CN1814695A - Method fox extracting sugar-cane-leaf oxidation-resisting matter and use thereof - Google Patents
Method fox extracting sugar-cane-leaf oxidation-resisting matter and use thereof Download PDFInfo
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- CN1814695A CN1814695A CN 200610032882 CN200610032882A CN1814695A CN 1814695 A CN1814695 A CN 1814695A CN 200610032882 CN200610032882 CN 200610032882 CN 200610032882 A CN200610032882 A CN 200610032882A CN 1814695 A CN1814695 A CN 1814695A
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Abstract
This invention discloses an extraction method for an antioxidant from sugar cane leaves and its application, in which, said preparation method includes: extracting alcohol-water, concentrating and recovering solvent and drying. This invention also discloses the application of the antioxidant in the preparation of foodstuff, medicines and chemical products.
Description
Technical field
The present invention relates to a kind of extracting method and application thereof of Caulis Sacchari sinensis leaf polyphenoils.
Background technology
Polyphenoils is extensive application in industry such as food, medicine, makeup.The synthetic polyphenoils mainly comprises BHA (BHA), butyl hydroxy toluene (BHT), tertiarybutylhydroquinone (TBHQ) and Tenox PG (PG) etc., that these polyphenoils have is cheap, the characteristics of good dispersity, stable performance, there is safety issue in the synthetic polyphenoils but because fears are entertained that, countries in the world are more and more stricter to the service requirements of synthetic polyphenoils, influenced the use of this class polyphenoils.Natural anti-reflecting oxide comprises kind surplus sage extract, Radix Glycyrrhizae extract, natural VE, tea-polyphenol, sodium phytate, the phosphatide etc. 40, and is safe all from the extract of natural animal-plant, is the focus of current polyphenoils research.But the raw material of natural anti-reflecting oxide is subjected to the region restriction, and the exploitation of natural anti-reflecting oxide must be carried out according to the characteristics of this country.The natural anti-reflecting oxide that China ratifies to use at present mainly contains tea-polyphenol, sodium phytate, Radix Glycyrrhizae extract, phosphatide etc.
Sugarcane (Saccharum sinensisRoxb) claim potato sugarcane, dried sugarcane again, be per nnial herb, all there are a large amount of cultivations provinces and regions such as China Guangdong, Guangxi, Fujian, Taiwan, Hainan, Jiangxi, produce about 6,960 ten thousand tons of sugarcane per year, and wherein the sugarcane leaf-making quantity is about 4,000,000 tons.The main application of sugarcane is to utilize contained sugar in the sugarcane stem, produces sucrose, or directly eats raw as fruit, and the sugarcane leaf is used as fuel and the animal feed except that part, and major part is dropped or is used for go back to the field.In fact Caulis Sacchari sinensis leaf contains the material that a large amount of flavones and Polyphenols etc. have anti-oxidant activity, and this class material is proposed and recycled, and can produce the healthcare products raw material with anti-oxidant, antisenility function or be used for food fresh keeping.Because Caulis Sacchari sinensis leaf as feed, is not seen untoward reaction for a long time, as seen its edible safety is very high, therefore utilizes Caulis Sacchari sinensis leaf to produce the Caulis Sacchari sinensis leaf polyphenoils, has broad application prospects, and yet there are no the report of producing the Caulis Sacchari sinensis leaf polyphenoils.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, primary and foremost purpose of the present invention is to provide a kind of extracting method of Caulis Sacchari sinensis leaf polyphenoils.Simply efficient, with low cost, the clean environmental protection of this extracting method, suitable large-scale industrial production.
Primary and foremost purpose of the present invention is achieved through the following technical solutions: the extracting method of described Caulis Sacchari sinensis leaf polyphenoils comprises the steps:
1. ethanol～hydro-thermal refluxing extraction: sugarcane leaf drying, fragmentation, extract with 20～40% aqueous ethanolic solution by weight percentage;
2. vacuum concentration, reclaim solvent: vacuum concentration reclaims etoh solvent, precipitation separation; Get Caulis Sacchari sinensis leaf polyphenoils concentrated solution;
3. dry: as, to make Caulis Sacchari sinensis leaf polyphenoils crude product with Caulis Sacchari sinensis leaf polyphenoils concentrated solution drying.
