG C.
Further, the complex enzyme is divided into two parts A, B, and order of addition is first to add A, then add B when grinding.
Further, the complex enzyme A is (3.5-5): (1- according to mass ratio by cellulase, amylase, protease
3) it: 1:(0.1-0.3) mixes.
Further, the complex enzyme B is superoxide dismutase.
Further, the sodium chloride concentration is 21-35%, and additive amount is the half of Tea Saponin mixed liquor quality.
Further, the Tea Saponin mixed liquor by chitosan, Tea Saponin according to mass ratio be (2-4): (1-2) mixing and
At.
In conclusion the beneficial effects of the present invention are: the first, this process simplify production technologies, improve production effect
Rate ensure that ascorbic quality；The second, the present invention in producing process be added chitosan, Tea Saponin, sodium chloride, nitration mixture into
Row is dissolved, is extracted, preventing the measures such as oxidation, and ascorbic recovery rate is increased to 50% or more；In third, the present invention rationally
Fruit of Grossularia burejensis Berger is utilized, effectively prevent vitamin C during the extraction process because oxidation caused by lose；4th, in raw material
Process of lapping in, with alcohol vapour, CO2Gas is as protective gas, it is suppressed that the activity of enzyme in grinding raw material prevents phenol
The substances oxidation stain such as class, reduces the coloring of the oxidation material of vitamin C finished product.
Specific embodiment
Specific embodiments of the present invention will be described in further detail below, but the invention is not limited to these realities
Mode is applied, it is claimed to still fall within the claims in the present invention for any improvement or replacement on the present embodiment essence spirit
Range.
Embodiment 1
(1) it grinds, digest: first by air-dried Rosa roxburghii Tratt, cleaning, sterilize, being ground into 90-120 mesh, and Single Roxburgh Rose Fruit entity is added
The water of 1 times of product stirs 5min, is being equipped with alcohol vapour and CO2As 6min is ground in the grinding pot of protective gas, quality is added
For 0.05% complex enzyme of fruit of Grossularia burejensis Berger, complex enzyme A, B two parts, A is cellulase, amylase, protease, and B is super oxygen
Complex enzyme A, complex enzyme B is first added in object mutase, constantly grinding 20-40min, and sterilize 5-8min, obtains Rosa roxburghii Tratt mixed liquor；
(2) it extracts: Tea Saponin, chitosan will be added in the Rosa roxburghii Tratt mixed liquor after sterilizing, continuous to shake, the time is
10min, it is 24% sodium chloride that concentration, which is then added, is centrifuged, filtering, obtains Rosa roxburghii Tratt clarification permeate, for use；
(3) it separates, be concentrated: being divided nitration mixture is added in step 2 gained Rosa roxburghii Tratt clarification permeate using separation film device
From obtaining seperation film permeate, seperation film is ultrafiltration membrane, reuses device for ultrafiltration membrane and carries out at concentration to seperation film permeate
Alkali is added in reason, neutralizes the nitration mixture in concentrate, obtains vitamin C concentrate, be freeze-dried at -15 DEG C, crystallizes；
Control group 1
(1) step is the same as embodiment 1
(2) it extracts: extracting: Tea Saponin will be added in the Rosa roxburghii Tratt mixed liquor after sterilizing, constantly shake, time 10min,
Then it is 24% sodium chloride that concentration, which is added, is centrifuged, filtering, obtains Rosa roxburghii Tratt clarification permeate, for use；
Control group 2
(1) step is the same as embodiment 1
(2) it extracts: Tea Saponin, distilled water will be added in the Rosa roxburghii Tratt mixed liquor after sterilizing, continuous to shake, the time is
10min, it is 24% sodium chloride that concentration, which is then added, is centrifuged, filtering, obtains Rosa roxburghii Tratt clarification permeate, for use；
Control group 3
(1) step is the same as embodiment 1
(2) it extracts: extracting: chitosan will be added in the Rosa roxburghii Tratt mixed liquor after sterilizing, distilled water constantly shakes, the time
For 10min, it is 24% sodium chloride that concentration, which is then added, is centrifuged, filtering, obtains Rosa roxburghii Tratt clarification permeate, for use；
Control group 4
(1) step is the same as embodiment 1
(2 extract: chitosan, benzene sulfonic acid will be added in the Rosa roxburghii Tratt mixed liquor after sterilizing, continuous to shake, the time is
10min, it is 24% sodium chloride that concentration, which is then added, is centrifuged, filtering, obtains Rosa roxburghii Tratt clarification permeate, for use；
