CN107362080A - A kind of extracting method of polyphenol in passion fruit pericarp - Google Patents

A kind of extracting method of polyphenol in passion fruit pericarp Download PDF

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CN107362080A
CN107362080A CN201710585096.6A CN201710585096A CN107362080A CN 107362080 A CN107362080 A CN 107362080A CN 201710585096 A CN201710585096 A CN 201710585096A CN 107362080 A CN107362080 A CN 107362080A
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polyphenol
passion fruit
macroreticular resin
fruit pericarp
pericarp
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CN107362080B (en
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刘慧敏
王伟
魏继文
刘清雷
吴健
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Shanghai Chuangyuan Cosmetics Co ltd
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Shanghai Institute of Technology
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
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    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
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    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/82Preparation or application process involves sonication or ultrasonication
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

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Abstract

The present invention discloses a kind of extracting method of the polyphenol in passion fruit pericarp, first by the freeze-drying of passion fruit pericarp, crushes;Then using 30% 80% ethanol as solution, and it is 200 400W in ultrasonic power, temperature carries out ultrasonic wave ethanol collaboration 5 35min of extraction under conditions of 30 70 DEG C, then filtered with 0.45 μm 0.80 μm of nylon filter, concentration;Concentrate is isolated and purified with the 1.25mm of particle diameter 0.30 macroreticular resin, vacuum freeze drying obtains the polyphenol powder in passion fruit pericarp.The extracting method cooperates with the combination of the technologies such as extraction, macroreticular resin separating-purifying and vacuum freeze drying by ultrasonic ethanol, ensure that the recovery rate and purity of polyphenol.The recovery rate of polyphenol in the passion fruit pericarp of final gained can reach 33.95 50.35%.The present invention is a kind of the effective using new method is provided of passion fruit pericarp, can be turned waste into wealth.

Description

A kind of extracting method of polyphenol in passion fruit pericarp
Technical field
The present invention relates to extracted form natural plant technical field, and in particular to a kind of extraction side of the polyphenol in passion fruit pericarp Method.
Background technology
Plant polyphenol is the complicated phenols secondary metabolites in plant, has polyhydric phenols structure, is primarily present in plant Skin, root, leaf, in fruit, the content in plant is only second to cellulose, hemicellulose and lignin.Class in polyphenol substance is yellow Ketone is antioxidant.Medical research finds that polyphenols plays an important role in human disease treatment and health protection, has There are a variety of physiology work(such as the cardiovascular and cerebrovascular diseases such as antitumor, anti-oxidant, anti arteriosclerosis, prevention and treatment of coronary heart disease and apoplexy and antibacterial Can, it is nature and the mankind " healthy bodyguard ".Since the late 1980s, both at home and abroad from multiple fields, multiple angle Degree has carried out basic research and application study to plant polyphenol.At present Tea Polyphenols, Punica granatum L. polyphenol, vine polyphenol extractive technique Through very ripe, and the polyphenol extracted has been applied to food, cosmetics and field of medicaments.
Passion fruit (passion fruit), is the herbaceous species plant of Passifloraceae Passiflora, also known as passion fruit, heat Feelings fruit, it is a kind of tropical fruit (tree), pulp is orange, seed edible;Mainly there are purple fruit and the major class of yellow fruit two.Passion fruit is because with super Cross the strong fragrance of 165 kinds of aromatic substances and 10 various fruits and well-known, enjoy the good reputation of " king of beverage " and " beverage essence ". Research finds that the composition beneficial to human body, wherein pectin, polysaccharide, Flavonoid substances, vitamin are all contained in each position of passion fruit Class content is the abundantest, while the mineral matter isoreactivity composition also containing kind more than 10, contains huge Development volue.Fruit juice can Natural quality beverage, fruit dew, jam, jelly, preserved fruit are processed into, not only unique flavor, nutritious, and healthcare, Help digest, supply falls short of demand in market.Seed oil content is up to 25%, and oil can match in excellence or beauty with sunflower oil, suitable for making edible oil;Pericarp carries The pectin taken is the good stabilizer and thickener of food processing;Root, stem, leaf can be used as medicine, have anti-inflammatory analgetic, promoting blood circulation, The curative effects such as blood fat-reducing blood pressure-decreasing;The essence of extraction is the good additive of dessert and drinks.Up to the present, passion fruit is to find to contain The most edible plants of polyphenol substance.More than 90% polyphenol is present in skin and core in document report passion fruit fruit, and Accessory substance of the passion fruit pericarp as passion fruit, the 40%-55% of gross mass is accounted for, wherein polyphenol content accounts for the quality percentage of pericarp Than for 0.28-0.55%, the pollution for causing environment causes the waste of resource again.At present for pericarp polyphenol in passion fruit The research of extraction process or vacancy.
In recent years, research of the passion fruit in nutrition, area of pharmacology has obtained many scientific achievements, and in extraction work Research in terms of skill optimization is mainly the extraction of pectin, seed oil, and the method and technique of the extraction to passion fruit polyphenols are ground Study carefully seldom, and the extraction research to passion fruit pericarp polyphenol yet there are no report, therefore necessary develop new technology Polyphenols polyphenoils is extracted from discarded passion fruit pericarp, strengthens the comprehensive utilization of passion fruit pericarp, turns waste into wealth, carries High added value.
