CN106753785A - A kind of Preparation method and use of phytic acid water-in-oil microemulsion - Google Patents

A kind of Preparation method and use of phytic acid water-in-oil microemulsion Download PDF

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Publication number
CN106753785A
CN106753785A CN201611231056.3A CN201611231056A CN106753785A CN 106753785 A CN106753785 A CN 106753785A CN 201611231056 A CN201611231056 A CN 201611231056A CN 106753785 A CN106753785 A CN 106753785A
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phytic acid
oil
aqueous solution
water
preparation
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沙如意
毛建卫
王少林
蔡成岗
汪文星
吴冬阳
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Zhejiang Lover Health Science and Technology Development Co Ltd
Zhejiang University of Science and Technology ZUST
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Zhejiang Lover Health Science and Technology Development Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B5/00Preserving by using additives, e.g. anti-oxidants
    • C11B5/0071Preserving by using additives, e.g. anti-oxidants containing halogens, sulfur or phosphorus

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Edible Oils And Fats (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention belongs to food additives and dispensing exploitation and applied technical field, more particularly to a kind of Preparation method and use of phytic acid water-in-oil microemulsion.The preparation method of the phytic acid water-in-oil microemulsion liquid product is:Edible oil, surfactant and cosurfactant are mixed into the oily mixed phase of composition or edible oil and surfactant are mixed into the oily mixed phase of composition, the mixture of the phytic acid aqueous solution or the phytic acid aqueous solution and cosurfactant composition is added dropwise in oily mixed phase under stirring, until the conductivity variations rate of solution is minimum, transparent or semitransparent phytic acid water-in-oil microemulsion is spontaneously formed.Phytic acid is applied to the present invention preparation of water-in-oil microemulsion liquid product, preparation method is simple, energy consumption is low, the phytic acid water-in-oil microemulsion product of preparation can be used in oil-soluble product as natural, the industry such as including food, medicine, cosmetics, has expanded range of application of the phytic acid as water-soluble natural antioxidant.

Description

A kind of Preparation method and use of phytic acid water-in-oil microemulsion
Technical field
The invention belongs to food additives and dispensing exploitation and applied technical field, more particularly to a kind of phytic acid Water-In-Oil is micro- The Preparation method and use of emulsion.
Background technology
Edible oil or the food containing animal fat and vegetable oil are in processing and storage, if long-term be subject to sky The influence of the factors such as gas, daylight, temperature, moisture, metal ion and enzyme, causes and contains unrighted acid, the grease in food Component will occur slow oxidation and go bad, and be mainly shown as becoming sour for grease.In spoiled by rancid oil or fat, oxidation deterioration or decomposition Primary oxidation thing, such as such as hydroperoxides, and suboxide, aldehyde, ketone, alcohol etc. are produced in course of reaction.These material meetings The local flavor of grease is significantly affected, and the noxious material that Oxidation of Fat and Oils is produced simultaneously is difficult in human body metabolism, can influence biology The organs such as body function, induced renal damage, liver.
In order to delay oxidative rancidity, decomposition reaction of grease etc. in the link such as the food processing containing grease and storage, Keep the freshness containing fatty foods and extend storage phase, it is often necessary to add a certain amount of anti-in grease or containing fatty foods Oxidant.The antioxidant of oil-control oxidation is broadly divided into artificial synthesized antioxidant and natural.Conventional people Work synthetized oxidation preventive agent butylated hydroxy anisole (BHA), dibutyl hydroxy toluene (BHT), TBHQ (TBHQ) etc. Widely used in oil prodution industry, however caused a disease there are some researches show such artificial synthesized antioxidant has, teratogenesis and carcinogenic etc. Side effect, therefore natural causes the concern of people.
