CN107362080B - 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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CN107362080B
CN107362080B CN201710585096.6A CN201710585096A CN107362080B CN 107362080 B CN107362080 B CN 107362080B CN 201710585096 A CN201710585096 A CN 201710585096A CN 107362080 B CN107362080 B CN 107362080B
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polyphenol
passion fruit
macroreticular resin
resulting
fruit pericarp
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CN107362080A (en
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刘慧敏
王伟
魏继文
刘清雷
吴健
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET PURPOSES
    • A61K8/00Cosmetics or similar toilet preparations
    • A61K8/18Cosmetics or similar toilet preparations characterised by the composition
    • A61K8/96Cosmetics or similar toilet preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toilet preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A23B - A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • 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 TOILET PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET 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
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET 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
    • A61K2800/82Preparation or application process involves sonication or ultrasonication
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL, OR TOILET 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

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, crush;It then using 30%-80% ethyl alcohol as solution, and is 200-400W in ultrasonic power, temperature carries out ultrasonic wave-ethyl alcohol collaboration under conditions of 30-70 DEG C and extracts 5-35min, then filtered with 0.45 μm -0.80 μm of nylon filter, concentration;Concentrate is isolated and purified with the macroreticular resin of partial size 0.30-1.25mm, vacuum freeze drying obtains the polyphenol powder in passion fruit pericarp.The recovery rate and purity that the extracting method cooperates with the combinations of technologies such as extraction, macroreticular resin separating-purifying and vacuum freeze drying by ultrasound-ethyl alcohol, ensures polyphenol.The recovery rate of polyphenol in final resulting passion fruit pericarp can reach 33.95-50.35%.The present invention provides a kind of new method for the effective use of passion fruit pericarp, can turn 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 fields, and in particular to a kind of extraction side of the polyphenol in passion fruit pericarp Method.
Background technique
Plant polyphenol is the intracorporal complicated phenols secondary metabolites of 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 discovery polyphenols plays an important role in human disease treatment and health protection, has There are a variety of physiology function 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 mature, and the polyphenol extracted has been applied to food, cosmetics and field of medicaments.
Passion fruit (passion fruit) is herbaceous species plant also known as the passion fruit, heat of Passifloraceae Passiflora Feelings fruit is a kind of tropical fruit (tree), and pulp is orange, and seed is edible;Mainly there are purple fruit and yellow fruit two major classes.Passion fruit is super because having It crosses the strong fragrance of 165 kinds of aromatic substances and 10 various fruits and well-known, enjoys the good reputation of " king of beverage " and " beverage essence ". Research finds that the ingredient beneficial to human body is all contained at each position of passion fruit, wherein pectin, polysaccharide, Flavonoid substances, vitamin Class content is the abundantest, while also containing huge Development volue containing more than 10 kinds of minerals isoreactivity ingredient.Fruit juice can It is processed into natural quality beverage, fruit dew, jam, jelly, preserved fruit, not only unique flavor, full of nutrition, and healthcare, It helps 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 mentions The pectin taken is the good stabilizer and thickener of food processing;Root, stem, Ye Junke are 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 that discovery contains The most edible plants of polyphenol substance.90% or more polyphenol is present in skin and core in document report passion fruit fruit, and By-product of the passion fruit pericarp as passion fruit, accounts for the 40%-55% of gross mass, and 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 or vacancy of extraction process.
In recent years, research of the passion fruit in nutrition, area of pharmacology has obtained many scientific achievements, and is extracting work The research of skill optimization aspect is mainly the extraction of pectin, seed oil, is ground to the method and technique of the extraction of passion fruit polyphenols Study carefully seldom, and report yet there are no to the extraction of passion fruit pericarp polyphenol research, therefore it is necessary to develop new technology Polyphenols antioxidant is extracted from discarded passion fruit pericarp, is reinforced the comprehensive utilization of passion fruit pericarp, is turned waste into wealth, mentions High added value.
Summary of the invention
It is an object of the invention to provide a kind of extracting method of polyphenol in passion fruit pericarp, which has operation letter Just, extraction efficiency is high, can reinforce the comprehensive utilization of passion fruit pericarp, turn waste into wealth, improves added value.