The content of the invention
It is an object of the invention to provide a kind of extracting method of polyphenol in passion fruit pericarp, the extracting method has operation letter Just, extraction efficiency is high, can strengthen the comprehensive utilization of passion fruit pericarp, turn waste into wealth, improves added value.
Technical scheme:
A kind of extracting method of polyphenol in passion fruit pericarp, i.e., extraction is assisted to obtain passion fruit fruit with ultrasonic wave-ethanol Skin polyphenol crude product, is then separated by macroreticular resin, and the polyphenol in passion fruit pericarp is obtained after drying.
Finally determine that the optimum condition isolated and purified is:Select DM-301 macroreticular resins, adsorption rate 78.89%, desorption Rate is 98.95%;The ethanol that concentration is 90%v/v is strippant elution.
Its extraction process specifically includes following steps:
(1), pre-process
Passion fruit pericarp is cleaned, dried, then with vacuum freeze drier drying process, is then crushed passion fruit pericarp It is 60-200 targeted fine powders, preferably 60 mesh to granularity, obtains passion fruit fruit peel powder;
(2), ultrasound-ethanol collaboration processing
By passion fruit fruit peel powder:The ethanol water that concentration of volume percent is 30-80% is 1g:20-50ml ratio, Passion fruit fruit peel powder obtained by step (1) is added in the ethanol water that concentration of volume percent is 30-80%, stirring is equal After even, to control frequency be 30-40KHz, power 200-400W, temperature are 30-70 DEG C and carry out supersound process 5-35min, preferably It is 30 DEG C for 40KHz, power 350W, temperature and carries out supersound process 25min, obtains ultrasonication liquid;
(3), filter
After the static placement of ultrasonication liquid obtained by step (2), supernatant is taken, with 0.45 μm -0.80 μm, preferably 0.45 μm of nylon filter filtering, obtains crude extract;
(4), concentrate
The crude extract obtained by step (3) is concentrated under conditions of to control temperature be 20-25 DEG C with Rotary Evaporators thick The 1/20-1/15 of extracting liquid volume, obtain concentrate;
(5), separation absorption
Calculate by volume, i.e. concentrate obtained by step (4):Deionized water is 1g:20-30ml ratio, to step (4) deionized water is added in the concentrate obtained by, stirs to concentrate and is completely dissolved in deionized water, it is water-soluble to obtain concentrate Liquid;
The macroreticular resin solid for adding that particle diameter is 0.30-1.25mm in the concentrate aqueous solution of gained is stated then up, is put It is placed in constant-temperature table, polyphenol absorption 2-4h is carried out under conditions of it is 25-45 DEG C to control temperature, rotating speed is 100-180rpm, is obtained To the macroreticular resin of adsorbing polyphenols, then filtering, the macroreticular resin of deionized water cleaning adsorbing polyphenols 3-5 times controls the temperature to be 20-30 DEG C is dried, and obtains the macroreticular resin of dry adsorbing polyphenols;
The macroreticular resin solid that described particle diameter is 0.30-1.25mm is AB-8, HP-20, FPX-66, SP-850, DM- 301 or XAD-2, preferably DM-301 or AB-8, its addition, by the macroreticular resin solid that particle diameter is 0.30-1.25mm:Concentrate The aqueous solution is 1g:20-30ml ratio calculates;
(6), separation desorption
By the macroreticular resin of dry adsorbing polyphenols:The ethanol water that concentration of volume percent is 80-90% is 1g: 20-30ml ratio is calculated, and concentration of volume percent is added into the macroreticular resin of the adsorbing polyphenols of the drying obtained by step (5) For 80-90% ethanol water, it is then placed into constant-temperature table, to control temperature be 25-45 DEG C, rotating speed 100-180rpm Under conditions of carry out desorption 1-2h, be filtered to remove macroreticular resin, obtain polyphenol stripping liquid;
(7) the polyphenol stripping liquid obtained by step (6), is concentrated into the 1/20- of polyphenol stripping liquid volume with Rotary Evaporators 1/15, it is to be freeze-dried at -50--60 DEG C then to control temperature, obtains the polyphenol powder in passion fruit pericarp.
Polyphenol powder in the passion fruit pericarp of above-mentioned gained, the content of polyphenol are calculated by every gram of passion fruit pericarp, and it contains Some polyphenol reach as high as 14.06mg, can be added to as functional components in cosmetics and play it and remove free radical, anti-ageing Old purposes.
The advantageous effects of the present invention
The extracting method of polyphenol in a kind of passion fruit pericarp of the present invention, due to being made using ultrasound-ethanol collaboration extraction With the polyphenol in extraction passion fruit, pericarp garbage utilization rate is substantially increased, the extraction rate reached of polyphenol in final passion fruit pericarp 33.95-50.35%, the extracted amount of passion fruit polyphenol reach 9.87-14.06mg/g.