Phytic acid is primarily present in the seed of most plants, is existed with the Multiple salts forms of calcium, magnesium, potassium, agricultural byproducts depth Processing byproduct such as rice bran, corn pulp waste water is medium also to contain substantial amounts of phytic acid.Phytic acid, can be with by strong metal chelation abilities Weaken catalysed oxidn of the metal ion for grease, especially suppress the Oxidation of Fat and Oils reaction of iron catalysis.But naturally carry The phytic acid for taking can only be dissolved in water, and oil-soluble is poor, so being less susceptible to be added in grease or in oil-containing food as antioxygen Agent, limits its extensive use as antioxidant in the food industry.There are many researchs to show that phytic acid can significantly prolong The oxidation of slow vegetative grease, such as rapeseed oil, soybean oil, peanut oil, lard etc., however, in existing research report, Phytic acid is that its solubility property is poor in being added to grease or oil-containing food with water miscible material, or by means of high energy consumption High speed shear mode is added, and the grease for obtaining is emulsion, and transparency is not high, influences the exterior quality of grease;Or directly add It is added in edible oil and fat, but layering is easier after standing, therefore, there is inventor (CN101390641) to be changed phytic acid Property be used for the anti-oxidant of grease into oil-soluble phytic acid amino-acid ester salt, but modified phytic acid amino-acid ester salt and exclude In the use list of food additives.
Microemulsion is to be in by surfactant, cosurfactant, oil phase and the equal Thermodynamically stable for constituting of water, outward appearance Transparent or semitransparent, isotropic homogeneous dispersion system.The Dispersed Phase Size of microemulsion is small and uniform, and with good steady Qualitative and dispersing characteristic, can spontaneously form.Water insoluble oil soluble material is wrapped up using oil-in-water microemulsion, Strengthen its solubility in water-soluble medium;It is equally possible that using water in oil microemulsion by insoluble in oily material It is well dispersed in oil phase.Therefore, between the good antioxidant effect of natural phytic acid and oily insoluble feature, the present invention is with edible Oil prepares the water-in-oil microemulsion liquid product of phytic acid as oil phase, so as to be disperseed, strengthens it in grease or containing in fatty foods Solubility, for replace artificial synthesized antioxidant.
The content of the invention
The present invention be just directed to prior art by water-soluble phytic acid be used for oil-soluble system solubility it is smaller, fail fully The deficiency of phytic acid antioxidant effect is played, there is provided a kind of preparation method of phytic acid water-in-oil microemulsion, by phytic acid water-in-oil microemulsion Liquid is used for animals and plants edible oil and fat or the antioxidant containing vegetable and animals oils fat foods.
The present invention solve the technical scheme that is used of above-mentioned technical problem for:A kind of preparation side of phytic acid water-in-oil microemulsion Method, comprises the following steps
1) edible oil, surfactant and cosurfactant are mixed into the oily mixed phase of composition or edible oil and surface The oily mixed phase of activating agent mixing composition;
2) the phytic acid aqueous solution is added dropwise to step 1 under stirring) in edible oil, surfactant and help surface Until the conductivity variations rate of solution is minimum in the oily mixed phase of activating agent mixing composition, transparent or semitransparent plant is spontaneously formed Sour water-in-oil microemulsion;Or the mixture that the phytic acid aqueous solution and cosurfactant are constituted is added dropwise under stirring Step 1) in obtained oily mixed phase, until the conductivity variations rate of solution is minimum, spontaneously form transparent or semitransparent phytic acid Water-in-oil microemulsion.
Preferably, the edible oil is rapeseed oil, peanut oil, soybean oil, sesame oil, linseed oil, olive oil, corn Oil, sunflower oil, lard, butter, one or more in fish oil, edible oil quality used is phytic acid water-in-oil microemulsion matter The 70~80% of amount.
Preferably, the surfactant is polysorbas20 (polyoxyethylene sorbitan monolaurate), polysorbate40 (polyoxy Ethene sorbitan monopalmitate), polysorbate60 (polyoxyethylene sorbitan monostearate), Tween 80 (polyoxyethylene Sorbitan mono-oleic acid ester), this disk 20 (sorbitanmonolaureate), sucrose fatty ester, rhamnolipid, in lecithin One or more in, surfactant qualities used are the 10~20% of phytic acid water-in-oil microemulsion quality.
