CN104886577B - A kind of preparation method of Lee fruit polyphenol - Google Patents

A kind of preparation method of Lee fruit polyphenol Download PDF

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CN104886577B
CN104886577B CN201510330668.7A CN201510330668A CN104886577B CN 104886577 B CN104886577 B CN 104886577B CN 201510330668 A CN201510330668 A CN 201510330668A CN 104886577 B CN104886577 B CN 104886577B
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lee
fruit
wall material
polyphenol
fruit polyphenol
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CN104886577A (en
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李怡彬
陈君琛
赖谱富
汤葆莎
吴俐
翁敏劼
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Institute of Agricultural Engineering Technology of Fujian Academy of Agricultural Sciences
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Institute of Agricultural Engineering Technology of Fujian Academy of Agricultural Sciences
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    • 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

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Abstract

The invention discloses the multinomial technology such as a kind of preparation method of Lee fruit polyphenol, integrated micro vacuum drying, the extraction of ultrasonic assistant ethanol, macroporous resin adsorption purification, spray drying micro encapsulation, prepares Lee's fruit polyphenol fine powder product.The present invention can reduce polyphenol because losing in production process, reduce energy loss, improve and extract production efficiency, reduce sensitivity of Lee fruit polyphenol product to environment simultaneously, strengthen its storage-stable, improve its water-soluble, increase its flexibility (adaptability) of operation, widen the range of application of Lee's fruit polyphenol.Lee's fruit polyphenol fine powder prepared by the present invention can be applied to food service industry as natural pigment, the Natural antioxidant.

Description

A kind of preparation method of Lee fruit polyphenol
Technical field
The invention belongs to fruit and vegerable deep process technology field, and in particular to a kind of preparation method of Lee fruit polyphenol.
Background technology
Lee(PrunusSpp. it is) Rosaceae cherry, sweet and sour taste is nutritious, deep is liked by consumer Fruit, in China and all over the world has cultivation, is one of important temperate fruit tree.Fujian is the main producing region of China Lee fruit, forever There is Lee such as establishing in large scale Fu-Rong plums, kermes Lee, Flos Rosae Rugosae Lee, double Hua Li fruit on the ground such as Thailand, Fuan, Yongan, Zhaoan, through counting, entirely Plantation Lee's 30 multiaspect mus of fruit are saved, yield is nearly 200,000 tons.
Plum fruit is rich in polyphenols, and polyphenol is a kind of Natural antioxidant, with removing free radical, anti-ageing Always, the effects such as anticancer, blood fat reducing, have broad application prospects in food additive and pharmaceutical sanitary field.But polyphenol is in oxygen The reaction such as easily aoxidize, be polymerized, being condensed under the conditions of gas, illumination, high temperature etc., so as to reduce active effect, it is also possible to cause There is brown stain in food, this limits the storage of polyphenol and application to a certain extent;Additionally, polyphenol is in gastrointestinal disturbances process, many Phenol structure can be destroyed in peracidity gastric juice and intestinal, have impact on its health-care effect.
At present in terms of many phenol extraction separation of Lee's fruits and stability study, Chen Dan etc.(Number of patent application: 201110226278.7)With fresh Fu-Rong plums sarcocarp as raw material, polyphenol is separated using alcohol reflux, HPD-100 macropores are inhaled Attached resin purification, drying under reduced pressure prepare Fu-Rong plums total polyphenols highly finished product;But due to flesh as extracting raw material, ethanol consumption Greatly, and reflux, extract, extraction time longer, while prepare polyphenol fine work be vulnerable to environmental effect occur oxidation cause to preserve Phase is short.Li Ou etc. is compared analysis to the polyphenol content at the positions such as the peel of different cultivars Prunus humilis, sarcocarp, fruit juice(Li Ou etc., Chinese experimental pharmacology of Chinese medical formulae magazine, 2012,22(18):53-56);Li Xueqiang etc. is using ethanol and the list of acetone extraction Prunus humilis peel Rather(Li Xueqiang etc., Sichuan Agricultural University's journal, 2009,27(4):462-465);Wang Hongtao etc. extracts purple leaf using 50% ethanol Plum fruit total polyphenols(Wang Hongtao etc., Henan Agricultural Sciences, 2013,42(10):153-156).It is main at present that Lee fruit extracts polyphenol Using ethanol, acetone and other organic solvent extraction, and using Lee fruit of fresh Lee fruit or hot air drying as raw material is extracted, with fresh fruit it is Raw material, the organic solvent of consumption are big, long, the power consumption with hot air drying Lee fruit as extracting raw material, hot-wind-drying time, and Lee's fruit polyphenol Loss is big;Have not yet to see the report of Lee fruit polyphenol microcapsules and storage-stable.
