CN106108019A - A kind of method of total flavones in microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck - Google Patents

A kind of method of total flavones in microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck Download PDF

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Publication number
CN106108019A
CN106108019A CN201610528124.6A CN201610528124A CN106108019A CN 106108019 A CN106108019 A CN 106108019A CN 201610528124 A CN201610528124 A CN 201610528124A CN 106108019 A CN106108019 A CN 106108019A
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China
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microwave
assisted
extraction
peel
pericarpium citri
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Inventor
张秀玲
王晓君
陈少华
柳晓晨
于鹏
王炬
闫安
高宁
李凤凤
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Northeast Agricultural University
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Northeast Agricultural University
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463Organic compounds; Microorganisms; Enzymes
    • A23L3/3544Organic compounds containing hetero rings
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention discloses a kind of method of total flavones in microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck, belong to the extractive technique field of agricultural byproducts effective ingredient.It concretely comprises the following steps: orange peel cleans, dry, pulverized 60 mesh sieves after, first carry out microwave-assisted process after obtaining Pericarpium Citri junoris powder, its solid-liquid ratio is 1:20, and concentration of alcohol is 70% 73%, and microwave power is 240w, and the microwave time is 60s, and extraction time is 3 times;The sample processed through microwave-assisted extracts further by adding compound enzyme, and sample is cooled to pH regulator to 5.0 after room temperature, adds cellulase and the pectase of 4% 5%, extracts 1 1.2h, complete the whole leaching process of flavedo flavone under conditions of 50 DEG C;Solution after filtration obtains flavedo flavone goods through rotary evaporation, purification by macroporous resin, lyophilization;The general flavone content that the present invention extracts from peel of Citrus sinensis Osbeck reaches 39.5mg/g, simple to operate, and extraction ratio is high, good product quality.

