CN107496290A - A kind of method for extracting rice bran polyphenol and application - Google Patents
A kind of method for extracting rice bran polyphenol and application Download PDFInfo
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- CN107496290A CN107496290A CN201710767463.4A CN201710767463A CN107496290A CN 107496290 A CN107496290 A CN 107496290A CN 201710767463 A CN201710767463 A CN 201710767463A CN 107496290 A CN107496290 A CN 107496290A
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- rice bran
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- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 77
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 76
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- 235000009566 rice Nutrition 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 37
- 240000007594 Oryza sativa Species 0.000 title 1
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- 238000000605 extraction Methods 0.000 claims abstract description 23
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- 239000002904 solvent Substances 0.000 description 4
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Birds (AREA)
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- Mycology (AREA)
- Engineering & Computer Science (AREA)
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- Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Biotechnology (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Nutrition Science (AREA)
- Emergency Medicine (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Dermatology (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a kind of method for extracting rice bran polyphenol and application, belong to plant polyphenol extractive technique field.It the described method comprises the following steps：Using rice bran powder as raw material, the glycerite that concentration of volume percent is 5~15% is added according to 25~35mL/g liquid ratios, 1~2h is extracted in 60~70 DEG C of water-baths, supernatant is separated and collected, produces rice bran polyphenol extract solution.The present invention carries out the extraction of rice bran polyphenol using glycerine, glycerine Nantural non-toxic, avoid the potential safety hazard brought using other toxic reagents, in addition, glycerine is the constituent in some food or cosmetics, therefore, the extract solution that prepared by the present invention can be directly made an addition in these products, be advantageous to industrialization production；In addition, glycerine is advantageous to extract more polyphenol substances from rice bran.The present invention utilizes response phase method optimization optimised process, while extraction efficiency is improved, reduces the discharge of energy consumption and pollutant, has the practical significance of industrialization production.
Description
Technical field
The present invention relates to plant polyphenol extractive technique field, and in particular to a kind of method for extracting rice bran polyphenol and application.
Background technology
Polyphenol is a kind of Secondary metabolites, is the derivative of phosphopentose in plant, shikimic acid and Phenylpropanoid Glycosides approach
Thing.Polyphenol in cereal kind skin predominantly has the very phenolic acid of strong anti-oxidative activity, flavone compound and OPC etc., pole
Has potentiality to be exploited.Research shows, phenolic compound has the effect such as preferable anti-oxidant, colour generation, antibacterial in cereal, food,
Medicine and other fields have good application prospect.
Rice bran is the superficial layer being attached to after paddy husking on brown rice, by exocarp, middle pericarp, cross-linked layer, kind skin and paste
Bisque forms, and accounts for the 5~7% of paddy quality.China's rice bran stock number is occupied first of the world, and annual production is more than 16,000,000 tons.Rice
Chaff is a kind of renewable resource having a large capacity and a wide range.Rice bran is utilized mainly as feed at present, and otherwise utilization are also
Have much room for improvement.Rice bran is the good source of polyphenol substance, and the polyphenol substance species in rice bran is more, content is high, is a kind of inexpensive thing
Beautiful polyphenol substance natural resources.Therefore, it is significant in actual life to develop and utilize rice bran polyphenol.
Solvent extraction is one of current domestic most popular polyphenol extracting method, is mainly used in extracting soluble phenolics
Class compound, using phenol generalizations such as solvent extraction extraction grape seed polyphenols, Chinese chestnut shell polyphenol, pericarp of Fructus Musae polyphenol in existing report
Compound, conventional solvent have methanol, ethanol, acetone.Polyphenol source is different, when its suitable extracting condition, digestion agent, extraction
Between, the extraction conditions such as temperature, number it is also different, it is most commonly seen as 60-70% ethanol using volume fraction, but ethanol valency
Lattice are higher and reclaim inconvenience, and there is many deficiencies in application.Organic reagent that solvent extraction uses is inflammable, partly has
Poison, it is very unfavorable to keeping the safety in production.
Therefore, in order to rationally efficiently extract the polyphenol substance in rice bran, need badly a kind of simple to operate, cost of offer compared with
It is low, recovery rate is high, the extracting method of safe green.