Content of the invention
It is an object of the invention to provide a kind of preparation method of Lee fruit polyphenol, so as to reduce the loss of Lee fruit polyphenol, efficiently Aldehydes matter is extracted, Lee's fruit polyphenol product storage-stable is improved, products application scope is widened, promotes Lee's fruit natural pigment, day So production application of antioxidant.
For achieving the above object, the present invention is adopted the following technical scheme that:
A kind of preparation method of Lee fruit polyphenol:After fresh Lee fruit is cleaned up, enucleation, section, microwave vacuum drying, powder Broken, ultrasonic assistant ethanol is extracted, and is filtered, concentrated in vacuo, macroporous resin adsorption purification, and eluent is concentrated in vacuo to obtain Lee's fruit polyphenol Extracting solution;Extracting solution is dissolved in preparation microcapsule solution in wall material, is spray-dried and obtains Lee's fruit polyphenol fine powder product.
Described microwave vacuum drying condition be microwave intensity 3W/g ~ 10W/g, vacuum 60kPa ~ 85kPa, temperature 50 C ~ 60 DEG C, drying mode is vacuum dried for batch microwave, i.e. microwave heating 30s, stopping heating 30s, so alternately;Li Guo Piece drying is less than 15% to moisture.
Described ultrasonic assistant ethanol extraction conditions are:Concentration of alcohol is 60vol.% ~ 80vol.%, and material ratio is Lee fruit Powder: ethanol=1g: 20mL, ultrasonic power are 150 ~ 500W, and extraction time is 30 ~ 60min.
Described preparation microcapsule solution is to be slowly added in wall material solution Lee's fruit polyphenol extracting solution as core, warp 8 ~ 20min of homogenizing under 5000~15000rpm speed conditions;The weight ratio of core and wall material is 1: 3 ~ 8, wall material be beta-schardinger dextrin-, Arabic gum and the mixture of maltodextrin, its weight ratio are 1: 0.3 ~ 0.5: 0.6 ~ 1, wall material in wall material solution: water=1g: 4~ 10ml;Emulsifying agent glyceryl monostearate or soybean lecithin is added in wall material, and the addition of emulsifying agent is the 0.2 of wall material weight ~ 0.5%.
The technological parameter of described spray drying is:Charging solid content 10 ~ 25%, inlet temperature are 150 ~ 200 DEG C, 80 ~ 90 DEG C of leaving air temp.
Described Lee fruit is Fu-Rong plums, Flos Rosae Rugosae Lee, kermes Lee, red heart Lee, the one kind in Gentiana triflora.
The remarkable advantage of the present invention is:
(1)Using microwave vacuum drying, reducing Lee's fruit polyphenol oxidase activity, polyphenol is reduced because there is enzyme in production process Promote brown stain and lose, improve Lee's fruit dry materials quality, while drying time can be shortened, improve production efficiency reduces the energy and damages Consumption;
(2)Extracted using ultrasonic assistant, shorten Lee's fruit polyphenol extraction time, improve Lee's fruit polyphenol recovery rate;
(3)Using microcapsule method is spray-dried, Lee's fruit polyphenol is embedded, reduces sensitivity of Lee fruit polyphenol product to environment, Strengthen its storage-stable, while improving water-soluble, increase its flexibility (adaptability) of operation, widen the range of application of Lee's fruit polyphenol, this Outward, Lee fruit polyphenol microcapsules product can discharge activity on demand, and under nonprotected state, bioavailability is not in gastrointestinal to solve polyphenol High problem.