Preferably, the cosurfactant is ethanol, glycerine, one or more in n-butanol, and used helps table Face activating agent quality is the 5~10% of phytic acid water-in-oil microemulsion quality.
Preferably, the oily mixed phase of the edible oil, surfactant and cosurfactant mixing composition, is 20~50 At DEG C, first surfactant and cosurfactant are mixed, then under the conditions of speed of agitator is 100~400rpm, added To in edible oil.
Preferably, the edible oil and the oily mixed phase of surfactant mixing composition, are at 20~50 DEG C, to turn in stirring Speed is under the conditions of 100~400rpm, surfactant to be added in edible oil.
Preferably, the mass concentration of phytic acid is 1~10% in the phytic acid aqueous solution, and phytic acid aqueous solution pH=3~10 add Plus phytic acid aqueous solution quality for phytic acid water-in-oil microemulsion quality 5~10%.
Preferably, the phytic acid aqueous solution is added dropwise to step 1 under stirring) in obtained oily mixed phase, It is that at 20~50 DEG C, by the phytic acid aqueous solution by peristaltic pump or micro-injection pump, the inlet pressure for adjusting pump is 1-3 air Pressure, drop outlets flow is 50~100 drops/min, and at 20~50 DEG C, speed of agitator is 100~400rpm, is added to oily mixing Xiang Zhong.
Preferably, the mixture of the phytic acid aqueous solution and cosurfactant composition is added dropwise under stirring Step 1) in obtained oily mixed phase, be the mixing for constituting the phytic acid aqueous solution and cosurfactant at 20~50 DEG C By peristaltic pump or micro-injection pump, the inlet pressure for adjusting pump is 1-3 atmospheric pressure to thing, and drop outlets flow is 50~100 Drop/min, at 20~50 DEG C, speed of agitator is 100~400rpm, is added in oily mixed phase.
Preferably, the conductivity variations rate is minimum, refers to by the phytic acid aqueous solution or the phytic acid aqueous solution and to help surface The mixture of activating agent composition is added to step 1) in obtained oily mixed phase when, the record phytic acid aqueous solution or phytic acid are water-soluble Liquid and cosurfactant composition mixture addition, and using conductivity meter monitor different additions when solution conductance Rate, calculates conductivity variations rate, is minimum rate of change when rate of change is intended to 0.
Preferably, the transparent or semitransparent phytic acid water-in-oil microemulsion absorbance is between 0~0.2, under State method measurement:Take a small amount of phytic acid water-in-oil microemulsion to be placed in cuvette, mensuration absorbance under 650nm, made with deionized water It is blank, absorbance is between 0~0.2.
The transparent or semitransparent phytic acid water-in-oil microemulsion particle size range between 20~400nm, by following sides Method is measured:Transparent or semitransparent phytic acid water-in-oil microemulsion being scattered in after eat accordingly in oil medium, particle size range exists Between 20~400nm.
The preparation method of the phytic acid aqueous solution is comprised the following steps:
(1) rice bran was crushed into 40~60 mesh sieves, it is dry after solvent flashing using petroleum ether or n-hexane degreasing 3 times To defatted rice bran powder;
(2) by defatted rice bran powder and deionized water according to mass ratio 1:5~15 mixing, pH value is 6~8, using retention point Son amount synchronously extracts rice bran protein matter therein and rice bran polysaccharide in the flat board filter membrane or hollow fiber filter membrane of 5kDa~100kDa, Rice bran residue is collected after filtering;
(3) by the rice bran residue of gained using the acetic acid aqueous solution of 1~3wt% for solvent is extracted, stir at room temperature 1~3h, 6000r/min centrifugation 30min are extracted, supernatant is collected;Gained supernatant is passed through into anion exchange resin adsorption layer Analysis, and using the sodium-chloride water solution wash-out of 0.1~1mol/L, eluent is collected, through cationic ion-exchange resin desalination, after concentration Obtain the phytic acid aqueous solution of 30~50wt%.