Technical solution of the present invention:
A kind of extracting method of polyphenol in passion fruit pericarp, i.e., assist to extract and obtain passion fruit fruit with ultrasonic wave-ethyl alcohol Then skin polyphenol crude product is separated by macroreticular resin, the polyphenol in passion fruit pericarp is obtained after dry.
It is final to determine the optimum condition isolated and purified are as follows: selection DM-301 macroreticular resin, adsorption rate 78.89%, desorption Rate is 98.95%;The ethyl alcohol that concentration is 90%v/v is strippant elution.
Its extraction process specifically includes the following steps:
(1), it pre-processes
Passion fruit pericarp is cleaned, is dried, then is dried with vacuum freeze drier, then crushes passion fruit pericarp It is 60-200 targeted fine powder to granularity, preferably 60 mesh obtain passion fruit fruit peel powder;
(2), ultrasound-ethyl alcohol collaboration processing
In passion fruit fruit peel powder: the ratio that the ethanol water that concentration of volume percent is 30-80% is 1g:20-50ml, The resulting passion fruit fruit peel powder of step (1) is added in the ethanol water that concentration of volume percent is 30-80%, stirring is equal After even, control frequency is 30-40KHz, power 200-400W, temperature are 30-70 DEG C and carry out ultrasonic treatment 5-35min, preferably It is 30 DEG C for 40KHz, power 350W, temperature and carries out ultrasonic treatment 25min, obtains ultrasonication liquid;
(3), it filters
After the resulting static placement of ultrasonication liquid of step (2), supernatant is taken, with 0.45 μm -0.80 μm, preferably 0.45 μm of nylon filter filtering, obtains crude extract;
(4), it is concentrated
Step (3) resulting crude extract is concentrated under conditions of 20-25 DEG C with Rotary Evaporators thick The 1/20-1/15 of extracting liquid volume obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. step (4) resulting concentrate: deionized water is the ratio of 1:20-30, to step (4) Deionized water is added in resulting concentrate, stirring is completely dissolved in deionized water to concentrate, obtains concentrate aqueous solution;
The macroreticular resin solid for being added that partial size is 0.30-1.25mm in resulting concentrate aqueous solution is stated then up, is put It is placed in constant-temperature table, carries out polyphenol under conditions of being 100-180rpm controlled at 25-45 DEG C, revolving speed and adsorb 2-4h, obtain To the macroreticular resin of adsorbing polyphenols, filtering, deionized water cleans macroreticular resin 3-5 times of adsorbing polyphenols, then controlled at 20-30 DEG C is dried, and obtains the macroreticular resin of dry adsorbing polyphenols;
The macroreticular resin solid that the partial size 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, additional amount, the macroreticular resin solid for being 0.30-1.25mm by partial size: concentrate The ratio that aqueous solution is 1g:20-30ml 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: The ratio of 20-30ml calculates, and concentration of volume percent is added into the macroreticular resin of the adsorbing polyphenols of step (5) resulting drying It for the ethanol water of 80-90%, is then placed into constant-temperature table, controlled at 25-45 DEG C, revolving speed 100-180rpm Under conditions of carry out desorption 1-2h, be filtered to remove macroreticular resin, obtain polyphenol stripping liquid;
(7), the resulting polyphenol stripping liquid of step (6) is concentrated into the 1/20- of polyphenol stripping liquid volume with Rotary Evaporators 1/15, then controlled at being freeze-dried at -50--60 DEG C, obtain the polyphenol powder in passion fruit pericarp.
The content of polyphenol powder in above-mentioned resulting passion fruit pericarp, polyphenol is calculated by every gram of passion fruit pericarp, is contained Some polyphenol reach as high as 14.06mg, can be used as functional components and are added in cosmetics and play it and remove free radical, anti-ageing Old purposes.
Advantageous effects of the invention
The extracting method of polyphenol in a kind of passion fruit pericarp of the invention, due to extracting and making using ultrasound-ethyl alcohol collaboration With the polyphenol extracted in passion fruit, pericarp garbage utilization rate is substantially increased, the recovery rate of polyphenol reaches in final passion fruit pericarp The extracted amount of 33.95-50.35%, 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, due to utilizing ultrasonic wave in the process Cavitation realize ethyl alcohol localized hyperthermia, high pressure, along with ultrasonic wave mechanical disturbance act on, 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 extraction side of the invention Method has the time short, and low energy consumption, and medicinal raw material treating capacity is big, extracts active material and is not destroyed;It is environmentally protective, reduce environment The features such as pollution, has good commercial introduction value.