Further, the extracting method of the polyphenol in a kind of passion fruit pericarp of the invention, utilizes ultrasonic wave due to during Cavitation realize ethanol localized hyperthermia, high pressure, along with ultrasonic wave mechanical disturbance act on, so as to accelerate passion fruit fruit Skin polyphenol crude extract, to the speed of sovent diffusion, shortens extraction time from passion fruit fruit peel powder.Therefore the extraction side of the present invention Method has the time short, and energy consumption is low, and medicinal raw material treating capacity is big, and extraction active material is not destroyed;It is green, reduce environment The features such as pollution, there is good commercial introduction to be worth.
Further, the extracting method of the polyphenol in a kind of passion fruit pericarp of the invention, the passion fruit polyphenol of gained slightly carry Liquid is taken to can reach 78.01% to the clearance rate of DPPH free radicals;To ABTS+The clearance rate of free radical can reach 95.68%, therefore the passion fruit pericarp polyphenol extract solution of gained can be applied to food, cosmetics as functional additive In, play it and remove free radical, anti-aging purposes.Because adsorption process uses physical method to make polyphenol absorption in macroreticular resin In, the impurity such as plant polyose, albumen are effectively removed, significantly improve the yield and antioxidation activity of polyphenol, and are isolated and purified into This is low;Macroreticular resin desorption efficiency reaches 98.95%.
Further, the extracting method of the polyphenol in a kind of passion fruit pericarp of the invention, due to using cheap passion fruit Pericarp is that raw material extracts Polyphenols polyphenoils, passion fruit pericarp has been obtained effective comprehensive utilization, turns waste into wealth, improves The added value of passion fruit pericarp, for increasing peasant income provides a kind of new approach.
In summary, the extracting method of the polyphenol in a kind of passion fruit pericarp of the invention, carried by ultrasound-ethanol collaboration Take, the combination of technology such as macroreticular resin separating-purifying and vacuum freeze drying, the recovery rate and purity that ensure that polyphenol, have and carry Take the time short, the advantages of polyphenol recovery rate is high, and polyphenol inoxidizability is strong, before being had a wide range of applications in foods and cosmetics Scape.
Brief description of the drawings
Fig. 1, embodiment 1-3, the comparative examples 1 of embodiment 3, the step of the extraction process of the comparative examples 2 of embodiment 3 Suddenly the crude extract obtained by (3) is respectively to the clearance rate situation of DPPH free radicals;
Fig. 2, embodiment 1-3, the comparative examples 1 of embodiment 3, the step of the extraction process of the comparative examples 2 of embodiment 3 Suddenly the crude extract obtained by (3) is respectively to ABTS+The clearance rate situation of free radical.
Embodiment
With reference to specific embodiment, the present invention will be further described, but is not intended to limit the present invention.
The content of polyphenol in various embodiments of the present invention in the passion fruit pericarp of gained is:
W=CVN/1000M
In formula:W:Polyphenol content mg/g;C:Gallic acid concentration mg/l;V:Extracting liquid volume ml;N:Extension rate;
M:Sampling amount g;
Gained
In formula:m1:Extract the quality of obtained passion fruit pericarp polyphenol;m2:The quality of passion fruit pericarp polyphenol in raw material.
Polyphenol content is determined by Folin-Ciocalteu methods in passion fruit pericarp, reference literature Juliane Vigan ó (Food Research International 85:51-58,2016,Brazil).Method is as follows:Prepare liquid is diluted 100 times Afterwards, 1.0ml dilutions are accurately pipetted into 10ml colorimetric cylinders, 1.0ml Folin-Ciocalteu reagents is added, is mixed; In 0.5min~2min, the sodium carbonate liquors of 1.5ml 10% are separately added into, are vibrated, with deionized water constant volume.Above-mentioned standard is molten Liquid 25 DEG C place 1.5h after, with ultraviolet specrophotometer (Alpha-1860S, Shanghai spectral element) in wavelength be 765nm place measure Light absorption value.Corresponding gallic acid concentration is calculated from gallic acid standard curve, polyphenol content is calculated by above-mentioned formula.
The adsorption rate of macroreticular resin, the measure of desorption efficiency in various embodiments of the present invention, reference literature Lisha Xi (Food Chemistry172:166-174,2015,China).Method is as follows, accurately weighs wet resin (the filter paper suction by pretreatment It is dry) each M g, it is placed in 100ml tool plug ground triangular flasks, it is C to add total phenol concentration0Extraction filtered fluid V ml, in a constant temperature The lower Static Adsorption 2-4h of degree, makes up to adsorption equilibrium.Resin is filtered out, residue is more in Folin-Ciocalteu methods measure solution Phenol concentration Ce;Vibrate the resin that polyphenol has been adsorbed in elution, Folin-Ciocalteu methods at a certain temperature with appropriate eluant, eluent Determine total phenol concentration in stripping liquid.Adsorption rate, desorption efficiency are calculated according to the following formula.