A kind of above-mentioned phytic acid water-in-oil microemulsion liquid product is as edible oil or the purposes containing fatty foods antioxidant.
Compared with prior art, the present invention has following good effect:
1st, phytic acid water-in-oil microemulsion liquid product prepared by the present invention can in edible oil or containing fatty foods in it is uniform, stably Dispersion, overcomes natural phytic acid undissolvable problem in oil-soluble medium, is effectively improved water-soluble phytic acid edible Antioxidant effect in the oil-soluble food such as oil, and being easily added in oil-soluble food, expand its Range of application in food additives, has broad application prospects;
2nd, phytic acid water-in-oil microemulsion liquid product prepared by the present invention is transparent or semitransparent system, and particle diameter is small, stability Get well, and placement will not also be layered long;
3rd, phytic acid water-in-oil microemulsion liquid product prepared by the present invention is added in vegetable fat, with same amount phytic acid Under the conditions of, phytic acid water-in-oil microemulsion has stronger antioxidant effect;And BHT, TBHQ, vitamin E with Isodose Deng with suitable Anti-oxidant effect.
Brief description of the drawings
Fig. 1 is different antioxidants to rapeseed oil anti-oxidation characteristics;
Fig. 2 difference antioxidants are to peanut oil anti-oxidation characteristics;
Fig. 3 difference antioxidants are to soybean oil anti-oxidation characteristics.
Specific embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, with reference to specific embodiment, to this Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
Embodiment 1
1st, the preparation of plant acid solution:
(1) rice bran was crushed into 40 mesh sieves, using petroleum ether or n-hexane degreasing 3 times, was dried to obtain after solvent flashing de- Fat bran powder;
(2) by defatted rice bran powder and deionized water according to mass ratio 1:5 mixing, pH value 6, using molecular cut off in 5kDa Flat board filter membrane synchronously extract rice bran protein matter therein and rice bran polysaccharide, rice bran residue is collected after filtering;
(3) acetic acid aqueous solution that the rice bran residue of gained is utilized 1% is solvent, and stirring at room temperature extracts 1,6000r/ Min is centrifuged 30min, collects supernatant;By gained supernatant by anion exchange resin adsorption chromatography, and utilize 0.1mol/L Sodium-chloride water solution wash-out, collect eluent, 30% plant acid solution is obtained through cationic ion-exchange resin desalination, after concentration.
2nd, at 20 DEG C, surface active agent tween 20 and cosurfactant ethanol are mixed into water phase, then in stirring Under the conditions of 100rpm, water to be added in edible rapeseed oil, mixing constitutes oily mixed phase to rotating speed, wherein edible vegetable seed Oil, surfactant, cosurfactant quality are respectively the 70%, 10% and 10% of phytic acid water-in-oil microemulsion quality.
3rd, it is the 1% phytic acid aqueous solution (pH3) by mass concentration, at 20 DEG C, is passed through peristaltic pump, adjusts the entrance of pump Pressure is 1 atmospheric pressure, and drop outlets flow is 50 drops/min, and speed of agitator is 100rpm, is added to obtained oil in step 2 In mixed phase, record the phytic acid aqueous solution addition, and using conductivity meter monitor different additions when solution electrical conductivity, meter Conductivity variations rate is calculated, stops being added dropwise when rate of change is intended to 0, the phytic acid aqueous solution quality now added is phytic acid Water-In-Oil The 10% of microemulsion quality, the microemulsion that will be obtained takes and is placed in cuvette on a small quantity, mensuration absorbance under 650nm, with deionization Used as blank, absorbance 0 is transparent phytic acid water-in-oil microemulsion to water, and after being scattered in edible oil medium, particle diameter is 20nm。
4th, the phytic acid water-in-oil microemulsion liquid product of preparation is taken, (addition is in being added to the edible rapeseed oils of 30g 0.01%), it is well mixed and is placed in 60 degree of constant temperature oven, stirred 1 time every 12h, and exchanges its position in an oven, it is fixed When sampling detection edible oil peroxide value (POV), wherein 1 part be blank control group, 3 parts respectively according to identical phytic acid dosage The addition phytic acid aqueous solution, vitamin E, BHT and TBHQ, as a result as shown in Figure 1.