The content of the invention
It is an object of the invention to provide it is a kind of it is simple to operate, cost is cheap, safe green, and can be rationally efficiently from rice
The method that polyphenol substance is extracted in chaff.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method for extracting rice bran polyphenol, comprises the following steps：Using rice bran powder as raw material, according to 25~35mL/g liquid
Expect, than adding the glycerite that concentration of volume percent is 5~15%, 1~2h to be extracted in 60~70 DEG C of water-baths, is separated and collected
Supernatant, produce rice bran polyphenol extract solution.
Rice bran is the good source of polyphenol substance, is a kind of renewable resource having a large capacity and a wide range, it is developed, had
Preferable economic benefit and social benefit.
The present invention uses extractant of the glycerine as rice bran polyphenol substance, because glycerine is a kind of the biological molten of Nantural non-toxic
Agent, not only facilitates cost-effective, and avoids the potential safety hazard that other toxic reagents are brought.Research of the present invention has shown that, sweet
Oil contributes to the dissolution of rice bran polyphenol substance.
Described rice bran powder after 70~80 DEG C of conditions are dried, is made by fresh rice bran after being crushed to 60~80 mesh.
The present invention is optimized using response phase method to the factor for influenceing the more phenol extractions of rice bran, is sent out in single factor experiment
Existing, liquid ratio, glycerol concentration, Extracting temperature are 3 principal elements.
Preferably, described liquid ratio is 28~30mL/g.
Described glycerite is the mixture of glycerine and water.G ＆ W is all natural materials, is carried using glycerite
After taking, without further removing solvent, the extract solution for collecting to obtain can be directly used for producing.
Preferably, the concentration of volume percent of described glycerite is 8~10%.
Preferably, described bath temperature is 63~65 DEG C.
After the completion of extraction, using centrifugation carry out separation of solid and liquid, it is described be separated into 10000~11000 turns/min centrifugation 10~
20min。
Preferably, the process conditions after being optimized using response phase method, including：Fresh rice bran is dried at a temperature of 70 DEG C
After 24h, 60 mesh are crushed to, the glycerite that concentration of volume percent is 10% are added by 30mL/g liquid ratios, in 65 DEG C of water-baths
After lower extraction 1h, centrifuged with 10000 turns/min, supernatant is collected after 15min, produce rice bran polyphenol extract solution.
Present invention also offers the rice bran polyphenol extract solution as made from the above method food or change are being prepared as additive
Application in cosmetic.
In foods and cosmetics field, G ＆ W is conventional additive, therefore as made from extraction process of the present invention
Rice bran polyphenol extract solution need not directly can be used in the production of food or cosmetics except the post processing such as solvent.
The beneficial effect that the present invention possesses：
(1) present invention carries out the extraction of rice bran polyphenol using glycerine, glycerine Nantural non-toxic, avoids using other toxic reagents
The potential safety hazard brought, in addition, glycerine is the constituent in some food or cosmetics, therefore, extraction prepared by the present invention
Liquid can be directly made an addition in these products, be advantageous to industrialization production；In addition, glycerine be advantageous to extract from rice bran it is more more
Phenol material.
(2) compared with Orthogonal Method, the present invention is using Box-Behnken Designs (BBD) center combination design model
Responds Surface Methodology, optimization knot is drawn with 3 changed factors, 3 levels and a small amount of experimental group (only 17 groups of experiments) can
Fruit, optimum yields are obtained, while extraction efficiency is improved, the discharge of energy consumption and pollutant is reduced, there is industry metaplasia
The practical significance of production.
(3) present invention is simple to operate, cost-effective, improves production efficiency, promotes food security, has preferably warp
Benefit of helping and social benefit.
Brief description of the drawings
Fig. 1 is that Extracting temperature of the present invention changes on polyphenol recovery rate influence figure.
Fig. 2 is that glycerol concentration of the present invention changes on polyphenol recovery rate influence figure.
Fig. 3 is that liquid ratio of the present invention changes on polyphenol recovery rate influence figure.
Fig. 4 is the response surface graphics that Extracting temperature of the present invention influences with glycerol concentration on polyphenol recovery rate.