C in formula0:The initial concentration (mg/ml) of total polyphenols;Ce:Total polyphenols concentration (mg/ml) during adsorption equilibrium;VA:Absorption Volume (ml);A:Adsorption rate (%);D:Desorption efficiency (%);CD:Total polyphenols concentration (mg/ml) in desorbed solution;VD:Stripping liquid volume (ml)。
Embodiment 1
A kind of extracting method of polyphenol in passion fruit pericarp, specifically includes following steps:
(1), pre-process
Passion fruit pericarp is cleaned, dried, then with vacuum freeze drier drying process, is then crushed passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), ultrasound-ethanol collaboration processing
By passion fruit fruit peel powder:The ethanol water that concentration of volume percent is 80% is 1g:50ml ratio, by step (1) the passion fruit fruit peel powder obtained by is added in the ethanol water that concentration of volume percent is 80%, after stirring, control Frequency is 40KHz, power 200W, temperature are 70 DEG C and carry out supersound process 5min, obtains ultrasonication liquid;
(3), filter
After the static placement of ultrasonication liquid obtained by step (2), supernatant is taken, with 0.45 μm of nylon filter mistake Filter, obtains crude extract;
(4), concentrate
With Rotary Evaporators by the crude extract obtained by step (3) control temperature be 20 DEG C under conditions of be concentrated into coarse extraction The 1/20 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. concentrate obtained by step (4):Deionized water is 1:25 ratio, to obtained by step (4) Concentrate in add deionized water, stir to concentrate and be completely dissolved in deionized water, obtain the concentrate aqueous solution;
The HP-20 macroreticular resin solids for adding that particle diameter is 0.30mm in the concentrate aqueous solution of gained are stated then up, are put It is placed in constant-temperature table, polyphenol absorption 4h is carried out under conditions of it is 25 DEG C to control temperature, rotating speed is 180rpm, obtains adsorbing polyphenols Macroreticular resin, filtering, the macroreticular resin 3 times of deionized water cleaning adsorbing polyphenols, then control temperature to be 30 DEG C and is dried, Obtain the macroreticular resin of dry adsorbing polyphenols;
Described particle diameter is the addition of 0.30-1.25mm HP-20 macroreticular resin solids, is 0.30- by particle diameter 1.25mm HP-20 macroreticular resin solids:The concentrate aqueous solution is 1g:25ml ratio calculates;
Macroreticular resin HP-20 adsorption rate is determined to 68.63%;
(6), separation desorption
By the macroreticular resin of dry adsorbing polyphenols:The ethanol water that concentration of volume percent is 90% is 1g:25ml Ratio calculate, into the macroreticular resin of the adsorbing polyphenols of the drying obtained by step (5) add concentration of volume percent be 90% Ethanol water, be then placed into constant-temperature table, to control temperature be 25 DEG C, rotating speed is desorbed under conditions of being 180rpm 2h, macroreticular resin is filtered to remove, obtains polyphenol stripping liquid;
Macroreticular resin HP-20 desorption efficiency is determined to 90.51%;
(7) the polyphenol stripping liquid obtained by step (6), is concentrated into the 1/20 of polyphenol stripping liquid volume with Rotary Evaporators, Then it is to be freeze-dried at -60 DEG C to control temperature, obtains the polyphenol powder in passion fruit pericarp.
After testing, the wherein cubage of polyphenol is 9.87mg/g to polyphenol powder in the passion fruit pericarp of above-mentioned gained, The recovery rate of polyphenol powder in passion fruit pericarp is 33.95%.
Embodiment 2
A kind of extracting method of polyphenol in passion fruit pericarp, specifically includes following steps:
(1), pre-process
Passion fruit pericarp is cleaned, dried, then with vacuum freeze drier drying process, is then crushed passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), ultrasound-ethanol collaboration processing
By passion fruit fruit peel powder:The ethanol water that concentration of volume percent is 55% is 1g:50ml ratio, by step (1) the passion fruit fruit peel powder obtained by is added in the ethanol water that concentration of volume percent is 55%, after stirring, control Frequency is 40KHz, power 350W, temperature are 30 DEG C and carry out supersound process 25min, obtains ultrasonication liquid;
(3), filter
After the static placement of ultrasonication liquid obtained by step (2), supernatant is taken, with 0.45 μm of nylon filter mistake Filter, obtains crude extract;
(4), concentrate
With Rotary Evaporators by the crude extract obtained by step (3) control temperature be 25 DEG C under conditions of be concentrated into coarse extraction The 1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. concentrate obtained by step (4):Deionized water is 1:30 ratio, to obtained by step (4) Concentrate in add deionized water, stir to concentrate and be completely dissolved in deionized water, obtain the concentrate aqueous solution;
The DM-301 macroreticular resin solids for adding that particle diameter is 0.30mm in the concentrate aqueous solution of gained are stated then up, are put It is placed in constant-temperature table, polyphenol absorption 4h is carried out under conditions of it is 25 DEG C to control temperature, rotating speed is 180rpm, obtains adsorbing polyphenols Macroreticular resin, filtering, the macroreticular resin 3 times of deionized water cleaning adsorbing polyphenols, then control temperature to be 30 DEG C and is dried, Obtain the macroreticular resin of dry adsorbing polyphenols;
Described particle diameter is the addition of 0.30-1.25mm DM-301 macroreticular resin solids, is 0.30- by particle diameter 1.25mm DM-301 macroreticular resin solids:The concentrate aqueous solution is 1g:30ml ratio calculates;
Macroreticular resin DM-301 adsorption rate is determined to 78.89%;
(6), separation desorption
By the macroreticular resin of dry adsorbing polyphenols:The ethanol water that concentration of volume percent is 80% is 1g:30ml Ratio calculate, into the macroreticular resin of the adsorbing polyphenols of the drying obtained by step (5) add concentration of volume percent be 80% Ethanol water, be then placed into constant-temperature table, to control temperature be 25 DEG C, rotating speed is desorbed under conditions of being 180rpm 2h, macroreticular resin is filtered to remove, obtains polyphenol stripping liquid;
Macroreticular resin DM-301 desorption efficiency is determined to 98.95%;
(7) the polyphenol stripping liquid obtained by step (6), is concentrated into the 1/15 of polyphenol stripping liquid volume with Rotary Evaporators, Then it is to be freeze-dried at -60 DEG C to control temperature, obtains the polyphenol powder in passion fruit pericarp.