Further, the extracting method of the polyphenol in a kind of passion fruit pericarp of the invention, resulting passion fruit polyphenol slightly mention Liquid is taken to can reach 78.01% to the clearance rate of DPPH free radical;To ABTS+The clearance rate of free radical can reach 95.68%, therefore resulting passion fruit pericarp polyphenol extracting solution can be used as functional additive and be applied to food, cosmetics In, it plays it and removes free radical, anti-aging purposes.Since adsorption process makes polyphenol be adsorbed on macroreticular resin using physical method In, plant polyose is effectively removed, the impurity such as albumen significantly improve the yield and antioxidant activity of polyphenol, and isolate and purify 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 antioxidant, so that passion fruit pericarp has been obtained effective comprehensive utilization, turns waste into wealth, improves The added value of passion fruit pericarp provides a kind of new approach for increasing peasant income.
In conclusion the extracting method of the polyphenol in a kind of passion fruit pericarp of the invention, is mentioned by ultrasound-ethyl alcohol collaboration It takes, the combination of technologies such as macroreticular resin separating-purifying and vacuum freeze drying, the recovery rate and purity for ensuring polyphenol, has and mention Take the time short, polyphenol recovery rate is high, the strong advantage of polyphenol inoxidizability, before having a wide range of applications in foods and cosmetics Scape.
Detailed description of the invention
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 (3) resulting crude extract is respectively to the clearance rate situation of DPPH free radical;
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 (3) resulting crude extract is respectively to ABTS+The clearance rate situation of free radical.
Specific embodiment
Below 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 passion fruit pericarp obtained in various embodiments of the present invention are as follows:
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;
In formula: m1: the quality of the passion fruit pericarp polyphenol extracted;m2: the quality of passion fruit pericarp polyphenol in raw material.
Polyphenol content is measured by Folin-Ciocalteu method 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 dilution is accurately pipetted into 10ml colorimetric cylinder, is added 1.0ml Folin-Ciocalteu reagent, is mixed;In In 0.5min~2min, it is separately added into 10% sodium carbonate liquor of 1.5ml, is vibrated, with deionized water constant volume.Above-mentioned standard is molten Liquid after 25 DEG C of placement 1.5h, with ultraviolet specrophotometer (Alpha-1860S, Shanghai spectral element) in wavelength be 765nm place measurement Light absorption value.Corresponding gallic acid concentration is calculated from gallic acid standard curve, calculates polyphenol content by above-mentioned formula.
The measurement of the adsorption rate of macroreticular resin, desorption efficiency in various embodiments of the present invention, reference literature Lisha Xi (Food Chemistry 172:166-174,2015,China).Method is as follows, accurately weighs by (the filter paper suction of pretreated wet resin It is dry) each M g, it is placed in 100ml tool plug ground triangular flask, additions total phenol concentration is C0Extraction filtered fluid V ml, in certain temperature Lower Static Adsorption 2-4h is spent, adsorption equilibrium is made up to.Resin is filtered out, Folin-Ciocalteu method measures remaining more in solution Phenol concentration Ce;Vibrate the resin that polyphenol has been adsorbed in elution, Folin-Ciocalteu method at a certain temperature with eluant, eluent appropriate Measure 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) when 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 the following steps:
(1), it pre-processes
Passion fruit pericarp is cleaned, is dried, then is dried with vacuum freeze drier, then crushes passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), ultrasound-ethyl alcohol collaboration processing
In passion fruit fruit peel powder: the ratio that the ethanol water that concentration of volume percent is 80% is 1g:50ml, by step (1) resulting passion fruit fruit peel powder is added in the ethanol water that concentration of volume percent is 80%, after mixing evenly, control Frequency is 40KHz, power 200W, temperature are 70 DEG C and carry out ultrasonic treatment 5min, obtains ultrasonication liquid;
(3), it filters
After the resulting static placement of ultrasonication liquid of step (2), supernatant is taken, with 0.45 μm of nylon filter mistake Filter, obtains crude extract;
(4), it is concentrated
