CN104256635A - Method for extracting apple polyphenol by ethyl alcohol solvent with assistance of pressure ultrasound - Google Patents
Method for extracting apple polyphenol by ethyl alcohol solvent with assistance of pressure ultrasound Download PDFInfo
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- 239000002904 solvent Substances 0.000 title claims abstract description 16
- 238000002604 ultrasonography Methods 0.000 title abstract description 11
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- 239000007788 liquid Substances 0.000 claims abstract description 19
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- 230000008569 process Effects 0.000 claims description 46
- 238000000605 extraction Methods 0.000 claims description 24
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- 238000005507 spraying Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 abstract 2
- 238000002137 ultrasound extraction Methods 0.000 description 21
- 230000000694 effects Effects 0.000 description 19
- 102000030523 Catechol oxidase Human genes 0.000 description 15
- 108010031396 Catechol oxidase Proteins 0.000 description 15
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- 230000009849 deactivation Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- -1 polyphenol compounds Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
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- 238000006243 chemical reaction Methods 0.000 description 2
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- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
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- 238000010521 absorption reaction Methods 0.000 description 1
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Classifications
-
- 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
-
- 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
- A61K8/347—Phenols
-
- 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
-
- 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
-
- 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
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
Abstract
The invention discloses a method for extracting apple polyphenol by ethyl alcohol solvent with the assistance of pressure ultrasound. The method comprises the following steps: (a) selecting crushed and juiced apple residues as raw materials; (b) putting the apple residue into a pressure ultrasound device, adding 40%-80% ethyl alcohol solution in the pressure ultrasound device, wherein the weight ratio of the apple residue to the ethyl alcohol solution is 1 to (15-30), and the pH value is adjusted to be between 3.0 and 4.5; carrying out pressurization ultrasound treatment, wherein the treatment conditions are that the pressure range is 0.20-0.50MPa, the ultrasound frequency is 20KHz, the ultrasound power is 150W-250W, the total ultrasound treatment time is 9-20 minutes, and the working temperature is 55 DEG C-85 DEG C. After the selected ultrasound time is reached, a feed liquid is taken out, and is centrifuged, and then the solvent is recycled, and dried, thereby obtaining a crude apple polyphenol product.
Description
Technical field
The present invention relates to food processing field, refer in particular to a kind of method of pressure ultrasonic wave added ethonal extraction apple polyphenol.
Background technology
Apple polyphenol is the general name of contained phenolic compound in apple, and mainly comprise phenolic acid class and flavonoid class, wherein cinnamic acid derivative and flavanols account for 90% of apple polyphenol compounds.Research shows, apple polyphenol have anti-oxidant, antibacterial, scavenging free radicals, antitumor, suppress the various health care functions such as hypertension and control cardiovascular and cerebrovascular disease, be the native compound that a class has important physiologically active.In apple polyphenol extraction, there is traditional simple solvent extraction method at present, have the method that solvent extraction method combines with ultrasonic wave, microwave and supercritical liquid extraction technique etc., also have super-pressure secondary solvent to extract and the multiple methods such as liquid-phase extraction of pressurizeing.But these extractive techniques also exist such as extraction time long, the problem such as Extracting temperature is high, and equipment is loaded down with trivial details, and cause the degree of oxidation of apple polyphenol in leaching process to increase, polyphenol yield is lower.Comparatively speaking, ultrasonic assistant organic solvent extraction increases extraction efficiency owing to effectively can shorten extraction time, and the factors such as cost is low, are therefore applied widely.Ultrasonic assistant solvent extraction technology utilizes the ul-trasonic irradiation of certain frequency in extraction system, the institutional framework of large biological molecule or cell can be destroyed by effects such as the cavitation phenomenons that hyperacoustic mechanism (mainly radiation pressure and ultrasonic pressure) and sonochemistry produce, accelerate object and enter Extraction solvent, thus reach the leach extraction method shortening extraction time and save solvent.
But, the subject matter existed in existing apple polyphenol extractive technique is " polyphenol oxidase can be oxidized polyphenol; reduce the yield of polyphenol ", in view of pressure can effectively strengthen hyperacoustic cavitation effect, pressure is combined with ultrasonic wave and can effectively reduces the factors such as the activity of enzyme, and pressure and ultrasonic combination secondary solvent are extracted the yield that effectively can increase apple polyphenol.