Description

A kind of method of total flavones in microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck
Technical field
In a kind of microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck, the method for total flavones, belongs to the extraction of agricultural byproducts effective ingredient Technical field, is specifically related to a kind of microwave combined-enzyme method and extracts the treatment technology of flavone, final obtain content reach 39.5mg/g with On total flavones goods, for flavone compound extracting method provide foundation.
Background technology
Citrus sinensis Osbeck (Citrus sinensis Osbeck), Rutaceae Citrus, aiphyllium, be China so that the world important Fruit resource.Often edible can with blood fat reducing, skin care, the effect such as anticancer, have become as the world eat raw in kind " mandarin orange it King ".Therefore, Citrus sinensis Osbeck industry has good application prospect and the highest economic benefit.But, the practical efficiency of peel of Citrus sinensis Osbeck is relatively Low, most of peel of Citrus sinensis Osbeck are unprocessed to be directly dropped, and causes the most serious environmental pollution and the biggest wasting of resources, therefore, How to better profit from peel of Citrus sinensis Osbeck, it may be assumed that turned waste into wealth, have become as problem of concern.At present, the most from Citrus Its effective ingredient extracted in skin, is applied to the fields such as chemistry, dyestuff, varnish and cosmetics, and develop pectin, essential oil, The products such as dietary fiber, achieve good economic benefit.
Containing abundant natural flavone compounds in Citrus sinensis Osbeck peel, flavone compound is most in yellow or faint yellow, Therefore flavone it is referred to as.It is a class low-molecular-weight natural plant composition, is often combined into glycosides with free state or with sugar in plant Presented in, there is preferable water solublity, can be dissolved in part organic solvent simultaneously, such as methanol, ethanol, ethyl acetate etc., Show certain acidity, be soluble in alkali, but be not readily dissolved in acid.Flavone compound, in addition to having important Nutrition, also has There are antibacterial, antioxidation, suppression erythrocyte agglutination and the biological activity such as sedimentation and antimutagenic.
Extracting method for flavone compound mainly has alcohol extraction, microwave-assisted extraction, supercritical fluid to extract Follow the example of.Alcohol extraction follows the example of that to have process simple, workable, it is to avoid heating, the advantage of consuming little energy, but extracting cycle Length, solvent consumption are bigger;Supercritical fluid extraction has that rate of extraction is fast, efficiency is high, simple to operate, reduce energy consumption, nothing The advantages such as machine dissolvent residual, but high to equipment requirements, it is unfavorable for industrialized production.Such as, patent " peel of Citrus reticulata Blanco total flavones Microwave auxiliary extracting method " (publication number: CN104306501A, publication date on 01 28th, 2015) to disclose a kind of peel of Citrus reticulata Blanco total The microwave auxiliary extracting method of flavone, the method technique is simple, low cost, but simple use microwave extraction power is relatively big, Time is longer, easily makes the effective ingredient of flavone be destroyed;Patent " method preparing tangeritin from peel of Citrus reticulata Blanco " is (open Number: CN1810819A, publication date on 08 02nd, 2006) disclose a kind of method preparing tangeritin in peel of Citrus reticulata Blanco, this method The method using backflow prepares tangeritin, higher to equipment requirements, and needs concentration of alcohol bigger so that energy waste is relatively For seriously.In recent years, zymotechnic quickly grows, and utilizing the effective ingredient in enzyme auxiliary extraction natural materials is a kind of efficient, ring The emerging technology protected, it is gentle that this method has extraction conditions, and the response rate is improved and can effectively protect the function of functional component Characteristic, and the advantage such as low cost, safety.Microwave field is mainly derived from microwave to carefully to the assosting effect that flavone compound extracts The biological effect of after birth: make cell interior temperature raise, pressure increases, when pressure exceedes the ability to bear of cell wall, cell Wall ruptures, and the chromocor compound being positioned at cell interior discharges from cell, is dissolved by the solvent of surrounding, and therefore its heat passes It is consistent for passing the direction with quality transmission, and this contributes to the Fast Stripping of flavone compound.Additionally, the Huang that microwave is to polarity Ketone compounds can produce heat effect and make temperature raise rapidly, and diffusion coefficient increases, and the also liquid film at the surface of solids produces Certain microcosmic " disturbance " so that it is thinning, decreases the resistance of flavonoid diffusion process, thus can improve extraction process on the whole Mass transfer rate and effect, serve the effect of assisted extraction.
The present invention utilizes microwave-assisted combined-enzyme method to extract the chromocor compound in Pericarpium Citri junoris, and this product is a kind of novel food Product additive and antistaling agent, functional character is strengthened, and takes full advantage of Pericarpium Citri junoris garbage, it is achieved turn waste into wealth, and increases The added value of Pericarpium Citri junoris, has considerable economic worth.
Summary of the invention
Technical problem: the extracting method for flavone compound mainly has alcohol extraction, ultrasonic assistant extraction method, surpasses Supercritical fluid extraction method etc..Extracting cycle length, solvent consumption that alcohol extraction is followed the example of are bigger;Supercritical fluid extraction is to equipment Require high;Simple microwave extraction rate is relatively low.