After testing, the cubage of wherein polyphenol obtains 14.06mg/g to polyphenol powder in the passion fruit pericarp of above-mentioned gained, The recovery rate of polyphenol powder in passion fruit pericarp is 50.35%.
Embodiment 3
A kind of extracting method of polyphenol in passion fruit pericarp, specifically includes following steps:
(1), pre-process
Passion fruit pericarp is cleaned, dried, then with vacuum freeze drier drying process, is then crushed passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), ultrasound-ethanol collaboration processing
By passion fruit fruit peel powder:The ethanol water that concentration of volume percent is 30% is 1g:50ml ratio, by step (1) the passion fruit fruit peel powder obtained by is added in the ethanol water that concentration of volume percent is 30%, after stirring, control Frequency is 40KHz, power 350W, temperature are 55 DEG C and carry out supersound process 5min, obtains ultrasonication liquid;
(3), filter
After the static placement of ultrasonication liquid obtained by step (2), supernatant is taken, with 0.45 μm of nylon filter mistake Filter, obtains crude extract;
(4), concentrate
With Rotary Evaporators by the crude extract obtained by step (3) control temperature be 20 DEG C under conditions of be concentrated into coarse extraction The 1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. concentrate obtained by step (4):Deionized water is 1:25 ratio, to obtained by step (4) Concentrate in add deionized water, stir to concentrate and be completely dissolved in deionized water, obtain the concentrate aqueous solution;
The AB-8 macroreticular resin solids for adding that particle diameter is 0.30mm in the concentrate aqueous solution of gained are stated then up, are placed Polyphenol absorption 4h is carried out in constant-temperature table, under conditions of it is 25 DEG C to control temperature, rotating speed is 180rpm, obtains adsorbing polyphenols Macroreticular resin, filtering, the macroreticular resin of deionized water cleaning adsorbing polyphenols 3 times, then control temperature to be dried for 30 DEG C, obtain To the macroreticular resin of dry adsorbing polyphenols;
Described particle diameter is the addition of 0.30-1.25mm AB-8 macroreticular resin solids, is 0.30-1.25mm by particle diameter AB-8 macroreticular resin solids:The concentrate aqueous solution is 1g:25ml ratio calculates;
Macroreticular resin AB-8 adsorption rate is determined to 67.49%;
(6), separation desorption
By the macroreticular resin of dry adsorbing polyphenols:The ethanol water that concentration of volume percent is 90% is 1g:25ml Ratio calculate, into the macroreticular resin of the adsorbing polyphenols of the drying obtained by step (5) add 25ml concentration of volume percent For 90% ethanol water, it is then placed into constant-temperature table, to control temperature be 25 DEG C, rotating speed enters under conditions of being 180rpm Row desorption 2h, is filtered to remove macroreticular resin, obtains polyphenol stripping liquid;
Macroreticular resin AB-8 desorption efficiency is determined to 87.59%;
(7) the polyphenol stripping liquid obtained by step (6), is concentrated into the 1/15 of polyphenol stripping liquid volume with Rotary Evaporators, Then it is to be freeze-dried at -60 DEG C to control temperature, obtains the polyphenol powder in passion fruit pericarp.
After testing, the wherein cubage of polyphenol is 10.93mg/g to polyphenol powder in the passion fruit pericarp of above-mentioned gained, The recovery rate of polyphenol powder in passion fruit pericarp is 39.31%.