Summary of the invention
For achieving the above object, the object of this invention is to provide a kind of method of pressure ultrasonic wave added ethonal extraction apple polyphenol, comprise the steps:
A) to smash the pomace after squeezing the juice for raw material;
B) pomace is put into pressure ultrasonic device, add 40% ~ 80% ethanolic solution that solid-liquid ratio is 1:15 ~ 30, adjusted to ph is between 3.0 ~ 4.5; Pressurize ultrasonic process, treatment conditions are: pressure limit: 0.20 ~ 0.50MPa; Supersonic frequency: 20KHz, ultrasonic power: 150W ~ 250W; Ultrasonic process total time: 9 ~ 20min; Operating temperature: 55 DEG C ~ 85 DEG C, after reaching selected ultrasonic time, take out feed liquid, centrifugal, decompression and solvent recovery, drying, obtain apple polyphenol semifinished product.
Described " ultrasonic process of pressurizeing " first applies 2-5 pressure to extract at normal temperatures, under packing state, carry out ultrasonic process again.Greatly can shorten extraction time (generally within 15 minutes) by pressurization and ultrasonic combination, recovery rate is high, owing to being extract under closed environment, greatly reduces the volatilization of ethanolic solution, saves solvent load; In leaching process, solvent not easily evaporate in surrounding environment, and environmental pollution is little.
On the other hand, pressure strengthens and can improve the flux and speed that solvent permeates histocyte significantly, causes the quantity of solvent penetrating into cell interior to increase, has more active ingredient simultaneously and be dissolved in solvent, the recovery rate of active ingredient is improved.The raising of speed can make process of osmosis required time shorten, and shortens extraction time significantly.In ultrasonic field due in the residing Extraction medium such as the thing that is broken containing a large amount of dissolved gases and small impurity, when there being higher pressure in environment, the cavitation phenomenon of ultrasonic generation is strengthened greatly, and the release diffusion of intracellular organic matter and rate of dissolution are strengthened.Pressure is combined the activity that effectively can reduce enzyme with ultrasonic wave.Therefore, pressurization and combination of ultrasound improve broken speed, shorten the broken time, reduce the activity of polyphenol oxidase, greatly improve the extraction efficiency of apple polyphenol.
Preferably, step b) described in solid-liquid ratio be 1:25, volumes of aqueous ethanol ratio is 60%, pH value is between 3.0 ~ 4.5, and pressure is 0.4MPa, supersonic frequency: 20KHz, ultrasonic power: 200W, ultrasonic process total time: 18min, operating temperature: 70 DEG C.
Preferably, step b) described in solid-liquid ratio be 1:30, volumes of aqueous ethanol ratio is 40%, and pH value is between 3.0 ~ 4.5, and pressure is 0.4MPa, supersonic frequency: 20KHz, ultrasonic power: 250W, ultrasonic process total time: 9min, operating temperature: 70 DEG C.
Preferably, step b) described in solid-liquid ratio be 1:25, volumes of aqueous ethanol ratio is 60%, pH value is between 3.0 ~ 4.5, and pressure is 0.3MPa, supersonic frequency: 20KHz, ultrasonic power: 200W, ultrasonic process total time: 15min, operating temperature: 70 DEG C.
Preferably, step b) described in drying mode be spraying dry or drying under reduced pressure.
By method of the present invention, available apple polyphenol semifinished product.Described apple polyphenol semifinished product can be used for preparing in food additives, health food or cosmetics.
On the other hand, the invention provides the apple polyphenol semifinished product obtained through the inventive method, the water content wherein as the pomace of raw material is 75% ~ 80% (by quality ratio).
The present invention is owing to taking above technical scheme, and it has the following advantages:
1. in leaching process the activity of polyphenol oxidase reduce faster, pressure is combined with ultrasonic wave and shortens polyphenol oxidase
The active time arrived required for minimum.
2. effectively increase the yield of apple polyphenol, pressurization ultrasonic assistant ethanolic solution extractive technique improves apple polyphenol yield 7.0% ~ 15.0% than normal ultrasound waves Assisted Ethanol solution extractive technique.
3., compared with Microwave Extraction, Extraction medium does not have particular/special requirement (microwave requires that the necessary dielectric constant of extractant is less, microwave absorption capacity is relatively poor).