Embodiment 2
1st, the preparation of plant acid solution:
(1) rice bran was crushed into 60 mesh sieves, using petroleum ether or n-hexane degreasing 3 times, was dried to obtain after solvent flashing de- Fat bran powder;
(2) by defatted rice bran powder and deionized water according to mass ratio 1:15 mixing, pH value 8 is existed using molecular cut off The hollow fiber filter membrane of 100kDa synchronously extracts rice bran protein matter therein and rice bran polysaccharide, and rice bran residue is collected after filtering;
(3) acetic acid aqueous solution that the rice bran residue of gained is utilized 3% is solvent, and 3h, 6000r/ are extracted in stirring at room temperature Min is centrifuged 30min, collects supernatant;By gained supernatant by anion exchange resin adsorption chromatography, and using 1mol/L's Sodium-chloride water solution is eluted, and collects eluent, and 50% plant acid solution is obtained through cationic ion-exchange resin desalination, after concentration.
2nd, at 50 DEG C, by surface active agent tween 80 under the conditions of speed of agitator is 400rpm, it is added to edible peanut In oil, the oily mixed phase of mixing composition, wherein edible peanut oil, surfactant qualities are respectively phytic acid water-in-oil microemulsion quality 80% and 15%.
3rd, it is the mixture that the 10% phytic acid aqueous solution (pH10) and cosurfactant glycerine are constituted by mass concentration. At 50 DEG C, passed through micro-injection pump, the inlet pressure for adjusting pump is 3 atmospheric pressure, drop outlets flow be 100 drops/ Min, speed of agitator is 400rpm, is added in step 2 in obtained oily mixed phase, the record phytic acid aqueous solution and helps surface-active Agent composition mixture addition, and using conductivity meter monitor different additions when solution electrical conductivity, calculate electrical conductivity Rate of change, stops being added dropwise when rate of change is intended to 0, and the phytic acid quality now added is phytic acid water-in-oil microemulsion quality 5%, cosurfactant quality is the 5% of phytic acid water-in-oil microemulsion quality.The microemulsion that will be obtained takes and is placed in colorimetric on a small quantity In ware, mensuration absorbance under 650nm, using deionized water as blank, absorbance is 0.2, is translucent phytic acid oil Bag water microemulsion, after being scattered in edible peanut oil medium, particle diameter is 400nm.
4th, the phytic acid water-in-oil microemulsion liquid product of preparation is taken, is added in 30g edible peanut oils (addition is 0.01%), It is well mixed to be placed in 60 degree of constant temperature oven, stirred 1 time every 12h, and its position in an oven is exchanged, timing sampling inspection The peroxide value (POV) of edible peanut oil is surveyed, wherein 1 part is blank control group, 3 parts are added according to identical phytic acid dosage respectively The phytic acid aqueous solution, vitamin E, BHT and TBHQ, as a result as shown in Figure 2.
Embodiment 3
1st, the preparation of plant acid solution:
(1) rice bran was crushed into 50 mesh sieves, using petroleum ether or n-hexane degreasing 3 times, was dried to obtain after solvent flashing de- Fat bran powder;
(2) by defatted rice bran powder and deionized water according to mass ratio 1:10 mixing, pH value 7 is existed using molecular cut off The flat board filter membrane or hollow fiber filter membrane of 50kDa synchronously extract rice bran protein matter therein and rice bran polysaccharide, and rice is collected after filtering Chaff residue;
(3) acetic acid aqueous solution that the rice bran residue of gained is utilized 2% is solvent, and 2h, 6000r/ are extracted in stirring at room temperature Min is centrifuged 30min, collects supernatant;By gained supernatant by anion exchange resin adsorption chromatography, and utilize 0.5mol/L Sodium-chloride water solution wash-out, collect eluent, 30% plant acid solution is obtained through cationic ion-exchange resin desalination, after concentration.