Step (3) resulting crude extract is concentrated into coarse extraction under conditions of 20 DEG C with Rotary Evaporators The 1/20 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. step (4) resulting concentrate: deionized water is the ratio of 1:25, to obtained by step (4) Concentrate in be added deionized water, stirring is completely dissolved in deionized water to concentrate, obtains concentrate aqueous solution;
The HP-20 macroreticular resin solid for being added that partial size is 0.30mm in resulting concentrate aqueous solution is stated then up, is put It is placed in constant-temperature table, carries out polyphenol under conditions of being 180rpm controlled at 25 DEG C, revolving speed and adsorb 4h, obtain adsorbing polyphenols Macroreticular resin, filtering, deionized water cleans macroreticular resin for 3 times of adsorbing polyphenols, is then dried controlled at 30 DEG C, Obtain the macroreticular resin of dry adsorbing polyphenols;
The partial size is the additional amount of the HP-20 macroreticular resin solid of 0.30-1.25mm, is 0.30- by partial size The HP-20 macroreticular resin solid of 1.25mm: the ratio that concentrate aqueous solution is 1g:25ml calculates;
The adsorption rate of macroreticular resin HP-20 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 step (5) resulting drying be added concentration of volume percent be 90% Ethanol water, be then placed into constant-temperature table, controlled at 25 DEG C, revolving speed be 180rpm under conditions of desorbed 2h is filtered to remove macroreticular resin, obtains polyphenol stripping liquid;
The desorption efficiency of macroreticular resin HP-20 is determined to 90.51%;
(7), the resulting polyphenol stripping liquid of step (6) is concentrated into the 1/20 of polyphenol stripping liquid volume with Rotary Evaporators, Then controlled at being freeze-dried at -60 DEG C, the polyphenol powder in passion fruit pericarp is obtained.
Polyphenol powder in above-mentioned resulting passion fruit pericarp is through detecting, and wherein the content of polyphenol is calculated as 9.87mg/g, 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 the following steps:
(1), it pre-processes
Passion fruit pericarp is cleaned, is dried, then is dried with vacuum freeze drier, then crushes passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), ultrasound-ethyl alcohol collaboration processing
In passion fruit fruit peel powder: the ratio that the ethanol water that concentration of volume percent is 55% is 1g:50ml, by step (1) resulting passion fruit fruit peel powder is added in the ethanol water that concentration of volume percent is 55%, after mixing evenly, control Frequency is 40KHz, power 350W, temperature are 30 DEG C and carry out ultrasonic treatment 25min, obtains ultrasonication liquid;
(3), it filters
After the resulting static placement of ultrasonication liquid of step (2), supernatant is taken, with 0.45 μm of nylon filter mistake Filter, obtains crude extract;
(4), it is concentrated
Step (3) resulting crude extract is concentrated into coarse extraction under conditions of 25 DEG C with Rotary Evaporators The 1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. step (4) resulting concentrate: deionized water is the ratio of 1:30, to obtained by step (4) Concentrate in be added deionized water, stirring is completely dissolved in deionized water to concentrate, obtains concentrate aqueous solution;
The DM-301 macroreticular resin solid for being added that partial size is 0.30mm in resulting concentrate aqueous solution is stated then up, is put It is placed in constant-temperature table, carries out polyphenol under conditions of being 180rpm controlled at 25 DEG C, revolving speed and adsorb 4h, obtain adsorbing polyphenols Macroreticular resin, filtering, deionized water cleans macroreticular resin for 3 times of adsorbing polyphenols, is then dried controlled at 30 DEG C, Obtain the macroreticular resin of dry adsorbing polyphenols;
The partial size is the additional amount of the DM-301 macroreticular resin solid of 0.30-1.25mm, is 0.30- by partial size The DM-301 macroreticular resin solid of 1.25mm: the ratio that concentrate aqueous solution is 1g:30ml calculates;
The adsorption rate of macroreticular resin DM-301 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 step (5) resulting drying be added concentration of volume percent be 80% Ethanol water, be then placed into constant-temperature table, controlled at 25 DEG C, revolving speed be 180rpm under conditions of desorbed 2h is filtered to remove macroreticular resin, obtains polyphenol stripping liquid;
The desorption efficiency of macroreticular resin DM-301 is determined to 98.95%;
(7), the resulting polyphenol stripping liquid of step (6) is concentrated into the 1/15 of polyphenol stripping liquid volume with Rotary Evaporators, Then controlled at being freeze-dried at -60 DEG C, the polyphenol powder in passion fruit pericarp is obtained.