Described step 1. in preferred especially sugarcane leaf: aqueous ethanolic solution is about 1: 20 by weight; Step 2. vacuum concentration to concentrated solution volume is about 1/12 of a material liquid volume.
In order to realize the present invention better, the 2. middle concentrated solution of step adopts twice extracting flavone class of propyl carbinol material, and vacuum concentration reclaims propyl carbinol, gets Caulis Sacchari sinensis leaf polyphenoils medicinal extract; In Caulis Sacchari sinensis leaf polyphenoils medicinal extract, add entry, fully disperse,, make the smart powder of Caulis Sacchari sinensis leaf polyphenoils through super-dry.
The 2. middle precipitation separation of described step adopts Plate Filtration or centrifugal separation method; Described dry adopt spraying drying or lyophilize; The weight ratio that extracts concentrated solution and propyl carbinol the described first time is 1: 1; The weight ratio that extracts for the second time concentrated solution and propyl carbinol is 1: 0.75; The water that adds about 20 times of weight in Caulis Sacchari sinensis leaf polyphenoils medicinal extract, described recovered solvent ethanol and recovered solvent propyl carbinol can be recycled and reused for and extract the Caulis Sacchari sinensis leaf polyphenoils.
Another object of the present invention is to provide the application of above-mentioned Caulis Sacchari sinensis leaf polyphenoils in preparation food, Chemicals and medicine etc., turn waste into wealth, make full use of the purpose of resource to reach.
For verify by method of the present invention extract the resistance of oxidation of product, the contriver has carried out the detection of following several respects to the polyphenoils product that obtains from Caulis Sacchari sinensis leaf:
A) general flavone content of Caulis Sacchari sinensis leaf polyphenoils
With the rutin is standard substance, measures the content of Flavonoid substances in the smart powder of Caulis Sacchari sinensis leaf polyphenoils crude product and Caulis Sacchari sinensis leaf polyphenoils, sees Table 1.
The Flavonoid substances content of two kinds of Caulis Sacchari sinensis leaf polyphenoils of table 1
| Caulis Sacchari sinensis leaf polyphenoils crude product | The smart powder of Caulis Sacchari sinensis leaf polyphenoils | |
| General flavone content (%) | 7.96 | 12.5 |
B) adopt DPPH (free radical scavenging activity) method, studied the removing free radical ability of two kinds of Caulis Sacchari sinensis leaf polyphenoils solution of different concns, be converted into Caulis Sacchari sinensis leaf polyphenoils quality, then the removing free radical ability of 0.026mg, 0.052mg, 0.104mg, 0.156mg Caulis Sacchari sinensis leaf polyphenoils crude product and 0.011mg, 0.022mg, 0.044mg, 0.088mg, the smart powder of 0.11mg Caulis Sacchari sinensis leaf polyphenoils is seen Fig. 2.
C) Caulis Sacchari sinensis leaf polyphenoils oxidation-resistance detects
Adopt the linolic acid experimental technique, studied the resistance of oxidation of two kinds of Caulis Sacchari sinensis leaf polyphenoils solution of different concns respectively, be converted into Caulis Sacchari sinensis leaf polyphenoils quality, then 0.026mg, 0.052mg, 0.104 * 10
-5The ability of the anti-linolic acid oxidation of mg, 0.156mg Caulis Sacchari sinensis leaf polyphenoils crude product and 0.022mg, 0.044mg, 0.088mg, 0.110mg, the smart powder of 0.154mg Caulis Sacchari sinensis leaf polyphenoils is seen Fig. 3.
D) the Caulis Sacchari sinensis leaf polyphenoils prevents the detection of soybean oil oxidation capacity
Adopt grease to preserve experiment, studied the ability that prevents the soybean oil oxidation of the smart powder of Caulis Sacchari sinensis leaf polyphenoils of different additions, the results are shown in Figure 4.