The purpose of the present invention: be for extracting flavonoids during disadvantages mentioned above and Pericarpium Citri junoris waste present situation, exploitation one The method of total flavones in microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck, the method is not only simple to equipment requirements, shortens extraction time, Improve extracting flavonoids rate, and Pericarpium Citri junoris is made full use of, add added value.
Technical scheme: a kind of method of total flavones in microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck, specifically includes following steps:
(1) pretreatment of raw material: fresh Pericarpium Citri junoris is cleaned, dries and put into the pulverizing of omnipotent high speed disintegrator, by 60 mesh sub-sieves Obtain Pericarpium Citri junoris powder standby;
(2) microwave-assisted processes: Pericarpium Citri junoris and the ethanol that concentration is 70 73% are mixed according to the ratio of weight ratio 1:17 1:20 Closing, place in triangular flask, extract 60s, extract 3 times under conditions of microwave power 240w, time interval is 10min;
(3) adding multiplex-enzyme extraction: after the sample that step (2) microwave-assisted processes is cooled to room temperature, regulation pH value is 5.0, to Wherein add cellulase and the pectase of 4% 5%, under the conditions of bath temperature is 50 53 DEG C, extracts 1-1.2h;
(4) post processing: after the operations such as the filtration of step (3) gained extracting solution, rotary evaporation, purification by macroporous resin and lyophilization Obtain flavone goods.
Beneficial effects of the present invention:
1. the extraction raw material that the present invention takes is peel of Citrus sinensis Osbeck, low price, and raw material sources are unrestricted, it is adaptable to large-scale production, Using microwave-assisted combined-enzyme method to extract system and substitute the methods such as conventional methanol, acetone equal solvent and supersound extraction, equipment is wanted Ask simple, improve extraction ratio, reduce production cost, avoid environmental pollution simultaneously.
2. the pretreatment of raw material in the present invention, uses high speed disintegrator to pulverize, and the standby Pericarpium Citri junoris powder obtained can be more preferable It is easy to the extraction of follow-up flavone, indirectly improves extraction efficiency.
3. use microwave-assisted combined-enzyme method to extract, substantially reduce extraction time, when can avoid long compared with tradition alcohol extracting method Between heat, destroy flavones ingredient sensitive to long-time heating in Pericarpium Citri junoris, extraction efficiency is big, and productivity is up to 39.5mg/g, relatively Traditional ethanol extraction improves 4.3 times, and the time shortens 3 times;More single microwave digestion method improves 2.18 times;Extraction ratio is relatively Single cellulase extraction improves 1.33 times, and the time shortens 1.7 times.The extracting flavonoids process route that method is carried out accordingly Farthest maintain flavone functional component, low cost, high efficiency.
Detailed description of the invention
Embodiment 1: by fresh Pericarpium Citri junoris clean, dry after put into omnipotent high speed disintegrator pulverize, by 60 mesh sub-sieves Obtain Pericarpium Citri junoris powder standby;Take 2g Pericarpium Citri junoris powder to be positioned in triangular flask, add the ethanol of 70% in the ratio of 1:20, at microwave power For extracting 60s under conditions of 240w, extracting 3 times, time interval is 10min;Regulate pH to 5.0 after being cooled to room temperature, add 4% Cellulase and pectase, under conditions of bath temperature is 50 DEG C extract 1h;Then extracting solution through filtration, rotary evaporation, Flavone goods are obtained after the operation such as purification by macroporous resin and lyophilization;After testing, the general flavone content that the method prepares is 39.5mg/g。
Embodiment 2: by fresh Pericarpium Citri junoris clean, dry after put into omnipotent high speed disintegrator pulverize, by 60 mesh sub-sieves Obtain Pericarpium Citri junoris powder standby;Take 2g Pericarpium Citri junoris powder to be positioned in triangular flask, add the ethanol of 73% in the ratio of 1:19, at microwave power For extracting 60s under conditions of 240w, extracting 3 times, time interval is 10min;Regulate pH to 5.0 after being cooled to room temperature, add 5% Cellulase and pectase, under conditions of bath temperature is 52 DEG C extract 1.2h;Then extracting solution steams through filtering, rotating Send out, obtain flavone goods after the operation such as purification by macroporous resin and lyophilization;After testing, the general flavone content that the method prepares is 40.3mg/g。
Embodiment 3: by fresh Pericarpium Citri junoris clean, dry after put into omnipotent high speed disintegrator pulverize, by 60 mesh sub-sieves Obtain Pericarpium Citri junoris powder standby;Take 2g Pericarpium Citri junoris powder to be positioned in triangular flask, add the ethanol of 71% in the ratio of 1:20, at microwave power For extracting 60s under conditions of 240w, extracting 3 times, time interval is 10min;Regulate pH to 5.0 after being cooled to room temperature, add 4% Cellulase and pectase, under conditions of bath temperature is 53 DEG C extract 1.1h;Then extracting solution steams through filtering, rotating Send out, obtain flavone goods after the operation such as purification by macroporous resin and lyophilization;After testing, the general flavone content that the method prepares is 39.8mg/g。
The above three kinds of embodiment is for only for ease of and understands the example lifted, it is noted that for this technology For the technical staff in field, under the premise without departing from the principles of the invention, can according to technical scheme and preferably Some improvement are made in the description of embodiment, and these improvement also should belong to protection scope of the present invention.