Control group 5
(1) step is the same as embodiment 1
(2) it extracts: Tea Saponin, benzene sulfonic acid will be added in the Rosa roxburghii Tratt mixed liquor after sterilizing, continuous to shake, the time is
10min, it is 24% sodium chloride that concentration, which is then added, is centrifuged, filtering, obtains Rosa roxburghii Tratt clarification permeate, for use；
Control group 6
(1) it digests, grind: first by air-dried Rosa roxburghii Tratt, cleaning, sterilize, being ground into 90-120 mesh, and Single Roxburgh Rose Fruit entity is added
The water of 1 times of product stirs 5min, and addition quality is 0.05% complex enzyme of fruit of Grossularia burejensis Berger, and complex enzyme A, B two parts, A is cellulose
Enzyme, amylase, protease, B are catalase, and complex enzyme B is first added, and are being equipped with alcohol vapour, CO2The grinding of protective gas
6min is ground in tank, adds complex enzyme A, constantly grinding 20-40min, and sterilize 5-8min, obtains Rosa roxburghii Tratt mixed liquor；
(2), (3) other steps are the same as embodiment 1；
Control group 7
(1) step is the same as embodiment 1
(2 extract: it is 30 DEG C that sodium chloride, temperature will be added in the Rosa roxburghii Tratt mixed liquor after sterilizing, and continuous to shake, the time is
Chitosan is added after adding Tea Saponin, standing 9h in 10min, is centrifuged, filtering, obtains Rosa roxburghii Tratt clarification permeate, for use；
(3) step is the same as embodiment 1；
Control group 8
(1) it grinds, digest: first by air-dried Rosa roxburghii Tratt, cleaning, sterilize, being ground into 90-120 mesh, and Single Roxburgh Rose Fruit entity is added
The water of 1 times of product stirs 5min, is being equipped with alcohol vapour and O2As 6min is ground in the grinding pot of protective gas, wherein O2It is located at
The innermost layer of material, alcohol vapour are located at outermost layer, and addition quality is 0.05% complex enzyme of fruit of Grossularia burejensis Berger, complex enzyme A, B two
Part, A are cellulase, amylase, protease, and B is superoxide dismutase, and complex enzyme B is first added, and complex enzyme A is constantly ground
20-40min is ground, sterilize 5-8min, obtains Rosa roxburghii Tratt mixed liquor；
(2), (3) other steps are the same as embodiment 1；
Test 1
(1) the prepared solution of control group 1-4 is put into incubator, incubator temperature is 30 DEG C, and solution and air are certainly
By contacting, it is protected from light after saving 2h in incubator, absorbance is measured using ultraviolet specrophotometer, and will be each right
Being recorded in table 1 according to the absorbance change value after preservation 2h, 4h in group, (note: absorbance changes >=5% and is considered as vitamin C concentration
It changes)；
(2) vitamin obtained by embodiment 1,6-8 is used in the every 100g product of high effective liquid chromatography for measuring and is contained
How many mg vitamin Cs, and result is recorded in table 2；
Table 1
| Control group | Control group 1 | Control group 2 | Control group 3 | Control group 4 | Control group 5 |
| 2h | 2% | 5% | 1% | 6% | 30% |
| 4h | 7% | 28% | 3% | 26% | 100% |
Table 2
| Group | Embodiment 1 | Control group 6 | Control group 7 | Control group 8 |
| Content mg/g | 398 | 387 | 384 | 389 |
As shown in Table 1, when vitamin C finished product being configured to different solution being detected, after 2h, absorbance changes
Most fast is control group 5, addition distilled water is made solution, followed by addition chitosan, benzene sulfonic acid sodium salt, changes minimum addition
Chitosan, Tea Saponin, it is seen that chitosan, Tea Saponin can effectively improve ascorbic stability；
As shown in Table 2, ascorbic content highest in embodiment 1, it is seen that increase Vitamin C content, passing through addition tea
Saponin, chitosan and sodium chloride, nitration mixture, which mutually act synergistically, makes ascorbic content highest, is to add in control group 6-8
The change of protective gas component, Tea Saponin, chitosan solution, sodium chloride and nitration mixture conditional during work, it is seen that use pair
Embodiment 1 is respectively less than according to the extracted ascorbic content of group 6-8；
It is important to point out that, above embodiments and test example are only limitted to do further technical solution of the present invention herein
Elaboration and understanding, should not be understood as it is further to technical solution of the present invention limited, what those skilled in the art made
The innovation and creation of non-protruding essential characteristics and marked improvement still fall within protection category of the invention.