In sum, the Caulis Sacchari sinensis leaf polyphenoils has very strong removing free radical ability and prevents the ability of Oxidation of Fat and Oils, it is a kind of very ideal natural anti-reflecting oxide, can be widely used in food, medicine, makeup and chemical industry, developing thisly has the polyphenoils of application prospect significant undoubtedly to the Economic development that promotes vast sucrose producing region.
The present invention compared with prior art, have the following advantages and beneficial effect: the extraction agent that the present invention adopts is an ethanol-water solution, extraction agent is a propyl carbinol, is the solvent of safety non-toxic, and polarity of solvent is moderate, a large amount of propositions of the impurity such as chlorophyll in the sugarcane leaf had both been prevented, fully extracted flavones ingredient again, by reclaim under reduced pressure, most of ethanol and propyl carbinol can utilize again, guarantee whole process of production safety, environmental protection, efficient, be fit to scale operation.The production method of the smart powder of Caulis Sacchari sinensis leaf polyphenoils crude product of the present invention and Caulis Sacchari sinensis leaf polyphenoils has reached the purpose that reduces cost, the requirement that can satisfy the different users.Caulis Sacchari sinensis leaf polyphenoils product can be widely used in food, medicine, makeup and chemical industry, and is significant for the Economic development that improves sugarcane grower's income, the vast product sugar of quickening district.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 removes the DPPH design sketch for the Caulis Sacchari sinensis leaf polyphenoils;
Fig. 3 tries hard to for the anti-linolic acid energy of oxidation of Caulis Sacchari sinensis leaf polyphenoils;
Fig. 4 is the influence figure of the smart powder of the Caulis Sacchari sinensis leaf polyphenoils of different additions to storage soybean oil peroxide value.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment one: the extraction of Caulis Sacchari sinensis leaf polyphenoils (spray-drying process)
Shown in Fig. 1 process flow sheet:
1. ethanol～hydro-thermal refluxing extraction: 20kg sugarcane leaf drying, be crushed to about 10 orders, extract, adopt the filter press filtering and impurity removing with the aqueous ethanolic solution reflux 2h of 400L 30%, sugarcane leaf ethanol extract 362L;
2. concentrate, reclaim solvent: vacuum concentration (60 ℃～70 ℃ of vacuum tightness 0.09Mpa, temperature) reclaims ethanol to concentrated solution volume 30L, adopts the centrifugal separation method precipitation separation; Get concentrated solution 30L;
3. spraying drying:, make Caulis Sacchari sinensis leaf polyphenoils crude product 0.52kg with 15L Caulis Sacchari sinensis leaf polyphenoils concentrated solution spraying drying;
4. extraction: other gets concentrated solution 15L, adds 15L propyl carbinol and twice extracting flavone class of 12L propyl carbinol material successively, merges the propyl carbinol phase, and vacuum concentration (80 ℃～90 ℃ of vacuum tightness 0.09Mpa, temperature) reclaim under reduced pressure propyl carbinol gets Caulis Sacchari sinensis leaf polyphenoils medicinal extract; Caulis Sacchari sinensis leaf polyphenoils medicinal extract 0.38kg; Commentaries on classics is dissolved in the 8L water, and thorough mixing is made suspension liquid;
5. spraying drying:, make the smart powder 0.29kg of Caulis Sacchari sinensis leaf polyphenoils with the suspension liquid spraying drying.
Embodiment two: the extraction of Caulis Sacchari sinensis leaf polyphenoils (freeze-drying)
1. ethanol～hydro-thermal refluxing extraction: 200g sugarcane leaf drying, be crushed to about 10 orders, extract, adopt the centrifugation removal of impurities with the ethanol-water solution reflux 2h of 4L 30%, sugarcane leaf ethanol extract 3.62L;
2. concentrate, reclaim solvent: vacuum concentration (60 ℃～70 ℃ of vacuum tightness 0.09Mpa, temperature) reclaims ethanol to concentrated solution volume 0.30L, adopts Plate Filtration method precipitation separation; Get the about 0.30L of concentrated solution;
3. lyophilize:, make Caulis Sacchari sinensis leaf polyphenoils crude product 5.5g with the lyophilize of 0.15L Caulis Sacchari sinensis leaf polyphenoils concentrated solution;
4. extraction: other gets concentrated solution 0.15L, add 0.15L propyl carbinol and twice extracting flavone class of 0.12L propyl carbinol material successively, merge the propyl carbinol phase, vacuum concentration (80 ℃～90 ℃ of vacuum tightness 0.09Mpa, temperature) reclaim under reduced pressure propyl carbinol gets Caulis Sacchari sinensis leaf polyphenoils medicinal extract; Caulis Sacchari sinensis leaf polyphenoils medicinal extract 4.1g commentaries on classics is dissolved in the 0.08L water, and thorough mixing is made suspension liquid;
5. lyophilize:, make the smart powder 3.1g of Caulis Sacchari sinensis leaf polyphenoils with the suspension liquid lyophilize.