Claims (4)

1. a method for total flavones in microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck, its feature is first carried out after being to pulverize Pericarpium Citri junoris Microwave-assisted processes, and after being cooled to room temperature, pH is adjusted to 5.0, is added to compound enzyme cellulase, pectase to orange Total flavones in skin continues to extract, and the solution after filtration is obtained by rotary evaporation, purification by macroporous resin and cryodesiccated method To flavone goods, the extracting flavonoids finally given reaches 39.5mg/g.
The extraction process of total flavones in Pericarpium Citri junoris the most according to claim 1, it is characterised in that specifically include following steps:
(1) pretreatment of raw material: fresh Pericarpium Citri junoris is cleaned, dries and put into the pulverizing of omnipotent high speed disintegrator, by 60 mesh sub-sieves Obtain Pericarpium Citri junoris powder standby;
(2) microwave-assisted processes: Pericarpium Citri junoris and the ethanol that concentration is 70 73% is mixed according to the ratio of 1:17 1:20, places In triangular flask, under conditions of microwave power 240w, extract 60s, extract 3 times;
(3) adding multiplex-enzyme extraction: after the sample that step (2) microwave-assisted processes is cooled to room temperature, regulation pH value is 5.0, to Wherein add compound enzyme cellulase and pectase, under the conditions of 50 53 DEG C, extract 1-1.2h;
(4) post processing: after the operations such as the filtration of step (3) gained extracting solution, rotary evaporation, purification by macroporous resin and lyophilization Obtain flavone goods.
The most according to claim 1 or claim 2, the method for total flavones, its feature in a kind of microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck Being, the time interval of microwave extraction is 10min.
The most according to claim 1 or claim 2, the method for total flavones, its feature in a kind of microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck Being, the ratio of cellulase and pectase is 3:2, and the addition of compound enzyme is 4% 5%, and mode of heating is water-bath vibration Formula heats.
CN201610528124.6A 2016-07-06 2016-07-06 A kind of method of total flavones in microwave-assisted multiplex-enzyme extraction peel of Citrus sinensis Osbeck Pending CN106108019A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106728213A (en) * 2017-04-06 2017-05-31 广州市嘛咪食品有限公司 A kind of dried orange peel extracts and its preparation method and application
CN107232264A (en) * 2017-07-24 2017-10-10 百色学院 A kind of fragrant citrus cake and preparation method thereof
CN111296838A (en) * 2020-02-28 2020-06-19 西昌市正中食品有限公司 Preparation process of tartary buckwheat nutritional extract rich in flavone

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CN102210472A (en) * 2010-04-07 2011-10-12 江南大学 Method for extracting flavone compounds from granatum
CN104173438A (en) * 2014-09-05 2014-12-03 南京泽朗生物科技有限公司 Preparation method of general flavone of purple perilla

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106728213A (en) * 2017-04-06 2017-05-31 广州市嘛咪食品有限公司 A kind of dried orange peel extracts and its preparation method and application
CN106728213B (en) * 2017-04-06 2020-08-07 广东大汉三墩食品科技有限公司 Dried orange peel extract and preparation method and application thereof
CN107232264A (en) * 2017-07-24 2017-10-10 百色学院 A kind of fragrant citrus cake and preparation method thereof
CN111296838A (en) * 2020-02-28 2020-06-19 西昌市正中食品有限公司 Preparation process of tartary buckwheat nutritional extract rich in flavone

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Application publication date: 20161116