The comparative examples 1 of embodiment 3
A kind of extracting method (being only alcohol extracting, save the collaboration processing of ultrasound) of polyphenol in passion fruit pericarp, specifically Including following step:
(1), pre-process
Passion fruit pericarp is cleaned, dried, then with vacuum freeze drier drying process, is then crushed passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), surname extraction, i.e., only it is alcohol extracting, saves the synergy of ultrasound
By passion fruit fruit peel powder:The ethanol water that concentration of volume percent is 30% is 1g:50ml ratio, by step (1) the passion fruit fruit peel powder obtained by is added in the ethanol water that concentration of volume percent is 30%, after stirring, control Temperature is 95 DEG C and carries out surname extraction processing 8h, obtains Ethanol Treatment liquid;
(3), filter
Ethanol Treatment liquid obtained by step (2) is filtered with 0.45 μm of nylon filter, obtains crude extract;
(4), concentrate
With Rotary Evaporators by the crude extract obtained by step (3) control temperature be 20 DEG C under conditions of be concentrated into coarse extraction The 1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. concentrate obtained by step (4):Deionized water is 1:25 ratio, to obtained by step (4) Concentrate in add deionized water, stir to concentrate and be completely dissolved in deionized water, obtain the concentrate aqueous solution;
The AB-8 macroreticular resin solids for adding that particle diameter is 0.30mm in the concentrate aqueous solution of gained are stated then up, are placed Polyphenol absorption 4h is carried out in constant-temperature table, under conditions of it is 25 DEG C to control temperature, rotating speed is 180rpm, obtains adsorbing polyphenols Macroreticular resin, filtering, the macroreticular resin of deionized water cleaning adsorbing polyphenols 3 times, then control temperature to be dried for 30 DEG C, obtain To the macroreticular resin of dry adsorbing polyphenols;
Described particle diameter is the addition of 0.30-1.25mm AB-8 macroreticular resin solids, is 0.30-1.25mm by particle diameter AB-8 macroreticular resin solids:The concentrate aqueous solution is 1g:25ml ratio calculates;
Macroreticular resin AB-8 adsorption rate is determined to 68.51%;
(6), separation desorption
By the macroreticular resin of dry adsorbing polyphenols:The ethanol water that concentration of volume percent is 90% is 1g:25ml Ratio calculate, into the macroreticular resin of the adsorbing polyphenols of the drying obtained by step (5) add 25ml concentration of volume percent For 90% ethanol water, it is then placed into constant-temperature table, to control temperature be 25 DEG C, rotating speed enters under conditions of being 180rpm Row desorption 2h, is filtered to remove macroreticular resin, obtains polyphenol stripping liquid;
Macroreticular resin AB-8 desorption efficiency is determined to 85.62%;
(7) the polyphenol stripping liquid obtained by step (6), is concentrated into the 1/15 of polyphenol stripping liquid volume with Rotary Evaporators, Then it is to be freeze-dried at -60 DEG C to control temperature, obtains the polyphenol powder in passion fruit pericarp.
After testing, the wherein cubage of polyphenol is 3.54mg/g to polyphenol powder in the passion fruit pericarp of above-mentioned gained, The recovery rate of polyphenol powder in passion fruit pericarp is 11.02%.
The comparative examples 2 of embodiment 3
A kind of extracting method (being only ultrasonic extraction, save alcohol extracting) of polyphenol in passion fruit pericarp, is specifically included following Step:
(1), pre-process
Passion fruit pericarp is cleaned, dried, then with vacuum freeze drier drying process, is then crushed passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), ultrasonication, the synergy of alcohol extracting is saved
By passion fruit fruit peel powder:Deionized water ratio is 1g:50ml ratio, by the passion fruit fruit peel powder obtained by step (1) It is added in deionized water, after stirring, to control frequency be 40KHz, power 350W, temperature are 55 DEG C and carried out at ultrasonic waves 5min is managed, obtains sonification fluid;
(3), filter
Treatment fluid obtained by step (2) is filtered with 0.45 μm of nylon filter, obtains crude extract;
(4), concentrate
With Rotary Evaporators by the crude extract obtained by step (3) control temperature be 20 DEG C under conditions of be concentrated into coarse extraction The 1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. concentrate obtained by step (4):Deionized water is 1:25 ratio, to obtained by step (4) Concentrate in add deionized water, stir to concentrate and be completely dissolved in deionized water, obtain the concentrate aqueous solution;
The AB-8 macroreticular resin solids for adding that particle diameter is 0.30mm in the concentrate aqueous solution of gained are stated then up, are placed Polyphenol absorption 4h is carried out in constant-temperature table, under conditions of it is 25 DEG C to control temperature, rotating speed is 180rpm, obtains adsorbing polyphenols Macroreticular resin, filtering, the macroreticular resin of deionized water cleaning adsorbing polyphenols 3 times, then control temperature to be dried for 30 DEG C, obtain To the macroreticular resin of dry adsorbing polyphenols;
Described particle diameter is the addition of 0.30-1.25mm AB-8 macroreticular resin solids, is 0.30-1.25mm by particle diameter AB-8 macroreticular resin solids:The concentrate aqueous solution is 1g:25ml ratio calculates;
Macroreticular resin AB-8 adsorption rate is determined to 63.76%;
(6), separation desorption
By the macroreticular resin of dry adsorbing polyphenols:The ethanol water that concentration of volume percent is 90% is 1g:25ml Ratio calculate, into the macroreticular resin of the adsorbing polyphenols of the drying obtained by step (5) add concentration of volume percent be 90% Ethanol water, be then placed into constant-temperature table, to control temperature be 25 DEG C, rotating speed is desorbed under conditions of being 180rpm 1h, macroreticular resin is filtered to remove, obtains polyphenol stripping liquid;
Macroreticular resin AB-8 desorption efficiency is determined to 88.13%;
(7), with Rotary Evaporators by the polyphenol stripping liquid obtained by step (6) control temperature be 20 DEG C under conditions of be concentrated into The 1/15 of polyphenol stripping liquid volume, it is to be freeze-dried at -60 DEG C then to control temperature, obtains the polyphenol powder in passion fruit pericarp End.
After testing, the wherein cubage of polyphenol is 6.23mg/g to polyphenol powder in the passion fruit pericarp of above-mentioned gained, The recovery rate of polyphenol powder in passion fruit pericarp is 21.17%.