Embodiment three: the extraction of Caulis Sacchari sinensis leaf polyphenoils (spray-drying process)
1. ethanol～hydro-thermal refluxing extraction: 20kg sugarcane leaf drying, be crushed to about 20 orders, extract, adopt the centrifugation removal of impurities with the aqueous ethanolic solution reflux 2h of 400L 40%, sugarcane leaf ethanol extract 369L;
2. concentrate, reclaim solvent: vacuum concentration (60 ℃～70 ℃ of vacuum tightness 0.09Mpa, temperature) reclaims ethanol to concentrated solution volume 30L, adopts the centrifugal separation method precipitation separation; Get concentrated solution 30L;
3. spraying drying:, make Caulis Sacchari sinensis leaf polyphenoils crude product 0.57kg with 15L Caulis Sacchari sinensis leaf polyphenoils concentrated solution spraying drying;
4. extraction: other gets concentrated solution 15L, add 12L propyl carbinol and twice extracting flavone class of 7.5L propyl carbinol material successively, merge the propyl carbinol phase, vacuum concentration (80 ℃～90 ℃ of vacuum tightness 0.09Mpa, temperature) reclaim under reduced pressure propyl carbinol gets Caulis Sacchari sinensis leaf polyphenoils medicinal extract; Caulis Sacchari sinensis leaf polyphenoils medicinal extract 0.42kg; Commentaries on classics is dissolved in the 8L water, and thorough mixing is made suspension liquid;
5. spraying drying:, make the smart powder 0.30kg of Caulis Sacchari sinensis leaf polyphenoils with the suspension liquid spraying drying.
Embodiment four: the extraction of Caulis Sacchari sinensis leaf polyphenoils (freeze-drying)
1. ethanol～hydro-thermal refluxing extraction: 200g sugarcane leaf drying, be crushed to about 15 orders, extract, adopt the filter press filtering and impurity removing with the ethanol-water solution reflux 2h of 4L 20%, sugarcane leaf ethanol extract 3.62L;
2. concentrate, reclaim solvent: vacuum concentration (60 ℃～70 ℃ of vacuum tightness 0.09Mpa, temperature) reclaims ethanol to concentrated solution volume 0.3L, adopts Plate Filtration method precipitation separation; Get the about 0.3L of concentrated solution;
3. lyophilize:, make Caulis Sacchari sinensis leaf polyphenoils crude product 0.53g with the lyophilize of 0.15L Caulis Sacchari sinensis leaf polyphenoils concentrated solution;
4. extraction: other gets concentrated solution 0.15L, add 0.15L propyl carbinol and twice extracting flavone class of 0.12L propyl carbinol material successively, merge the propyl carbinol phase, vacuum concentration (80 ℃～90 ℃ of vacuum tightness 0.09Mpa, temperature) reclaim under reduced pressure propyl carbinol gets Caulis Sacchari sinensis leaf polyphenoils medicinal extract; Caulis Sacchari sinensis leaf polyphenoils medicinal extract 3.5g; Commentaries on classics is dissolved in the 0.08L water, and thorough mixing is made suspension liquid;
5. lyophilize:, make the smart powder 0.26g of Caulis Sacchari sinensis leaf polyphenoils with the suspension liquid lyophilize.