Claims (10)
1. one kind extracts ascorbic method from Rosa roxburghii Tratt, which is characterized in that the described method comprises the following steps (1) grinding, enzyme
Solution: first by air-dried Rosa roxburghii Tratt, cleaning, sterilize, being ground into 90-120 mesh, and the water of 1-2 times of fruit of Grossularia burejensis Berger volume is added, and stirs 3-
5min grinds 5-6min in the grinding pot for being equipped with protective gas, and it is that fruit of Grossularia burejensis Berger 0.04%-0.06% is compound that quality, which is added,
Enzyme, constantly grinding 20-40min, sterilize 5-8min, obtains Rosa roxburghii Tratt mixed liquor；(2) it extracts: by the Rosa roxburghii Tratt mixture after sterilizing
Tea Saponin mixed liquor is added in liquid, constantly shakes, then sodium chloride is added in time 10min, be centrifuged, and it is clear to obtain Rosa roxburghii Tratt for filtering
Clear permeate, for use；(3) it separates, be concentrated: step 2 gained Rosa roxburghii Tratt being clarified into addition nitration mixture in permeate and uses separation film device
It is separated, obtains seperation film permeate, seperation film is ultrafiltration membrane, reuses device for ultrafiltration membrane and carries out to seperation film permeate
Alkali is added in concentration, neutralizes the nitration mixture acid in concentrate, obtains vitamin C concentrate, freezes at -20~-40 DEG C dry
It is dry, crystallization.
2. ascorbic method is extracted from Rosa roxburghii Tratt as described in claim 1, which is characterized in that the nitration mixture include oxalic acid,
Phosphoric acid, hydrochloric acid, two or three in acetic acid.
3. ascorbic method is extracted from Rosa roxburghii Tratt as claimed in claim 2, which is characterized in that sour in the nitration mixture to mix
Zoarium product is identical, and the concentration for mixing acid later is 3-9%.
4. ascorbic method is extracted from Rosa roxburghii Tratt as described in claim 1, which is characterized in that used in the step (3)
It is 20000-27000 that ultrafiltration membrane, which carries out molecular cut off when separating treatment, and molecular cut off is 7000-10000 when being concentrated.
5. ascorbic method is extracted from Rosa roxburghii Tratt as described in claim 1, which is characterized in that the protection gas is ethyl alcohol
Steam, CO2According to volume by for (1-2): 3 mixing, temperature are 3-6 DEG C.
6. ascorbic method is extracted from Rosa roxburghii Tratt as described in claim 1, which is characterized in that the complex enzyme is divided into A, B
Two parts, order of addition is first to add A, then add B when grinding.
7. ascorbic method is extracted from Rosa roxburghii Tratt as claimed in claim 6, which is characterized in that the complex enzyme A is by fiber
Plain enzyme, amylase, protease are (3.5-5): (1-3): 1:(0.1-0.3 according to mass ratio) it mixes.
8. ascorbic method is extracted from Rosa roxburghii Tratt as claimed in claim 6, which is characterized in that the complex enzyme B is super oxygen
Compound mutase.
9. ascorbic method is extracted from Rosa roxburghii Tratt as described in claim 1, which is characterized in that the sodium chloride concentration is
21-35%, additive amount are the half of Tea Saponin mixed liquor quality.
10. ascorbic method is extracted from Rosa roxburghii Tratt as described in claim 1, which is characterized in that the Tea Saponin mixed liquor
By chitosan, Tea Saponin according to mass ratio be (2-4): (1-2) is mixed.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811124432.8A CN109232487A (en) | 2018-09-26 | 2018-09-26 | One kind extracting ascorbic method from Rosa roxburghii Tratt |
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Cited By (4)
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| CN110623951A (en) * | 2019-08-21 | 2019-12-31 | 湖北科技学院 | Preparation method of vitamin C granules in rosa roxburghii |
| CN114307241A (en) * | 2021-12-31 | 2022-04-12 | 海南黎草纪新生物科技有限公司 | Extraction method for kiwi fruit extract |
| CN114468086A (en) * | 2022-03-03 | 2022-05-13 | 贵州大学 | Roxburgh rose black tea and preparation method thereof |
| CN115260335A (en) * | 2022-09-28 | 2022-11-01 | 中国农业大学 | Method and system for simultaneously extracting rosa roxburghii polysaccharide, rosa roxburghii polyphenol and rosa roxburghii SOD and Vc from rosa roxburghii residues |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110623951A (en) * | 2019-08-21 | 2019-12-31 | 湖北科技学院 | Preparation method of vitamin C granules in rosa roxburghii |
| CN114307241A (en) * | 2021-12-31 | 2022-04-12 | 海南黎草纪新生物科技有限公司 | Extraction method for kiwi fruit extract |
| CN114468086A (en) * | 2022-03-03 | 2022-05-13 | 贵州大学 | Roxburgh rose black tea and preparation method thereof |
| CN115260335A (en) * | 2022-09-28 | 2022-11-01 | 中国农业大学 | Method and system for simultaneously extracting rosa roxburghii polysaccharide, rosa roxburghii polyphenol and rosa roxburghii SOD and Vc from rosa roxburghii residues |
| WO2024066140A1 (en) * | 2022-09-28 | 2024-04-04 | 中国农业大学 | Method and system for simultaneously extracting rosa roxburghii tratt polysaccharide, rosa roxburghii tratt polyphenol, rosa roxburghii tratt sod, and vc from rosa roxburghii tratt pomace |
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Application publication date: 20190118 |