Polyphenol powder in above-mentioned resulting passion fruit pericarp is through detecting, and wherein the content of polyphenol calculates to obtain 14.06mg/g, 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 the following steps:
(1), it pre-processes
Passion fruit pericarp is cleaned, is dried, then is dried with vacuum freeze drier, then crushes passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), ultrasound-ethyl alcohol collaboration processing
In passion fruit fruit peel powder: the ratio that the ethanol water that concentration of volume percent is 30% is 1g:50ml, by step (1) resulting passion fruit fruit peel powder is added in the ethanol water that concentration of volume percent is 30%, after mixing evenly, control Frequency is 40KHz, power 350W, temperature are 55 DEG C and carry out ultrasonic treatment 5min, obtains ultrasonication liquid;
(3), it filters
After the resulting static placement of ultrasonication liquid of step (2), supernatant is taken, with 0.45 μm of nylon filter mistake Filter, obtains crude extract;
(4), it is concentrated
Step (3) resulting crude extract is concentrated into coarse extraction under conditions of 20 DEG C with Rotary Evaporators The 1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. step (4) resulting concentrate: deionized water is the ratio of 1:25, to obtained by step (4) Concentrate in be added deionized water, stirring is completely dissolved in deionized water to concentrate, obtains concentrate aqueous solution;
The AB-8 macroreticular resin solid for being added that partial size is 0.30mm in resulting concentrate aqueous solution is stated then up, is placed In constant-temperature table, polyphenol is carried out under conditions of being 180rpm controlled at 25 DEG C, revolving speed and adsorbs 4h, obtains adsorbing polyphenols Macroreticular resin, filtering, deionized water clean macroreticular resin 3 times of adsorbing polyphenols, are then dried, obtain controlled at 30 DEG C To the macroreticular resin of dry adsorbing polyphenols;
The partial size is the additional amount of the AB-8 macroreticular resin solid of 0.30-1.25mm, is 0.30-1.25mm by partial size AB-8 macroreticular resin solid: concentrate aqueous solution be 1g:25ml ratio calculate;
The adsorption rate of macroreticular resin AB-8 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 step (5) resulting drying be added 25ml concentration of volume percent For 90% ethanol water, be then placed into constant-temperature table, controlled at 25 DEG C, revolving speed be 180rpm under conditions of into Row desorption 2h, is filtered to remove macroreticular resin, obtains polyphenol stripping liquid;
The desorption efficiency of macroreticular resin AB-8 is determined to 87.59%;
(7), the resulting polyphenol stripping liquid of step (6) is concentrated into the 1/15 of polyphenol stripping liquid volume with Rotary Evaporators, Then controlled at being freeze-dried at -60 DEG C, the polyphenol powder in passion fruit pericarp is obtained.