Embodiment five: be applied to protective foods
Take by weighing Caulis Sacchari sinensis leaf polyphenoils crude product, food starch, Magnesium Stearate by 2: 3: 1 weight ratios, each composition of mixing, be mixed with Caulis Sacchari sinensis leaf polyphenoils health care medicinal powder, make capsule by every ball 0.25g health care medicinal powder, anti-oxidant as having, the anti-ageing health care foods of waiting for a long time is used.
Embodiment six: be applied to medicine
Take by weighing Caulis Sacchari sinensis leaf polyphenoils crude product, food starch, Magnesium Stearate by 2: 3: 1 weight ratios, each composition of mixing, be mixed with Caulis Sacchari sinensis leaf polyphenoils health care medicinal powder, make capsule by every ball 0.25g, the medicine of anti-oxidant as having, the anti-ageing function of waiting for a long time uses.
Embodiment seven: as greasy polyphenoils
By 100～200mg/kg consumption the smart powder of Caulis Sacchari sinensis leaf polyphenoils is added in the grease, can reduce greasy oxidising process, prolong the greasy quality guaranteed period, to add the smart powder of 0.02% Caulis Sacchari sinensis leaf polyphenoils in soybean oil is example, under 63 ℃ of preservation conditions, can make the soybean oil peroxide value reach the time retardation 9 days of 30meg/kg.
Embodiment eight: the preparation sunscreen
Be used to prepare sunscreen, its raw material consumption (by weight percentage) is:
The smart powder 0.2%～0.5% of Caulis Sacchari sinensis leaf polyphenoils; Stearic acid: 1.5%～4.5%; Silicone oil: 3%～8%; Jojoba oil: 0.3%～0.85%; Ethyl p-hydroxybenzoate: 0.02%～0.2%; Triglyceride: 2.0%～5.0%; Glycerine: 3%～8%; Tegin 55G: 0.2%～3%; EDTA:0.1%～0.5%; Essence: 0.01%～0.05%, rest part is a deionized water.
Embodiment nine: be applied to drinks
The fresh sugarcane leaf of 5kg is cleaned, dry, be crushed to about 10 orders, add basic wine (alcoholic strength the is 40 °) 100L by rice fermentation production of ethanol content 40%, soaked 10 days press filtration about 25 ℃, get the about 88L of sugarcane phyllopodium wine, it is right that sugarcane phyllopodium wine is colluded, and Plate Filtration gets sugarcane leaf wine (alcoholic strength is 38 °) 91L.This sugarcane leaf wine by every bottle of 500ml packing, is inserted several tender cores of sugarcane leaf in every bottle and makees decoration, obtain little green, limpid characteristic sugarcane leaf wine.
Claims (10)
1, a kind of extracting method of Caulis Sacchari sinensis leaf polyphenoils is characterized in that comprising the steps:
1. ethanol～hydro-thermal refluxing extraction: sugarcane leaf drying, fragmentation, extract with 20～40% aqueous ethanolic solution by weight percentage;
2. vacuum concentration, reclaim solvent: vacuum concentration reclaims etoh solvent, precipitation separation; Get Caulis Sacchari sinensis leaf polyphenoils concentrated solution;
3. dry: as, to make Caulis Sacchari sinensis leaf polyphenoils crude product with Caulis Sacchari sinensis leaf polyphenoils concentrated solution drying.
2, the extracting method of Caulis Sacchari sinensis leaf polyphenoils according to claim 1 is characterized in that: the 1. middle sugarcane leaf of described step: aqueous ethanolic solution is counted 1: 20 by weight.
3, the extracting method of Caulis Sacchari sinensis leaf polyphenoils according to claim 1 is characterized in that: step 2. vacuum concentration to concentrated solution volume is 1/12 of a material liquid volume.
4, the extracting method of Caulis Sacchari sinensis leaf polyphenoils according to claim 1 is characterized in that: step 2. described in precipitation separation adopt Plate Filtration or centrifugation; Described recovered solvent ethanol is recycled and reused for and extracts the Caulis Sacchari sinensis leaf polyphenoils.