4. and CO
2supercritical fluid extraction is compared, and extract can be lipid small-molecule substance also can be soluble small molecular material; Equipment is simple, and do not need too loaded down with trivial details operation, extraction cost is low.
In sum, pressure and combination of ultrasound, be combined with the advantage of the two.The suitable rising of pressure strengthens ultrasonic cavitation phenomenon, causes plant cell wall and even whole organism is broken instantaneously, and the effect of vibration that ultrasonic wave produces simultaneously strengthens the release diffusion of intracellular organic matter and dissolves.Shorten extraction time, improve recovery rate, effectively improve economic benefit.Pressure raises and the polymer substance (as protein, enzyme etc.) combined primarily of non-covalent bond (hydrogen bond, ionic bond, hydrophobic bond) also can be caused to change, and on the small-molecule substance combined primarily of covalent bond form (as vitamin, pigment, flavor component, alkaloid, saponin, flavone compound etc.) not impact.Therefore, in the process extracting apple polyphenol, certain reduction active function is served on the polyphenol oxidase affecting recovery rate.The pressure that pressure ultrasound assisted extraction technique adopts is not too high (≤0.5MPa), so equipment requirement is low, device fabrication cost is lower than high pressure extraction equipment.Pressure ultrasound assisted extraction technique carries out ultrasound works in enclosed high pressure environment, greatly reduces the volatilization of ethanolic solution, saves solvent load, reduces financial cost; In addition in leaching process, solvent can not evaporate in surrounding environment, meets the requirement of " green " environmental protection.Therefore, applying pressure ultrasound assisted extraction technique extracts effective components in plants and has very high practical value, and overall economic efficiency is remarkable, is the new technology having development potentiality and competitiveness.Extraction rate is fast, with short production cycle.
Detailed description of the invention
Mode by the following examples further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, conventionally selects with condition.
Embodiment 1
Apple polyphenol assay in the present invention adopts Forint phenol method (FC method).Get apple polyphenol extract 2mL, after adding forint phenol 1ml, mixing leaves standstill 3 to 4 minutes, adds the Na of 10%
2cO
31ml, 25 DEG C of lucifuge water-baths 2 hours, using spectrophotometer to measure absorbance under 765nm, take distilled water as blank.According to gallic acid calibration curve equation, the yield of measuring and calculating apple polyphenol.
Embodiment 2
The activity determination method of the apple polyphenol oxidase in the present invention is as follows: in the reaction system of 2ml citric acid solution (pH=3.00) and the solution composition of 0.5ml 0.1mol/L catechol, add apple polyphenol extract 2mL to mix rapidly, take reagent as blank, with the crude enzyme liquid of heat inactivation (100 DEG C of heating 1min) for contrast, survey absorbance (OD value) in wavelength 420nm place.In 1min, every 15s records an OD and is worth over time, represents enzyme activity with the slope of initial straightway (△ OD/t).An enzyme activity unit (U) is defined as: under condition determination, and the absorbance that causes per minute changes enzyme amount needed for 0.001.
Pomace in the present invention is the fresh pomace that apple obtains after juice extractor is squeezed the juice, and adopts atmosphere pressure desiccation to measure moisture.
Embodiment 3
By red fuji apple slag, be placed in the ultrasonic extraction still of pressure, add 60% ethanolic solution of solid-liquid ratio 1:25, adjust ph, between 3.0 ~ 4.5, boosts to 0.4MPa, carries out ultrasonic extraction.Supersonic frequency: 20KHz, ultrasonic power 200W, ultrasonic process total time 18min, operating temperature: 70 DEG C.
Check experiment: above-mentioned process conditions are not pressurizeed and directly used ultrasonic process, carry out check experiment, measures the relative activity of polyphenol recovery rate and enzyme.
Obtain after measured, the apple polyphenol recovery rate obtained without the ultrasonic process of pressurization is 0.374g/kg, and the apple polyphenol recovery rate obtained through ultrasonic extraction of pressurizeing is 0.404g/kg.Compared with visible and direct ultrasonic extraction, the ultrasonic process apple polyphenol recovery rate that pressurizes improves 8.02%
Obtain after measured, after the ultrasonic process 5min of pressurization, the relative activity of polyphenol oxidase is 25%, and after the ultrasonic process 5min that pressurizes, the relative activity of polyphenol oxidase is 9.38%.Compared with visible and direct ultrasonic extraction, ultrasonic process of pressurizeing can make the deactivation rate of apple polyphenol oxidase accelerate.