The content of polyphenol is 10.93mg/g in polyphenol powder in the passion fruit pericarp of the final gained of above-described embodiment 3, hundred The recovery rate of polyphenol powder in fragrant fruit pericarp is the passion fruit fruit of the final gained of comparative examples 1 of 39.31%, embodiment 3 The content of polyphenol is 3.54mg/g in polyphenol powder in skin, and the recovery rate of the polyphenol powder in passion fruit pericarp is 11.02%, The content of polyphenol is 6.23mg/g in polyphenol powder in the passion fruit pericarp of the final gained of the comparative examples 2 of embodiment 3, hundred The recovery rate of polyphenol powder in fragrant fruit pericarp is 21.17%, passes through contrast, it can be seen that the step of the embodiment of the present invention 3 (2) The middle recovery rate that polyphenol powder in the passion fruit pericarp extracted is cooperateed with using ultrasound-ethanol, the comparative examples 1 of embodiment 3 Using the extraction of supercritical ultrasonics technology in the step of in step (2) using than comparative examples 2 of soxhlet extraction and embodiment 3 (2) Rate is all high, its reason, it may be possible to due to the result of ultrasound-ethanol collaboration extraction effect, is indicated above using ultrasound-ethanol collaboration Polyphenol can effectively improve the recovery rate of polyphenol in extraction passion fruit pericarp, while can provide in the polyphenol powder in passion fruit pericarp The content of polyphenol.
Further, the oxidation resistance of passion fruit pericarp polyphenol, reference literature are determined according to DPPH radicals scavengings method Xican Li(Chemistry Central Journal,2012,6:140), with ultraviolet specrophotometer (Alpha-1860S, Shanghai spectral element) in wavelength be 519nm place measure light absorption value.To above-described embodiment 1-3, the comparative examples 1 (in figure of embodiment 3 Reference examples 1), the extraction process of the comparative examples 2 (reference examples 2 in figure) of embodiment 3 the step of crude extract obtained by (3) The clearance rate situation of DPPH free radicals is measured respectively, as a result sees Fig. 1, as can be seen from Figure 1 ultrasonic wave-second of the invention The passion fruit pericarp polyphenol crude extract DPPH free radical scavenging activities that alcohol collaboration extraction method obtains can reach 78.01%;It is real Ultrasonic wave-ethanol collaboration extraction method passion fruit pericarp polyphenol crude extract DPPH the free radical scavenging activities for applying example 3 are 54.61%, Soxhlet extraction passion fruit pericarp polyphenol crude extract DPPH free radical scavenging activities in the comparative examples 1 of embodiment 3 are 10.85%;Supercritical ultrasonics technology passion fruit pericarp polyphenol crude extract DPPH radicals scavengings in the comparative examples 2 of embodiment 3 Rate is 21.78%, has also further been confirmed in the step (2) of the present invention using the effect of ultrasonic wave-ethanol collaboration extraction.
Further, according to ABTS+Radicals scavenging method determines the oxidation resistance of passion fruit pericarp polyphenol, reference literature Anna Floegel(Journal of Food Composition and Analysis,2011:1043-1048), use is ultraviolet Spectrophotometer (Alpha-1860S, Shanghai spectral element) is that light absorption value is determined at 734nm in wavelength.To above-described embodiment 1-3, reality Apply the extraction of the comparative examples 1 (reference examples 1 in figure), the comparative examples 2 of embodiment 3 (reference examples 2 in figure) of example 3 Crude extract is respectively to ABTS obtained by the step of journey (3)+The clearance rate situation of free radical is measured, and as a result sees Fig. 2, from Fig. 2 It can be seen that the passion fruit pericarp polyphenol crude extract ABTS that the ultrasonic wave of the present invention-ethanol collaboration extraction method obtains+Free radical Clearance rate can reach 95.68%.The ultrasonic wave of embodiment 3-ethanol collaboration extraction method passion fruit pericarp polyphenol crude extract ABTS+Free radical scavenging activity is 73.23%, and the soxhlet extraction passion fruit pericarp polyphenol in the comparative examples 1 of embodiment 3 is thick Extract solution ABTS+Free radical scavenging activity is 13.56%;Supercritical ultrasonics technology passion fruit pericarp in the comparative examples 2 of embodiment 3 is more Phenol crude extract ABTS+Free radical scavenging activity is 36.45%, has also further been confirmed in the step (2) of the present invention using ultrasound The effect of ripple-ethanol collaboration extraction.
In summary, the extracting method of the polyphenol in a kind of passion fruit pericarp of the invention, the polyphenol in passion fruit pericarp Powder yield is reached as high as 50.35%, and the content of polyphenol is calculated by the polyphenol powder in every gram of passion fruit pericarp, and it contains more Phenol reaches as high as 14.06mg, further, due to removing of the crude extract obtained by the extracting method of the present invention to DPPH free radicals Rate can reach 78.01%;To ABTS+The clearance rate of free radical can reach 95.68%, therefore the hundred of final gained are fragrant Polyphenol in fruit pericarp, which can be added to as functional components in cosmetics, plays its removing free radical, purposes of anti-aging. And the extracting method of the present invention has the advantages of extraction time is short, and polyphenol recovery rate is high, and polyphenol inoxidizability is strong.