Polyphenol powder in above-mentioned resulting passion fruit pericarp is through detecting, and wherein the content of polyphenol is calculated as 10.93mg/g, 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), it pre-processes
Passion fruit pericarp is cleaned, is dried, then is dried with vacuum freeze drier, then crushes passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), Soxhlet extraction is only alcohol extracting, save the synergistic effect of ultrasound
In passion fruit fruit peel powder: the ratio that the ethanol water that concentration of volume percent is 30% is 1g:50ml, by step (1) resulting passion fruit fruit peel powder is added in the ethanol water that concentration of volume percent is 30%, after mixing evenly, control Temperature is that 95 DEG C of progress Soxhlet extractions handle 8h, obtains alcohol treatment liquid;
(3), it filters
0.45 μm of nylon filter of the resulting alcohol treatment liquid of step (2) is filtered, crude extract is obtained;
(4), it is concentrated
Step (3) resulting crude extract is concentrated into coarse extraction under conditions of 20 DEG C with Rotary Evaporators The 1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. step (4) resulting concentrate: deionized water is the ratio of 1:25, to obtained by step (4) Concentrate in be added deionized water, stirring is completely dissolved in deionized water to concentrate, obtains concentrate aqueous solution;
The AB-8 macroreticular resin solid for being added that partial size is 0.30mm in resulting concentrate aqueous solution is stated then up, is placed In constant-temperature table, polyphenol is carried out under conditions of being 180rpm controlled at 25 DEG C, revolving speed and adsorbs 4h, obtains adsorbing polyphenols Macroreticular resin, filtering, deionized water clean macroreticular resin 3 times of adsorbing polyphenols, are then dried, obtain controlled at 30 DEG C To the macroreticular resin of dry adsorbing polyphenols;
The partial size is the additional amount of the AB-8 macroreticular resin solid of 0.30-1.25mm, is 0.30-1.25mm by partial size AB-8 macroreticular resin solid: concentrate aqueous solution be 1g:25ml ratio calculate;
The adsorption rate of macroreticular resin AB-8 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 step (5) resulting drying be added 25ml concentration of volume percent For 90% ethanol water, be then placed into constant-temperature table, controlled at 25 DEG C, revolving speed be 180rpm under conditions of into Row desorption 2h, is filtered to remove macroreticular resin, obtains polyphenol stripping liquid;
The desorption efficiency of macroreticular resin AB-8 is determined to 85.62%;
(7), the resulting polyphenol stripping liquid of step (6) is concentrated into the 1/15 of polyphenol stripping liquid volume with Rotary Evaporators, Then controlled at being freeze-dried at -60 DEG C, the polyphenol powder in passion fruit pericarp is obtained.
Polyphenol powder in above-mentioned resulting passion fruit pericarp is through detecting, and wherein the content of polyphenol is calculated as 3.54mg/g, 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, specifically includes following Step: (1) it, pre-processes
Passion fruit pericarp is cleaned, is dried, then is dried with vacuum freeze drier, then crushes passion fruit pericarp It is 60 targeted fine powders to granularity, obtains passion fruit fruit peel powder;
(2), ultrasonication saves the synergistic effect of alcohol extracting
In passion fruit fruit peel powder: deionized water is than the ratio for 1g:50ml, by the resulting passion fruit fruit peel powder of step (1) It is add to deionized water, after mixing evenly, control frequency is 40KHz, power 350W, temperature are at 55 DEG C of progress ultrasonic waves 5min is managed, sonification fluid is obtained;
(3), it filters
0.45 μm of nylon filter of step (2) resulting treatment fluid is filtered, crude extract is obtained;
(4), it is concentrated
Step (3) resulting crude extract is concentrated into coarse extraction under conditions of 20 DEG C with Rotary Evaporators The 1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. step (4) resulting concentrate: deionized water is the ratio of 1:25, to obtained by step (4) Concentrate in be added deionized water, stirring is completely dissolved in deionized water to concentrate, obtains concentrate aqueous solution;
The AB-8 macroreticular resin solid for being added that partial size is 0.30mm in resulting concentrate aqueous solution is stated then up, is placed In constant-temperature table, polyphenol is carried out under conditions of being 180rpm controlled at 25 DEG C, revolving speed and adsorbs 4h, obtains adsorbing polyphenols Macroreticular resin, filtering, deionized water clean macroreticular resin 3 times of adsorbing polyphenols, are then dried, obtain controlled at 30 DEG C To the macroreticular resin of dry adsorbing polyphenols;
The partial size is the additional amount of the AB-8 macroreticular resin solid of 0.30-1.25mm, is 0.30-1.25mm by partial size AB-8 macroreticular resin solid: concentrate aqueous solution be 1g:25ml ratio calculate;
The adsorption rate of macroreticular resin AB-8 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 step (5) resulting drying be added concentration of volume percent be 90% Ethanol water, be then placed into constant-temperature table, controlled at 25 DEG C, revolving speed be 180rpm under conditions of desorbed 1h is filtered to remove macroreticular resin, obtains polyphenol stripping liquid;
The desorption efficiency of macroreticular resin AB-8 is determined to 88.13%;
(7), the resulting polyphenol stripping liquid of step (6) is concentrated under conditions of 20 DEG C with Rotary Evaporators The 1/15 of polyphenol stripping liquid volume obtains the polyphenol powder in passion fruit pericarp then controlled at being freeze-dried at -60 DEG C End.