Embodiment 4,
By red fuji apple slag, be placed in the ultrasonic extraction still of pressure, 40% ethanolic solution adding solid-liquid ratio 1:30 boosts to 0.4MPa, carries out ultrasonic extraction.Ultrasonic power 250W, ultrasonic process total time 9min, other conditions are identical with embodiment 3.
Check experiment: above-mentioned process conditions are not pressurizeed and directly used ultrasonic process, carry out check experiment, measures the relative activity of polyphenol recovery rate and enzyme.
Obtain after measured, the apple polyphenol recovery rate obtained without the ultrasonic process of pressurization is 0.342g/kg, and the apple polyphenol recovery rate obtained through ultrasonic extraction of pressurizeing is 0.394g/kg.Compared with visible and direct ultrasonic extraction, the ultrasonic process apple polyphenol recovery rate that pressurizes improves 15.2%.
Obtain after measured, after the ultrasonic process 5min of pressurization, the relative activity of polyphenol oxidase is 24.8%, and after the ultrasonic process 5min that pressurizes, the relative activity of polyphenol oxidase is 9.51%.Compared with visible and direct ultrasonic extraction, ultrasonic process of pressurizeing can make the deactivation rate of apple polyphenol oxidase accelerate.
Embodiment 5,
By red fuji apple slag, be placed in the ultrasonic extraction still of pressure, 60% ethanolic solution adding solid-liquid ratio 1:25 boosts to 0.3MPa, carries out ultrasonic extraction.Ultrasonic power 200W, ultrasonic process total time 15min, other conditions are identical with embodiment 3.
Check experiment: above-mentioned process conditions are not pressurizeed and directly used ultrasonic process, carry out check experiment, measures the relative activity of polyphenol recovery rate and enzyme.
Obtain after measured, the apple polyphenol recovery rate obtained without the ultrasonic process of pressurization is 0.343g/kg, and the apple polyphenol recovery rate obtained through ultrasonic extraction of pressurizeing is 0.373g/kg.Compared with visible and direct ultrasonic extraction, the ultrasonic process apple polyphenol recovery rate that pressurizes improves 8.75%
Obtain after measured, after the ultrasonic process 5min of pressurization, the relative activity of polyphenol oxidase is 25%, and after the ultrasonic process 5min that pressurizes, the relative activity of polyphenol oxidase is 9.41%.Compared with visible and direct ultrasonic extraction, ultrasonic process of pressurizeing can make the deactivation rate of apple polyphenol oxidase accelerate.
Table 1 is at solid-liquid ratio 1:25,60% ethanolic solution, boost to 0.4MPa, ultrasonic power 200W, under the experiment condition of ultrasonic process total time 18min, the apple polyphenol recovery rate obtained without the ultrasonic process of pressurization is 0.374g/kg, and the apple polyphenol recovery rate obtained through ultrasonic extraction of pressurizeing is 0.404g/kg.Compared with direct ultrasonic extraction, the ultrasonic process apple polyphenol recovery rate that pressurizes improves 8.02%.
Due to this experiment employing is fresh pomace, through measuring and calculating water content be 80%, the weight being converted into dry pomace is about 4 ~ 5 times of wet slag, the apple polyphenol recovery rate obtained without the ultrasonic process of pressurization through conversion is 1.87mg/g, and the apple polyphenol recovery rate obtained through ultrasonic extraction of pressurizeing is 2.02mg/g.
Table 1 pressurizes ultrasonic assistant alcohol extract apple polyphenol
Treatment conditions: liquid ratio 25:1, concentration of alcohol 60%, adjust ph is between 3.0 ~ 4.5, supersonic frequency: 20KHz, ultrasonic power 200W, extraction time 15min, moulding pressure 0,0.2,0.3,0.4,0.5,0.6,0.7,0.8MPa, operating temperature: 70 DEG C.