Fig. 5 is the response surface X-Y scheme that Extracting temperature of the present invention influences with glycerol concentration on polyphenol recovery rate.
Fig. 6 is the response surface graphics that Extracting temperature of the present invention influences with liquid ratio on polyphenol recovery rate.
Fig. 7 is the response surface X-Y scheme that Extracting temperature of the present invention influences with liquid ratio on polyphenol recovery rate.
Fig. 8 is the response surface graphics that glycerol concentration of the present invention influences with liquid ratio on polyphenol recovery rate.
Fig. 9 is the response surface X-Y scheme that glycerol concentration of the present invention influences with liquid ratio on polyphenol recovery rate.
Embodiment
With reference to embodiment, the invention will be further described.
Experimental method used in following embodiments is conventional method unless otherwise specified.Used in embodiment
Material, reagent etc., unless otherwise specified, commercially obtain.
Rice bran is purchased from the Zhejiang market of farm produce；Drying unit is electric heating blast drier (the limited public affairs of Shanghai laboratory apparatus factory
Department)；Reducing mechanism is Portable high speed Universalpulverizer (Lin great Machinery Co., Ltd.s of Wenling city)；Constant temperature water bath apparatus is SHY-
2 water-bath constant temperature oscillators (Instrument Ltd. of Jiamei of Community of Jin Tan County city)；Centrifuge is TGL-16M table-type high-speed refrigerated centrifuges
(Hunan Xiang Yi centrifuges Instrument Ltd.)；Spectrophotometer is (the Shanghai member analysis of UV-5800PC ultraviolet-uisible spectrophotometers
Instrument Ltd.).
Embodiment 1
A kind of glycerine extracting method for being optimized rice bran polyphenol using response phase method, is comprised the following steps：
(1) sample preparation：
After fresh rice bran is dried into 24h at a temperature of 70 DEG C, crush, cross 60 mesh sieves, volume is added by 10-40mL/g liquid ratios
Concentration is 5-70% glycerite, after extracting 1-2h under 40-80 DEG C of water-bath, is centrifuged with 10000 turns/min, 15min
After collect supernatant, obtain the glycerine extract solution corresponding to various extracting conditions.
(2) Determination of Polyphenols in forint- phenol law measure extract solution
1. standard curve making：
Accurately weigh 10mg gallic acids, be configured to concentration be 0.1mg/mL solution, take respectively 0.125mL,
0.225mL, 0.325mL, 0.425mL, 0.525mL, add forint phenol reagent and the 0.5mL distillations of 0.5mL volume fractions 10%
Water, stand the Na of addition 1.25mL mass fractions 7% after 6min2CO3Solution, total solution is settled to 4mL with distilled water.Dark place
Absorbance is determined under 760nm wavelength after standing 90min, using gallic acid quality mg as abscissa, light absorption value is ordinate, is painted
Standard curve processed；
2. the measure of Determination of Polyphenols in sample：
Sample 0.125mL is taken, 1. remaining operation makes standard curve with the step identical, compares under 760nm wavelength
Color, institute's value find corresponding gallic acid equivalant on standard curve.
(3) experimental design and statistical analysis：
1. single factor experiment：
Change Extracting temperature, glycerol concentration, liquid ratio and extraction time progress single factor experiment successively, use forint- phenol law
Total polyphenols quality in measure gained rice bran polyphenol extract, and is calculated as follows total polyphenols yield, it is per treatment in triplicate；
Total polyphenols quality/rice bran powder quality × 100% in polyphenol yield (%)=sample liquid；
As Figure 1-3, Extracting temperature, glycerol concentration, liquid ratio influence more significant on the extraction effect of rice bran polyphenol.
2. response phase method optimization design：
According to single factor experiment result, fixed extraction time 90min, choosing polyphenol extraction effect influences more significant extraction
This 3 factors of temperature, glycerol concentration and liquid ratio, original is designed according to Box-Behnken using the softwares of Design Expert 8.0
Then carry out experimental design (setting result and experimental program are shown in Tables 1 and 2).