Polyphenol powder in above-mentioned resulting passion fruit pericarp is through detecting, and wherein the content of polyphenol is calculated as 6.23mg/g, 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 final resulting passion fruit pericarp of above-described embodiment 3, hundred The recovery rate of polyphenol powder in fragrant fruit pericarp is the final resulting passion fruit fruit 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 final resulting passion fruit pericarp of the comparative examples 2 of embodiment 3, hundred The recovery rate of polyphenol powder in fragrant fruit pericarp is 21.17%, passes through comparison, it can be seen that the step of the embodiment of the present invention 3 (2) The recovery rate of polyphenol powder in the middle passion fruit pericarp extracted using ultrasound-ethyl alcohol collaboration, 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, reason, it may be possible to since ultrasound-ethyl alcohol collaboration extraction effect is as a result, be indicated above using ultrasound-ethyl alcohol collaboration The recovery rate of polyphenol can be effectively improved by extracting polyphenol in passion fruit pericarp, while can be provided in the polyphenol powder in passion fruit pericarp The content of polyphenol.
Further, according to the oxidation resistance of DPPH radicals scavenging method measurement passion fruit pericarp polyphenol, reference literature Xican Li (Chemistry Central Journal, 2012,6:140), with ultraviolet specrophotometer (Alpha-1860S, Shanghai spectral element) in wavelength be 519nm place measurement light absorption value.To the comparative examples 1 of above-described embodiment 1-3, embodiment 3 (in figure Reference examples 1), the extraction process of the comparative examples 2 (reference examples 2 in figure) of embodiment 3 the step of (3) obtained by crude extract The clearance rate situation of DPPH free radical is measured respectively, the result is shown in Figure 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 activity that alcohol collaboration extraction method obtains can reach 78.01%;It is real Ultrasonic wave-ethyl alcohol collaboration extraction method passion fruit pericarp polyphenol crude extract DPPH the free radical scavenging activity for applying example 3 is 54.61%, Soxhlet extraction passion fruit pericarp polyphenol crude extract DPPH free radical scavenging activity in the comparative examples 1 of embodiment 3 is 10.85%;Supercritical ultrasonics technology passion fruit pericarp polyphenol crude extract DPPH radicals scavenging in the comparative examples 2 of embodiment 3 Rate is 21.78%, has also further confirmed the effect extracted in step of the invention (2) using ultrasonic wave-ethyl alcohol collaboration.
Further, according to ABTS+Radicals scavenging method measures 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 measured 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 obtained by the step of journey (3) is respectively to ABTS+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 ultrasonic wave of the invention-ethyl alcohol collaboration extraction method obtains+Free radical Clearance rate can reach 95.68%.The ultrasonic wave of embodiment 3-ethyl alcohol cooperates with 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 Extracting 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 step of the invention (2) using ultrasound The effect that wave-ethyl alcohol collaboration is extracted.
The polyphenol in conclusion extracting method of the polyphenol in a kind of passion fruit pericarp of the invention, in passion fruit pericarp Powder yield reaches as high as being 50.35%, and the content of polyphenol is calculated by the polyphenol powder in every gram of passion fruit pericarp, contains more Phenol reaches as high as 14.06mg, further, the removing due to the resulting crude extract of extracting method of the invention to DPPH free radical Rate can reach 78.01%;To ABTS+The clearance rate of free radical can reach 95.68%, therefore final resulting hundred perfume Polyphenol in fruit pericarp can be used as functional components and be added to the purposes for playing its removing free radical, anti-aging in cosmetics. And extracting method of the invention has extraction time short, and polyphenol recovery rate is high, the strong advantage of polyphenol inoxidizability.
The 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, several improvements and modifications can also be made, these improve and become Type also should be regarded as protection scope of the present invention.