2nd, at 35 DEG C, surfactant lecithin and cosurfactant n-butanol are mixed into water phase, are then being stirred Under the conditions of 250rpm, water to be added in food plant soybean oil, mixing constitutes oily mixed phase to mix rotating speed, wherein edible plant Thing soybean oil, surfactant, cosurfactant quality are respectively the 75% of phytic acid water-in-oil microemulsion quality, 10% He 7%.
3rd, it is the 5.5% phytic acid aqueous solution (pH6.5) by mass concentration, at 35 DEG C, is passed through peristaltic pump, regulation pump Inlet pressure is 2 atmospheric pressure, and drop outlets flow is 75 drops/min, and speed of agitator is 250rpm, is added in step 2 and is obtained Oily mixed phase in, record the phytic acid aqueous solution addition, and using conductivity meter monitor different additions when solution conductance Rate, calculates conductivity variations rate, stops being added dropwise when rate of change is intended to 0, and the phytic acid aqueous solution quality now added is phytic acid The 8% of water-in-oil microemulsion quality, the microemulsion that will be obtained takes and is placed in cuvette on a small quantity, mensuration absorbance under 650nm, to go Used as blank, absorbance is 0.1 to ionized water, is transparent phytic acid water-in-oil microemulsion, is scattered in food plant soybean After in oil medium, particle diameter is 300nm.
4th, the phytic acid water-in-oil microemulsion liquid product of preparation is taken, is added in 30g edible soybean oils (addition is 0.01%), It is well mixed to be placed in 60 degree of constant temperature oven, stirred 1 time every 12h, and its position in an oven is exchanged, timing sampling inspection The peroxide value (POV) of edible soybean oil is surveyed, wherein 1 part is blank control group, 3 parts are added according to identical phytic acid dosage respectively The phytic acid aqueous solution, vitamin E, BHT and TBHQ, as a result as shown in Figure 3.
Embodiment 4
1st, the preparation of plant acid solution:
(1) rice bran was crushed into 60 mesh sieves, using petroleum ether or n-hexane degreasing 3 times, was dried to obtain after solvent flashing de- Fat bran powder;
(2) by defatted rice bran powder and deionized water according to mass ratio 1:15 mixing, pH value 7 is existed using molecular cut off The hollow fiber filter membrane of 7100kDa synchronously extracts rice bran protein matter therein and rice bran polysaccharide, and rice bran residue is collected after filtering;
(3) acetic acid aqueous solution that the rice bran residue of gained is utilized 2.5% is solvent, and 2.5h is extracted in stirring at room temperature, 6000r/min is centrifuged 30min, collects supernatant;By gained supernatant by anion exchange resin adsorption chromatography, and utilize The sodium-chloride water solution wash-out of 0.1~1mol/L, collects eluent, through cationic ion-exchange resin desalination, 40% is obtained after concentration Plant acid solution.
2nd, at 40 DEG C, by surfactant rhamnolipid under the conditions of speed of agitator is 300rpm, it is added to corn oil In, the oily mixed phase of mixing composition, wherein edible corn oil, surfactant qualities are respectively phytic acid water-in-oil microemulsion quality 73% and 12%.