The empirical factor of table 1 and level set
Table 2Box-Behnken experimental designs and result
With Extracting temperature X1, glycerol concentration X2, liquid ratio X3For independent variable, using polyphenol yield as response y, establish polynary
Quadratic regression equation：
Y=677.37+36.23X1+27.29X2+10.62X3-40.26X1 2-25.91X2 2-31.45X3 2+22.19X1X2-
5.70X1X3+10.81X2X3。
Linear relationship conspicuousness between each factor and response, examined and judged by F values, P values are smaller, then explanatory variable
Conspicuousness is higher.From analysis of variance table (table 3), the linear relationship significantly (R between its dependent variable and all independents variable2=
0.9567), the model level of signifiance is less than 0.05, so the regression equation model is significant.
The results of analysis of variance of the experimental data of table 3
| Source | Sum of Squares | DF | Mean Square | F Value | Prob>F |
| Model | 35295.82 | 9 | 3921.76 | 40.31 | <0.0001 |
| A- Extracting temperatures | 10500.90 | 1 | 10500.90 | 107.94 | 0.0011 |
| B- glycerol concentrations | 5959.04 | 1 | 5959.04 | 61.25 | <0.0001 |
| C- liquid ratios | 902.28 | 1 | 902.28 | 9.27 | <0.0001 |
| AB | 1970.03 | 1 | 1970.03 | 20.25 | 0.4754 |
| AC | 130.07 | 1 | 130.07 | 1.34 | 0.1973 |
| BC | 467.64 | 1 | 467.64 | 4.81 | 0.0514 |
| A2 | 6823.10 | 1 | 6823.10 | 70.13 | 0.0013 |
| B2 | 2826.70 | 1 | 2826.70 | 29.06 | 0.2382 |
| C2 | 4164.71 | 1 | 4164.71 | 42.81 | <0.0001 |
| Residual | 681.01 | 7 | 97.29 | ||
| Lack of Fit | 407.14 | 3 | 135.71 | 1.98 | 0.1192 |
| Pure Error | 273.87 | 4 | 68.47 | ||
| Cor Total | 35976.83 | 16 | |||
| R2 | 0.8070 | ||||
| RAdj 2 | 0.9567 |
(4) analysis of experimental results and optimization：
Plot analysis is carried out according to polynary quadratic regression equation using the softwares of Design Expert 8.0, obtains recurrence side
The response surface and its contour map (such as Fig. 4-9) of journey.
By the softwares of Design Expert 8.0 obtain glycerine extraction rice bran polyphenol optimum extraction condition be：Liquid ratio
30mL/g, 65 DEG C of Extracting temperature, glycerol concentration 10%, the predicted value of polyphenol yield is 0.712%.
Embodiment 2
Fresh rice bran is dried into 24h at a temperature of 70 DEG C, crushed, crosses 60 mesh sieves, volumetric concentration is added by 30mL/g liquid ratios
For 10% glycerite, after extracting 1h under 65 DEG C of water-baths, centrifuged with 10000 turns/min, supernatant is collected after 15min
Liquid, produce rice bran polyphenol extract solution.
Determination of Polyphenols in extract solution is determined using forint- phenol law, polyphenol yield is 0.709%, approaches, says with predicted value
Bright optimum results are reliable.
Embodiment 3
Fresh rice bran is dried into 24h at a temperature of 80 DEG C, crushed, crosses 60 mesh sieves, volumetric concentration is added by 25mL/g liquid ratios
For 8% glycerite, after extracting 1h under 60 DEG C of water-baths, centrifuged with 10000 turns/min, supernatant collected after 15min,
Produce rice bran polyphenol extract solution.
Determination of Polyphenols in extract solution is determined using forint- phenol law, polyphenol yield is 0.643%.
Embodiment 4
Fresh rice bran is dried into 24h at a temperature of 80 DEG C, crushed, crosses 40 mesh sieves, volumetric concentration is added by 35mL/g liquid ratios
For 15% glycerite, after extracting 1h under 70 DEG C of water-baths, centrifuged with 10000 turns/min, supernatant is collected after 15min
Liquid, produce rice bran polyphenol extract solution.
Determination of Polyphenols in extract solution is determined using forint- phenol law, polyphenol yield is 0.668%.