Claims (4)

1. a kind of extracting method of the polyphenol in passion fruit pericarp, it is characterised in that specifically includes the following steps:
(1), it pre-processes
Passion fruit pericarp is cleaned, is dried, then is dried with vacuum freeze drier, passion fruit pericarp is then crushed to grain Degree is 60-200 targeted fine powder, obtains passion fruit fruit peel powder;
(2), alcohol steep and ultrasonic treatment
In passion fruit fruit peel powder: the ratio that the ethanol water that concentration of volume percent is 30-80% is 1g:20-50ml will walk Suddenly (1) resulting passion fruit fruit peel powder is added in the ethanol water that concentration of volume percent is 30-80%, is stirred evenly Afterwards, control frequency is 30-40KHz, power 200-400W, temperature are 30-70 DEG C and carry out ultrasonic treatment 5-35min, is obtained ultrasonic Wave treatment fluid;
(3), it filters
After the resulting static placement of ultrasonication liquid of step (2), supernatant is taken, with 0.45 μm -0.80 μm of nylon filter Device filtering, obtains crude extract;
(4), it is concentrated
Step (3) resulting crude extract is concentrated into coarse extraction under conditions of 20-25 DEG C with Rotary Evaporators The 1/20-1/15 of liquid product, obtains concentrate;
(5), separation absorption
Calculate by volume, i.e. step (4) resulting concentrate: deionized water is the ratio of 1:20-30, to obtained by step (4) Concentrate in be added deionized water, stirring is completely dissolved in deionized water to concentrate, obtains concentrate aqueous solution;
The macroreticular resin solid for being added that partial size is 0.30-1.25mm in resulting concentrate aqueous solution is stated then up, is placed in In constant-temperature table, polyphenol is carried out under conditions of being 100-180rpm controlled at 25 DEG C, revolving speed and adsorbs 2-4h, it is more to obtain absorption The macroreticular resin of phenol, filtering, deionized water clean macroreticular resin 3-5 time of adsorbing polyphenols, then controlled at 20-30 DEG C into Row drying obtains the macroreticular resin of dry adsorbing polyphenols;
The macroreticular resin solid that the partial size is 0.30-1.25mm be AB-8, HP-20, FPX-66, SP-850, DM-301 or XAD-2 type, additional amount, by the macroreticular resin solid that partial size is 0.30-1.25mm: 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- The ratio of 30ml calculates, and concentration of volume percent is added into the macroreticular resin of the adsorbing polyphenols of step (5) resulting drying and is The ethanol water of 80-90%, is then placed into constant-temperature table, controlled at 25 DEG C, the item that revolving speed is 100-180rpm Desorption 1-2h is carried out under part, is filtered to remove macroreticular resin, obtains polyphenol stripping liquid;
(7), the resulting polyphenol stripping liquid of step (6) is concentrated into the 1/20-1/15 of polyphenol stripping liquid volume with Rotary Evaporators, Then controlled at being freeze-dried at -50--60 DEG C, the polyphenol powder in passion fruit pericarp is obtained.
2. the extracting method of the polyphenol in a kind of passion fruit pericarp as described in claim 1, it is characterised in that:
It is 60 targeted fine powders that passion fruit pericarp, which is crushed to granularity, in step (1);
Control frequency 40KHz, power 350W, temperature are 30 DEG C and carry out ultrasonic treatment 25min in step (2), obtain at ultrasonic wave Manage liquid;
It is filtered in step (3) with 0.45 μm of nylon filter, obtains crude extract;
The macroreticular resin solid that partial size described in step (5) is 0.30-1.25mm is DM-301, HP-20 or AB-8, described Partial size is the additional amount of the macroreticular resin solid of 0.30-1.25mm, the macroreticular resin solid for being 0.30-1.25mm by partial size: dense The ratio that contracting liquid aqueous solution is 1g:30ml 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) is super In sound-ethyl alcohol collaboration processing, passion fruit fruit peel powder: the ethanol water that concentration of volume percent is 30-80% is 1g:50ml;
In step (5) separation absorption: carrying out polyphenol under conditions of being 180rpm controlled at 25 DEG C, revolving speed and adsorb 4h;
Step (6) separation desorption in controlled at 25 DEG C, revolving speed be 180rpm under conditions of carry out desorption 2h;
Freeze-drying temperature described in step (7) is -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) is super In sound-ethyl alcohol collaboration processing, passion fruit fruit peel powder: the ethanol water that concentration of volume percent is 55% is 1g:50ml.
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