3rd, it is the mixture that the 8% phytic acid aqueous solution (pH7) and cosurfactant glycerine are constituted by mass concentration.25 At DEG C, passed through micro-injection pump, the inlet pressure for adjusting pump is 2 atmospheric pressure, drop outlets flow is 70 drops/min, is stirred Mix rotating speed is 300rpm, is added in step 2 in obtained oily mixed phase, the record phytic acid aqueous solution and cosurfactant composition Mixture addition, and using conductivity meter monitor different additions when solution electrical conductivity, calculate conductivity variations rate, Stop being added dropwise when rate of change is intended to 0, the phytic acid aqueous solution quality now added is phytic acid water-in-oil microemulsion quality 6%, cosurfactant quality is the 9% of phytic acid water-in-oil microemulsion quality.The microemulsion that will be obtained takes and is placed in colorimetric on a small quantity In ware, mensuration absorbance under 650nm, using deionized water as blank, absorbance is 0.15, is transparent or semitransparent Phytic acid water-in-oil microemulsion, after being scattered in food plant corn oil medium, particle diameter is 100nm.
4th, the phytic acid water-in-oil microemulsion liquid product of preparation is taken, is added in 30g edible corn oils (addition is 0.01%), It is well mixed to be placed in 60 degree of constant temperature oven, stirred 1 time every 12h, and its position in an oven is exchanged, timing sampling inspection The peroxide value (POV) of edible corn oil is surveyed, wherein 1 part is blank control group, 3 parts are added according to identical phytic acid dosage respectively The phytic acid aqueous solution, vitamin E, BHT and TBHQ, as a result show that phytic acid water-in-oil microemulsion has the oil resistant fat oxygen equivalent to TBHQ Change ability.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from of the invention In the case of spirit and scope, embodiments of the present invention can be made with various changes, replace and change.

Claims (10)

1. a kind of preparation method of phytic acid water-in-oil microemulsion, comprises the following steps:
1) edible oil, surfactant and cosurfactant are mixed into the oily mixed phase of composition or edible oil and surface-active The oily mixed phase of agent mixing composition;
2) the phytic acid aqueous solution is added dropwise to step 1 under stirring) in edible oil, surfactant and help surface-active Until the conductivity variations rate of solution is minimum in the oily mixed phase of agent mixing composition, transparent or semitransparent phytic acid oil is spontaneously formed Bag water microemulsion;Or the mixture that the phytic acid aqueous solution and cosurfactant are constituted is added dropwise to step under stirring 1) obtained oily mixed phase in, until the conductivity variations rate of solution is minimum, spontaneously forms transparent or semitransparent phytic acid oil bag Water microemulsion;The mass concentration of phytic acid is 1~10% in the phytic acid aqueous solution;
The conductivity variations rate is minimum, refers to be constituted by the phytic acid aqueous solution or the phytic acid aqueous solution and cosurfactant Mixture is added to step 1) in obtained oily mixed phase when, the record phytic acid aqueous solution or the phytic acid aqueous solution and help surface to live Property agent composition mixture addition, and using conductivity meter monitor different additions when solution electrical conductivity, calculate conductance Rate rate of change, is minimum rate of change when rate of change is intended to 0.
2. the preparation method of phytic acid water-in-oil microemulsion according to claim 1, it is characterised in that:The edible oil is dish Seed oil, peanut oil, soybean oil, sesame oil, linseed oil, olive oil, corn oil, sunflower oil, lard, fish oil, in butter One or more, edible oil quality used is the 70~80% of phytic acid water-in-oil microemulsion quality.
3. the preparation method of phytic acid water-in-oil microemulsion according to claim 1, it is characterised in that:The surfactant It is polysorbas20, polysorbate40, polysorbate60, Tween 80, this disk 20, sucrose fatty ester, rhamnolipid, the one kind or several in lecithin Kind, surfactant qualities used are the 10~20% of phytic acid water-in-oil microemulsion quality.
4. the preparation method of phytic acid water-in-oil microemulsion according to claim 1, it is characterised in that:It is described to help surface-active Agent is ethanol, glycerine, one or more in n-butanol, and cosurfactant quality used is phytic acid water-in-oil microemulsion The 5~10% of quality.
5. the preparation method of phytic acid water-in-oil microemulsion according to claim 1, it is characterised in that:Phytic acid aqueous solution pH= 3~10, the phytic acid aqueous solution quality of addition is the 5~10% of phytic acid water-in-oil microemulsion quality.