Embodiment 5
By fresh rice bran, 24h is dried at a temperature of 80 DEG C, is crushed, crosses 60 mesh sieves, volumetric concentration is added by 28mL/g liquid ratios
For 11% glycerite, after extracting 1h under 63 DEG C of water-baths, centrifuged with 10000 turns/min, supernatant is collected after 15min
Liquid, produce rice bran polyphenol extract solution.
Determination of Polyphenols in extract solution is determined using forint- phenol law, polyphenol yield is 0.685%.
Comparative example 1
Fresh rice bran is dried into 24h at a temperature of 70 DEG C, crushed, crosses 60 mesh sieves, volumetric concentration is added by 30mL/g liquid ratios
For 10% ethanol solution, after extracting 1h under 65 DEG C of water-baths, centrifuged with 10000 turns/min, supernatant is collected after 15min
Liquid, produce rice bran polyphenol extract solution.
Determination of Polyphenols in extract solution is determined using forint- phenol law, polyphenol yield is 0.667%.With ethanol extraction method phase
Than polyphenol yield is improved about 6% by the inventive method, it was demonstrated that the inventive method is good to the extraction effect of rice bran polyphenol.
Application examples
The final purpose of present invention extraction rice bran polyphenol is exactly to use it in daily production, so as to play its biological work(
Can effect.Therefore a kind of mode of production that extract solution is directly used in food or cosmetics is proposed.
Glycerine can be directly made an addition in food or cosmetics as the important composition composition in numerous food product and cosmetics
's.Solvent step is removed this not only reduces traditional ethanol extraction method, greatlys save production cost, and meet green section
The Production trend of energy, avoids unnecessary emission.
By taking common on the market lycopene capsules and toner as an example, the general formula of lycopene capsules is tomato red
Element, soybean oil, beeswax, gelatin, G ＆ W；The general formula of toner is water, glycerine and some functional components.The present invention
Extracting the polyphenol contained by obtained glycerin extract has many physiological functions such as anti-oxidant, can strengthen above-mentioned food or cosmetic
The feature of product, attract more consumers.As can be seen here, the present invention is important life using the G ＆ W in extraction solution
Raw material is produced, possesses the possibility for being directly used in production.
The present invention lays a good foundation for the further research and integrated application of rice bran polyphenol.
Claims (9)
- A kind of 1. method for extracting rice bran polyphenol, it is characterised in that comprise the following steps：Using rice bran powder as raw material, according to 25 ~35mL/g liquid ratios add concentration of volume percent be 5~15% glycerite, in 60~70 DEG C of water-baths extract 1~ 2h, supernatant is separated and collected, produce rice bran polyphenol extract solution.
- 2. the method as described in claim 1, it is characterised in that described rice bran powder is by fresh rice bran in 70~80 DEG C of conditions After drying, it is made after being crushed to 60~80 mesh.
- 3. the method as described in claim 1, it is characterised in that described liquid ratio is 28~30mL/g.
- 4. the method as described in claim 1, it is characterised in that described glycerite is the mixture of glycerine and water.
- 5. method as claimed in claim 4, it is characterised in that the concentration of volume percent of described glycerite be 8~ 10%.
- 6. the method as described in claim 1, it is characterised in that described bath temperature is 63~65 DEG C.
- 7. method as claimed in claim 1, it is characterised in that it is described be separated into 10000~11000 turns/min centrifugation 10~ 20min。
- 8. method as claimed in claim 1, it is characterised in that the process conditions after being optimized using response phase method, including：Will be fresh Rice bran dries 24h at a temperature of 70 DEG C, is crushed to 60 mesh, and the glycerine that concentration of volume percent is 10% is added by 30mL/g liquid ratios Solution, after extracting 1h under 65 DEG C of water-baths, centrifuged with 10000 turns/min, supernatant is collected after 15min, it is more to produce rice bran Phenol extraction liquid.
- 9. the rice bran polyphenol extract solution as made from any one of claim 1-8 methods described is preparing food or change as additive Application in cosmetic.
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| CN108208506A (en) * | 2018-01-18 | 2018-06-29 | 浙江省柑桔研究所 | A kind of millet cavings beverage and preparation method thereof |
| CN108295013A (en) * | 2018-04-24 | 2018-07-20 | 南京财经大学 | A kind of rice bran facial mask and preparation method thereof |
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