5, the extracting method of Caulis Sacchari sinensis leaf polyphenoils according to claim 1 is characterized in that: step 2. described in concentrated solution adopt twice extraction of propyl carbinol, vacuum concentration reclaims solvent, n-butanol, Caulis Sacchari sinensis leaf polyphenoils medicinal extract; In Caulis Sacchari sinensis leaf polyphenoils medicinal extract, add entry, fully disperse,, make the smart powder of Caulis Sacchari sinensis leaf polyphenoils through super-dry.
6, the extracting method of Caulis Sacchari sinensis leaf polyphenoils according to claim 1 or 5 is characterized in that: described dry adopt spraying drying or lyophilize.
7, the extracting method of Caulis Sacchari sinensis leaf polyphenoils according to claim 6 is characterized in that: the weight ratio that extracts concentrated solution and propyl carbinol the described first time is 1: 1; The weight ratio that extracts for the second time concentrated solution and propyl carbinol is 1: 0.75.
8, the extracting method of Caulis Sacchari sinensis leaf polyphenoils according to claim 6 is characterized in that: the water that adds 20 times of weight in Caulis Sacchari sinensis leaf polyphenoils medicinal extract.
9, the extracting method of Caulis Sacchari sinensis leaf polyphenoils according to claim 6 is characterized in that: described recovered solvent propyl carbinol is recycled and reused for and extracts the Caulis Sacchari sinensis leaf polyphenoils.
10, the application of the Caulis Sacchari sinensis leaf polyphenoils that extracting method extracted of each described Caulis Sacchari sinensis leaf polyphenoils of claim 1～9 in preparation food, Chemicals or medicine.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101530193A (en) * | 2009-04-20 | 2009-09-16 | 四川大学 | Method for comprehensively extracting and purifying oxidation-resistant active ingredient in sugarcane toppers or slag |
| CN101337035B (en) * | 2008-08-08 | 2011-10-12 | 广西中医学院 | Traditional Chinese preparation with bacteriostatic action for preventing blood sugar rising and preparation method thereof |
| CN102660290A (en) * | 2012-04-27 | 2012-09-12 | 东北林业大学 | Acorn shell pigment with antioxidant activity and preparation method and application thereof |
| CN103007090A (en) * | 2013-01-16 | 2013-04-03 | 广西中医药大学 | Preparation and application of sugarcane leaf extractive for preventing and curing decsyed teeth and preparations |
| CN104957602A (en) * | 2015-05-22 | 2015-10-07 | 长沙普源生物科技有限公司 | Sugarcane bioactive component composition, functional health food, and preparation method of sugarcane bioactive component composition and functional health food |
| CN113248382A (en) * | 2021-05-26 | 2021-08-13 | 云南农业大学 | Antioxidant compound and preparation method and application thereof |
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2006
- 2006-01-13 CN CNB2006100328825A patent/CN100467567C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337035B (en) * | 2008-08-08 | 2011-10-12 | 广西中医学院 | Traditional Chinese preparation with bacteriostatic action for preventing blood sugar rising and preparation method thereof |
| CN101530193A (en) * | 2009-04-20 | 2009-09-16 | 四川大学 | Method for comprehensively extracting and purifying oxidation-resistant active ingredient in sugarcane toppers or slag |
| CN102660290A (en) * | 2012-04-27 | 2012-09-12 | 东北林业大学 | Acorn shell pigment with antioxidant activity and preparation method and application thereof |
| CN102660290B (en) * | 2012-04-27 | 2014-03-12 | 东北林业大学 | Acorn shell pigment with antioxidant activity and preparation method and application thereof |
| CN103007090A (en) * | 2013-01-16 | 2013-04-03 | 广西中医药大学 | Preparation and application of sugarcane leaf extractive for preventing and curing decsyed teeth and preparations |
| CN104957602A (en) * | 2015-05-22 | 2015-10-07 | 长沙普源生物科技有限公司 | Sugarcane bioactive component composition, functional health food, and preparation method of sugarcane bioactive component composition and functional health food |
| CN113248382A (en) * | 2021-05-26 | 2021-08-13 | 云南农业大学 | Antioxidant compound and preparation method and application thereof |
| CN113248382B (en) * | 2021-05-26 | 2023-08-18 | 云南农业大学 | Antioxidant compound and preparation method and application thereof |
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