Specific embodiment
After fresh Lee fruit is cleaned up, enucleation, microwave vacuum drying are crushed, and ultrasonic assistant ethanol is extracted, and are filtered, Concentrated in vacuo, macroporous resin adsorption purification, eluent is concentrated in vacuo to obtain Lee's fruit polyphenol extracting solution;Extracting solution dissolves wall material, passes through Micro encapsulation embedding Lee's fruit polyphenol is spray-dried, Lee's fruit polyphenol fine powder product is prepared.Its concrete preparation process is as follows:
(1)Fresh Lee fruit is cleaned up with water, and quick enucleation, section are put into 1% before drying(By weight)In citric acid Color fixative;Lee fruit is Fu-Rong plums, Flos Rosae Rugosae Lee, kermes Lee, red heart Lee or Gentiana triflora;
(2)Lee's chankings after draining uniformly is placed in the material disc of microwave vacuum drying chamber, is carried out microwave vacuum and is done Dry, described microwave vacuum drying condition is microwave intensity 3W/g~10W/g, and vacuum 60kPa ~ 85kPa, temperature range are 50 DEG C~60 DEG C under conditions of be dried, drying mode be batch microwave vacuum drying, i.e. microwave heating 30s, stop heating 30s So alternately;Dried Lee's chankings is crushed to below particle diameter 1mm to moisture less than 15% by the drying of Lee's chankings;
(3)Lee's fruit powder is dissolved with 60% ~ 80% ethanol, ultrasonic assistant is extracted, material ratio is Lee's fruit powder: ethanol=1g: 20mL, ultrasonic power are 150 ~ 500W, and extraction time is 30 ~ 60min, filters to obtain Lee's fruit polyphenolic extract;
(4)Through 50 DEG C of removal ethanol concentrated in vacuo, vacuum is 0.01MPa~0.06MPa to crude extract;HP-20 macropore trees Fat purification Lee's fruit polyphenol, distillating washing resin, 60% ethanol solution desorbing eluting, eluent are concentrated in vacuo to stock solution 30% ~ 60%, Obtain Lee's fruit polyphenol extracting solution;
(5)Lee's fruit polyphenol extracting solution is slowly added in wall material solution as core, through 5000~15000rpm speed conditions Lower high-speed stirred 8 ~ 20min of homogenizing;Core: wall material=1: 3 ~ 8, mixing of the wall material for beta-schardinger dextrin-, arabic gum and maltodextrin Thing, wall material proportioning by weight are beta-schardinger dextrin-: arabic gum: maltodextrin=1: 0.3 ~ 0.5: 0.6 ~ 1, wall material is mixed with water Mass volume ratio by wall material: water is 1g: 4~10mL, and wall material solution is stirred to full and uniform;Add emulsifying agent list hard in wall material Glycerol or soybean lecithin, the addition of emulsifying agent is the 0.2 ~ 0.5% of wall material quality;
(6)The spray-dried equipment of mixed solution is dried, and obtains Lee's fruit polyphenol microcapsules product;Spray drying condition parameter For:Charging solid content 10 ~ 25%, inlet temperature are 150 ~ 200 DEG C, 80 ~ 90 DEG C of leaving air temp.
In order that content of the present invention easily facilitates understanding, with reference to specific embodiment to of the present invention Technical scheme is described further, but the present invention is not limited only to this.
Embodiment 1
(1)Fresh Hibisci Mutabilises plum fruit is cleaned up with water, and quick enucleation, section are put into 1% before drying(By weight)Lemon Color fixative in lemon acid;
(2)Lee's chankings after draining uniformly is placed in the material disc of microwave vacuum drying chamber, is carried out microwave vacuum and is done Dry, described microwave vacuum drying condition is microwave intensity 3W/g, vacuum 60kPa, and temperature range is to enter under conditions of 50 DEG C Row drying, drying mode are vacuum dried for batch microwave, i.e. microwave heating 30s, stopping heating 30s are so alternately;Li Guo Dried Lee's chankings is crushed to below particle diameter 1mm to moisture less than 15% by piece drying;
(3)Lee's fruit powder is dissolved with 60% ethanol, ultrasonic assistant is extracted, material ratio is Lee's fruit powder: ethanol=1g: 20 mL, Ultrasonic power is 150W, and extraction time is 60min, filters to obtain Lee's fruit polyphenolic extract;
(4)Through 50 DEG C of removal ethanol concentrated in vacuo, vacuum is 0.01MPa to crude extract;HP-20 purification by macroporous resin Lee fruit Polyphenol, distillating washing resin, 60% ethanol solution desorbing eluting, eluent are concentrated in vacuo to stock solution 30%, obtain many phenol extractions of Lee fruit Liquid;
(5)Lee's fruit polyphenol extracting solution is slowly added in wall material solution as core, through high speed under 15000rpm speed conditions Stirring homogenizing 8min;Core: wall material=1: 8, mixture of the wall material for beta-schardinger dextrin-, arabic gum and maltodextrin, wall material is by weight Gauge proportioning is beta-schardinger dextrin-: arabic gum: maltodextrin=1: 0.3: 0.6, the mass volume ratio that wall material is mixed with water is by wall material : water is 1g: 4mL, and wall material solution is stirred to full and uniform;Emulsifying agent glyceryl monostearate is added in wall material, addition is wall The 0.2% of material amount;
(6)The spray-dried equipment of mixed solution is dried, and obtains Lee's fruit polyphenol microcapsules product;Spray drying condition parameter For:Charging solid content 10%, inlet temperature are 200 DEG C, 90 DEG C of leaving air temp.