6. the preparation method of phytic acid water-in-oil microemulsion according to claim 1, it is characterised in that:The edible oil, table Face activating agent and the cosurfactant mixing oily mixed phase of composition, are at 20~50 DEG C, first by surfactant and to help surface Activating agent mixes, and then under the conditions of speed of agitator is 100~400rpm, is added in edible oil;The edible oil and surface The oily mixed phase of activating agent mixing composition, is at 20~50 DEG C, under the conditions of speed of agitator is 100~400rpm, surface to be lived Property agent is added in edible oil.
7. the preparation method of phytic acid water-in-oil microemulsion according to claim 1, it is characterised in that:The phytic acid aqueous solution Be added dropwise to step 1 under stirring) in obtained oily mixed phase, be at 20~50 DEG C, the phytic acid aqueous solution to be led to Cross peristaltic pump or micro-injection pump, the inlet pressure for adjusting pump is 1-3 atmospheric pressure, drop outlets flow be 50~100 drip/ Min, at 20~50 DEG C, speed of agitator is 100~400rpm, is added in oily mixed phase;The phytic acid aqueous solution and help surface The mixture of activating agent composition is added dropwise to step 1 under stirring) in obtained oily mixed phase, be at 20~50 DEG C Under, the mixture that the phytic acid aqueous solution and cosurfactant are constituted adjusts the entrance of pump by peristaltic pump or micro-injection pump Pressure is 1-3 atmospheric pressure, and drop outlets flow is 50~100 drops/min, at 20~50 DEG C, speed of agitator for 100~ 400rpm, is added in oily mixed phase.
8. the preparation method of phytic acid water-in-oil microemulsion according to claim 1, it is characterised in that:It is described transparent or semi-transparent Between 0~0.2, particle size range is between 20~400nm for bright phytic acid water-in-oil microemulsion absorbance.
9. the preparation method of phytic acid water-in-oil microemulsion according to claim 1, it is characterised in that:The phytic acid aqueous solution Preparation method comprise the following steps:
1) rice bran was crushed into 40~60 mesh sieves, using petroleum ether or n-hexane degreasing 3 times, degreasing was dried to obtain after solvent flashing Bran powder;
2) by defatted rice bran powder and deionized water according to mass ratio 1:5~15 mixing, pH value is 6~8, is existed using molecular cut off The flat board filter membrane or hollow fiber filter membrane of 5kDa~100kDa synchronously extract rice bran protein matter therein and rice bran polysaccharide, after filtering Collect rice bran residue;
3) the rice bran residue of gained is stirred using the acetic acid aqueous solution of 1~3wt% for solvent is extracted, at room temperature and extracts 1 ~3h, 6000r/min are centrifuged 30min, collect supernatant;By gained supernatant by anion exchange resin adsorption chromatography, and Eluted using the sodium-chloride water solution of 0.1~1mol/L, collect eluent, through cationic ion-exchange resin desalination, obtained after concentration The phytic acid aqueous solution of 30~50wt%.
10. a kind of purposes of phytic acid water-in-oil microemulsion, the phytic acid water-in-oil microemulsion is as preparation method described in claim 1 Prepare, it is characterised in that:It is used for edible oil or containing fatty foods as antioxidant.
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CN110256486A (en) * 2019-06-26 2019-09-20 浙江科技学院 A kind of Extraction of acetic acid rice bran phytic acid technique based on surfactant auxiliary
CN113273606A (en) * 2021-06-09 2021-08-20 浙江省农业科学院 Natural antioxidant composition for nuts

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CN110256486A (en) * 2019-06-26 2019-09-20 浙江科技学院 A kind of Extraction of acetic acid rice bran phytic acid technique based on surfactant auxiliary
CN113273606A (en) * 2021-06-09 2021-08-20 浙江省农业科学院 Natural antioxidant composition for nuts

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