Described above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art For personnel, without departing from the technical principles of the invention, some improvement and modification can also be made, these improve and become Type also should be regarded as protection scope of the present invention.

Claims (4)

1. the extracting method of the polyphenol in a kind of passion fruit pericarp, it is characterised in that specifically include following steps:
(1), pretreatment
Passion fruit pericarp is cleaned, dried, then with vacuum freeze drier drying process, passion fruit pericarp is then crushed to grain Spend for 60-200 targeted fine powders, obtain passion fruit fruit peel powder;
(2), alcohol steep and supersound process
By passion fruit fruit peel powder:The ethanol water that concentration of volume percent is 30-80% is 1g:20-50 ml ratio, it will walk Suddenly(1)The passion fruit fruit peel powder of gained is added in the ethanol water that concentration of volume percent is 30-80%, after stirring, To control frequency be 30-40KHz, power 200-400W, temperature are 30-70 DEG C and carry out supersound process 5-35min, is obtained at ultrasonic wave Manage liquid;
(3), filtering
By step(2)After the static placement of ultrasonication liquid of gained, supernatant is taken, with 0.45 μm -0.80 μm of nylon filter Device filters, and obtains crude extract;
(4), concentration
With Rotary Evaporators by step(3)The crude extract of gained control temperature be 20-25 DEG C under conditions of be concentrated into coarse extraction The 1/20-1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. step(4)The concentrate of gained:Deionized water is 1g:20-30ml ratio, to step(4)Institute Deionized water is added in the concentrate obtained, stirs to concentrate and is completely dissolved in deionized water, obtain the concentrate aqueous solution;
The macroreticular resin solid for adding that particle diameter is 0.30-1.25mm in the concentrate aqueous solution of gained is stated then up, is positioned over Polyphenol absorption 2-4h is carried out in constant-temperature table, under conditions of it is 25 DEG C to control temperature, rotating speed is 100-180rpm, it is more to obtain absorption The macroreticular resin of phenol, filtering, the macroreticular resin of deionized water cleaning adsorbing polyphenols 3-5 times, temperature is then controlled to enter for 20-30 DEG C Row drying, obtain the macroreticular resin of dry adsorbing polyphenols;
The macroreticular resin solid that described particle diameter is 0.30-1.25mm be AB-8, HP-20, FPX-66, SP-850, DM-301 or XAD-2 types, its addition, by the macroreticular resin solid that particle diameter is 0.30-1.25mm:The concentrate aqueous solution is 1g:20-30ml Ratio calculate;
(6), separation desorption
By the macroreticular resin of dry adsorbing polyphenols:The ethanol water that concentration of volume percent is 80-90% is 1g:20-30ml Ratio calculate, to step(5)It is 80- that concentration of volume percent is added in the macroreticular resin of the adsorbing polyphenols of the drying of gained 90% ethanol water, is then placed into constant-temperature table, under conditions of it is 25 DEG C to control temperature, rotating speed is 100-180rpm Desorption 1-2h is carried out, is filtered to remove macroreticular resin, obtains polyphenol stripping liquid;
(7), with Rotary Evaporators by step(6)The polyphenol stripping liquid of gained is concentrated into the 1/20-1/15 of polyphenol stripping liquid volume, Then it is to be freeze-dried at -50--60 DEG C to control temperature, obtains the polyphenol powder in passion fruit pericarp.
A kind of 2. extracting method of the polyphenol in passion fruit pericarp as described in right 1, it is characterised in that:
Step(1)It is middle that passion fruit pericarp is crushed into granularity is 60 targeted fine powders;
Step(2)It is middle to control frequency 40KHz, power 350W, temperature to be 30 DEG C to carry out supersound process 25min, obtain at ultrasonic wave Manage liquid;
Step(3)It is middle to be filtered with 0.45 μm of nylon filter, obtain crude extract;
Step(5)Described in particle diameter be 0.30-1.25mm macroreticular resin solid be DM-301, HP-20 or AB-8, it is described Particle diameter is the addition of 0.30-1.25mm macroreticular resin solid, by the macroreticular resin solid that particle diameter is 0.30-1.25mm:It is dense The contracting liquid aqueous solution is 1g:30ml ratio calculates.
3. the extracting method of the polyphenol in a kind of passion fruit pericarp as claimed in claim 2, it is characterised in that step(2)It is super In sound-ethanol collaboration processing, passion fruit fruit peel powder:The ethanol water that concentration of volume percent is 30-80% is 1g:50ml;
Step(5)In separation absorption:Polyphenol absorption 4h is carried out under conditions of it is 25 DEG C to control temperature, rotating speed is 180rpm;
Step(6)Desorption 2h is carried out under conditions of it is 25 DEG C that temperature is controlled in separation desorption, rotating speed is 180rpm;
Step(7)Described in freeze-drying temperature be -60 DEG C.
4. the extracting method of the polyphenol in a kind of passion fruit pericarp as claimed in claim 3, it is characterised in that step(2)It is super In sound-ethanol collaboration processing, passion fruit fruit peel powder:The ethanol water that concentration of volume percent is 55% is 1g:50ml.
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