Embodiment 2
(1)Fresh Flos Rosae Rugosae plum fruit is cleaned up with water, and quick enucleation, section are put into 1% before drying(By weight)Lemon Color fixative in lemon acid;
(2)Lee's chankings after draining uniformly is placed in the material disc of microwave vacuum drying chamber, is carried out microwave vacuum and is done Dry, described microwave vacuum drying condition is microwave intensity 10W/g, vacuum 85kPa, and temperature range is to enter under conditions of 60 DEG C Row drying, drying mode are vacuum dried for batch microwave, i.e. microwave heating 30s, stopping heating 30s are so alternately;Li Guo Dried Lee's chankings is crushed to below particle diameter 1mm to moisture less than 15% by piece drying;
(3)Lee's fruit powder is dissolved with 80% ethanol, ultrasonic assistant is extracted, material ratio is Lee's fruit powder: ethanol=1g: 20 mL, Ultrasonic power is 500W, and extraction time is 30min, filters to obtain Lee's fruit polyphenolic extract;
(4)Through 50 DEG C of removal ethanol concentrated in vacuo, vacuum is 0.06MPa to crude extract;HP-20 purification by macroporous resin Lee fruit Polyphenol, distillating washing resin, 60% ethanol solution desorbing eluting, eluent are concentrated in vacuo to stock solution 60%, obtain many phenol extractions of Lee fruit Liquid;
(5)Lee's fruit polyphenol extracting solution is slowly added in wall material solution as core, through high-speed stirring under 5000rpm speed conditions Mix homogenizing 20min;Core: wall material=1: 3, mixture of the wall material for beta-schardinger dextrin-, arabic gum and maltodextrin, wall material is by weight Gauge proportioning is beta-schardinger dextrin-: arabic gum: maltodextrin=1: 0.5: 1, the mass volume ratio that wall material is mixed with water is by wall material: Water is 1g: 10mL, and wall material solution is stirred to full and uniform;Emulsifying agent soybean lecithin, the addition of emulsifying agent is added in wall material For wall material quality 0.5%;
(6)The spray-dried equipment of mixed solution is dried, and obtains Lee's fruit polyphenol microcapsules product;Spray drying condition parameter For:Charging solid content 25%, inlet temperature are 150 DEG C, 80 DEG C of leaving air temp.
Embodiment 3
(1)Fresh kermes plum fruit is cleaned up with water, and quick enucleation, section are put into 1% before drying(By weight)Lemon Color fixative in lemon acid;
(2)Lee's chankings after draining uniformly is placed in the material disc of microwave vacuum drying chamber, is carried out microwave vacuum and is done Dry, described microwave vacuum drying condition is microwave intensity 5W/g, vacuum 75kPa, and temperature range is to enter under conditions of 50 DEG C Row drying, drying mode are vacuum dried for batch microwave, i.e. microwave heating 30s, stopping heating 30s are so alternately;Li Guo Dried Lee's chankings is crushed to below particle diameter 1mm to moisture less than 15% by piece drying;
(3)Lee's fruit powder is dissolved with 70% ethanol, ultrasonic assistant is extracted, material ratio is Lee's fruit powder: ethanol=1g: 20 mL, Ultrasonic power is 300W, and extraction time is 40min, filters to obtain Lee's fruit polyphenolic extract;
(4)Through 50 DEG C of removal ethanol concentrated in vacuo, vacuum is 0.03MPa to crude extract;HP-20 purification by macroporous resin Lee fruit Polyphenol, distillating washing resin, 60% ethanol solution desorbing eluting, eluent are concentrated in vacuo to stock solution 50%, obtain many phenol extractions of Lee fruit Liquid;
(5)Lee's fruit polyphenol extracting solution is slowly added in wall material solution as core, through high speed under 10000rpm speed conditions Stirring homogenizing 10min;Core: wall material=1: 5, mixture of the wall material for beta-schardinger dextrin-, arabic gum and maltodextrin, wall material are pressed Weight meter proportioning is beta-schardinger dextrin-: arabic gum: maltodextrin=1: 0.4: 0.8, the mass volume ratio that wall material is mixed with water is by wall Material: water is 1g: 6mL, wall material solution are stirred to full and uniform;Emulsifying agent glyceryl monostearate is added in wall material, emulsifying agent Addition for wall material quality 0.3%;
(6)The spray-dried equipment of mixed solution is dried, and obtains Lee's fruit polyphenol microcapsules product;Spray drying condition parameter For:Charging solid content 15%, inlet temperature are 180 DEG C, 85 DEG C of leaving air temp.