Table 2 pressurizes ultrasonic assistant alcohol extract apple polyphenol
Treatment conditions: solid-liquid ratio 1:25, volume fraction of ethanol 60%, adjust ph is between 3.0 ~ 4.5, supersonic frequency: 20KHz, ultrasonic power 200W, ultrasonic time 0,3,6,9,12,15,18,21min, pressure 0.1/0.4MPa, operating temperature 70 DEG C.
Although above-mentioned, the specific embodiment of the present invention is described; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (10)
1. a method for pressure ultrasonic wave added ethonal extraction apple polyphenol, is characterized in that, comprise the steps:
A) to smash the pomace after squeezing the juice for raw material;
B) pomace is put into pressure ultrasonic device, add 40% ~ 80% ethanolic solution that solid-liquid ratio is 1:15 ~ 30, adjusted to ph is between 3.0 ~ 4.5; Pressurize ultrasonic process, treatment conditions are: pressure limit: 0.20 ~ 0.50MPa; Supersonic frequency: 20KHz, ultrasonic power: 150W ~ 250W; Ultrasonic process total time: 9 ~ 20min; Operating temperature: 55 DEG C ~ 85 DEG C; After reaching selected ultrasonic time, take out feed liquid, centrifugal, decompression and solvent recovery, drying, obtain apple polyphenol semifinished product.
2. the method for claim 1, it is characterized in that, step b) described in solid-liquid ratio be 1:25, volumes of aqueous ethanol ratio is 60%, and pH value is between 3.0 ~ 4.5, and pressure is 0.4MPa, supersonic frequency: 20KHz, ultrasonic power: 200W, ultrasonic process total time: 18min, operating temperature: 70 DEG C.
3. the method for claim 1, it is characterized in that, step b) described in solid-liquid ratio be 1:30, volumes of aqueous ethanol ratio is 40%, and pH value is between 3.0 ~ 4.5, and pressure is 0.4MPa, supersonic frequency: 20KHz, ultrasonic power: 250W, ultrasonic process total time: 9min, operating temperature: 70 DEG C.
4. the method for claim 1, it is characterized in that, step b) described in solid-liquid ratio be 1:25, volumes of aqueous ethanol ratio is 60%, and pH value is between 3.0 ~ 4.5, and pressure is 0.3MPa, supersonic frequency: 20KHz, ultrasonic power: 200W, ultrasonic process total time: 15min, operating temperature: 70 DEG C.
5. the method for claim 1, is characterized in that, step b) described in drying mode be spraying dry or drying under reduced pressure.
6. by the apple polyphenol semifinished product that the arbitrary described method of claim 1-5 is obtained.
7. apple polyphenol semifinished product as claimed in claim 6, it is characterized in that, the water content of described pomace is 75% ~ 80%.
8. the application in food additives prepared by apple polyphenol semifinished product according to claim 6.
9. the application in health food prepared by apple polyphenol semifinished product according to claim 6.
10. the application in cosmetics prepared by apple polyphenol semifinished product according to claim 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410432549.8A CN104256635B (en) | 2014-08-28 | 2014-08-28 | A kind of method of pressure ultrasonic wave added ethonal extraction apple polyphenol |
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| CN114486415A (en) * | 2021-12-23 | 2022-05-13 | 广东贝源检测技术股份有限公司 | Method for extracting petroleum hydrocarbon in soil |
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| CN104622757A (en) * | 2015-02-11 | 2015-05-20 | 广州赛莱拉干细胞科技股份有限公司 | Extraction method and application of apple fruit cell extract |
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| CN104886577A (en) * | 2015-06-16 | 2015-09-09 | 福建省农业科学院农业工程技术研究所 | Preparation method of prunus fruit polyphenol |
| CN104886577B (en) * | 2015-06-16 | 2017-03-15 | 福建省农业科学院农业工程技术研究所 | A kind of preparation method of Lee fruit polyphenol |
| CN110521889A (en) * | 2019-09-10 | 2019-12-03 | 西北农林科技大学 | A kind of composite fruit juice and preparation method thereof with Weight-reducing and lipid-lowering |
| CN110521889B (en) * | 2019-09-10 | 2022-05-17 | 西北农林科技大学 | Compound fruit juice with auxiliary weight-losing and lipid-lowering effects and preparation method thereof |
| CN114486415A (en) * | 2021-12-23 | 2022-05-13 | 广东贝源检测技术股份有限公司 | Method for extracting petroleum hydrocarbon in soil |
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