Using said method, Lee's fruit polyphenol extracting solution extract yield up to 40mgGAE/g dries more than;Prepared Lee Fruit polyphenol product removes DPPH free radical IC50Less than 60 μ g/mL, ABTS is removed+Free radical IC50It is less than 100 μ g/mL.Produce Product are packed using foil sealing bag, and at 25 DEG C, at 10 DEG C, the shelf-life was up to 360 days up to 200 days the shelf-life.Quality standard and property Energy parameter is shown in Tables 1 and 2.
1 organoleptic requirements of table
2 physical and chemical index of table
The foregoing is only presently preferred embodiments of the present invention, all impartial changes that is done according to scope of the present invention patent with Modification, should all belong to the covering scope of the present invention.

Claims (4)

1. a kind of preparation method of Lee fruit polyphenol, it is characterised in that:After fresh Lee fruit is cleaned up, enucleation, section, microwave Vacuum drying, crushes, and ultrasonic assistant ethanol is extracted, and filters, and concentrated in vacuo, macroporous resin adsorption purification, eluent vacuum are dense Contract to obtain Lee's fruit polyphenol extracting solution;Extracting solution is dissolved in preparation microcapsule solution in wall material, is spray-dried and obtains Lee's fruit polyphenol fine powder Product;Described preparation microcapsule solution is to be slowly added in wall material solution Lee's fruit polyphenol extracting solution as core, warp Homogenizing 8min ~ 20min under 5000rpm~15000rpm speed conditions;The weight ratio of core and wall material is 1: 3 ~ 8, wall material be β- The mixture of cyclodextrin, arabic gum and maltodextrin, its weight ratio are 1: 0.3 ~ 0.5: 0.6 ~ 1, wall material in wall material solution: water =1g: 4~10mL;Emulsifying agent glyceryl monostearate or soybean lecithin is added in wall material, and the addition of emulsifying agent is wall material weight The 0.2% ~ 0.5% of amount;Described microwave vacuum drying condition be microwave intensity 3W/g ~ 10W/g, vacuum 60kPa ~ 85kPa, Temperature 50 C ~ 60 DEG C, drying mode are vacuum dried for batch microwave, i.e. microwave heating 30s, stopping heating 30s, are so alternately entered OK;The drying of Lee's chankings is less than 15% to moisture.
2. the preparation method of Lee fruit polyphenol according to claim 1, it is characterised in that:Described ultrasonic assistant ethanol Extraction conditions are:Concentration of alcohol is 60vol.% ~ 80vol.%, and material ratio is Lee's fruit powder: ethanol=1g: 20mL, and ultrasonic power is 150W ~ 500W, extraction time are 30min ~ 60min.
3. the preparation method of Lee fruit polyphenol according to claim 1, it is characterised in that:The technique of described spray drying Conditional parameter is:Charging solid content 10% ~ 25%, inlet temperature are 150 DEG C ~ 200 DEG C, 80 DEG C ~ 90 DEG C of leaving air temp.
4. the preparation method of Lee fruit polyphenol according to claim 1, it is characterised in that:Described Lee fruit is Fu-Rong plums, rose Rare Lee, kermes Lee, red heart Lee, the one kind in Gentiana triflora.
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