CN108477455B

CN108477455B - Preparation method of whole citrus fruit superfine powder and whole citrus fruit superfine powder

Info

Publication number: CN108477455B
Application number: CN201810219265.9A
Authority: CN
Inventors: 单杨; 李绮丽; 李高阳; 刘伟; 付复华; 孙俊杰; 李涛; 谢秋涛
Original assignee: HUNAN AGRICULTURAL PRODUCTS PROCESSING INSTITUTE
Current assignee: HUNAN AGRICULTURAL PRODUCTS PROCESSING INSTITUTE
Priority date: 2018-03-16
Filing date: 2018-03-16
Publication date: 2022-02-18
Anticipated expiration: 2038-03-16
Also published as: CN108477455A

Abstract

The invention discloses a preparation method of whole citrus fruit superfine powder and the whole citrus fruit superfine powder, wherein the preparation method comprises the following steps: carrying out ozone cleaning treatment on oranges, and then sequentially carrying out coarse crushing, wet superfine crushing, ultrasonic crushing, enzymolysis, colloid milling and high-pressure homogenization to obtain full fruit pulp with the particle size of 5-15 microns; and then carrying out vacuum freezing spray drying on the whole fruit pulp to obtain the whole fruit superfine powder. The invention effectively solves the problem that macromolecules such as fiber, pectin and the like in the peel and seeds of the whole citrus are difficult to dissolve in water, realizes the full utilization of the citrus and furthest reserves the nutrient components; the self pectin is utilized to realize the stability of the superfine powder in a fruit juice system, and the chemical addition is reduced; the essential oil of the fruit powder is utilized to promote the effective bacteriostasis of the fruit powder; the functional components such as flavone, limonin, carotenoid and the like enhance the functions of antioxidation, anti-inflammation and the like; the obtained whole citrus fruit powder has strong fragrance, bright color, rich functional nutrient components and good stability.

Description

Preparation method of whole citrus fruit superfine powder and whole citrus fruit superfine powder

Technical Field

The invention relates to the technical field of food, in particular to a preparation method of whole citrus fruit superfine powder and the whole citrus fruit superfine powder.

Background

Citrus is the first fruit in the world with growing in 146 countries and regions in the world, mainly concentrated in china, brazil, the united states and countries along the coast of the mediterranean sea. China is the first major citrus nation in the world, and the citrus planting area and yield are in the first place in the world. In 2014, the planting area of China reaches 242 million hectares, the yield is 3494.22 million tons, and the yield accounts for about 22.4 percent of the total world yield. The citrus industry involves 19 provinces (cities and districts) over 100 citrus counties across the country, and 1.82 hundred million rural populations.

The traditional citrus fruit powder is powder obtained by directly obtaining juice from citrus in a squeezing mode and then performing spray drying, and the brewed citrus juice is delicious in color, rich in nutrition and pleasant in taste, and has the advantages of being light and convenient to carry compared with the traditional citrus juice. However, the juice yield of the citrus juice obtained by the squeezing method is only 30-50%, only limited water-soluble nutrient components (such as sugar, acid, vitamins, minerals and the like) in the juice are reserved, the remaining 50-70% of citrus peel residues are discarded as waste, a large amount of nutrient components in the peel residues are not utilized, huge waste is caused, the acidity of the peel residues is extremely high, and the peel residues are easy to pollute ecological environment such as soil as waste. In fact, the citrus peel dregs contain rich nutrient components, particularly functional components such as flavonoids, limonoids and carotenoids, and have multiple physiological effects of resisting oxidation, inflammation, tumors and the like. Therefore, the traditional citrus fruit powder has the defect of insufficient nutrient content, the problem of great nutrient loss exists in the processing process, and the peel and residue left after the traditional citrus fruit powder is prepared not only cause resource waste, but also pollute the environment.

Disclosure of Invention

The invention aims to overcome the defects of the prior art, in particular to the technical problems of insufficient deep processing of whole citrus fruits, poor water solubility of whole citrus fruit powder, more loss of nutrient substances in the processing process, low retention rate of functional ingredients and the like, and provides a preparation method of whole citrus fruit superfine powder which is rich in functional ingredients, good in water solubility and high in retention rate of nutrient substances and whole citrus fruit superfine powder.

In order to solve the technical problems, the invention adopts the following technical scheme:

the preparation method of the whole citrus fruit superfine powder comprises the following steps:

(1) degrading and sterilizing pesticide residues: carrying out ozone cleaning treatment on the pretreated citrus, and carrying out pesticide residue degradation and sterilization on citrus peel;

(2) fruit pulp micronization: carrying out coarse crushing on the citrus treated in the step (1) to obtain a citrus juice residue mixture, then carrying out wet superfine crushing to obtain superfine crushed whole fruit pulp, then carrying out ultrasonic crushing to obtain ultrasonic crushed whole fruit pulp, and carrying out enzymolysis, colloid milling and high-pressure homogenization to obtain whole fruit pulp with the particle size of 5-15 microns;

(3) preparing full-superfine fruit powder: and (3) carrying out spray drying on the whole fruit pulp obtained in the step (2) to obtain the whole citrus fruit superfine powder.

In the above method for preparing ultrafine powder of whole citrus fruit, preferably, in the step (2), the particle sizes of pulp and peel residues in the citrus juice and residue mixture are both 3mm to 5mm, and the rotation speed of coarse grinding is 1500r/min to 2000 r/min.

In the above method for preparing ultrafine whole citrus fruit powder, preferably, in the step (2), the particle size of the ultrafine whole citrus fruit pulp is 50 to 100 μm, the wet ultrafine grinding is performed for 3 to 4 times, and the rotation speed of the wet ultrafine grinding is 6000 to 9000 r/min.

In the above method for preparing ultrafine powder of whole citrus fruit, preferably, in the step (2), the particle size of the ultrasonically-crushed whole fruit pulp is 40 to 70 μm, the ultrasonic crushing is performed for 1 time, the power of the ultrasonic crushing is 2200 to 3000W, and the time of the ultrasonic crushing is 10 to 20 min.

In the above method for preparing citrus whole fruit ultrafine powder, preferably, in the step (2), the complex enzyme preparation used for enzymolysis includes pectinase, cellulase, hemicellulase and acid protease, and the volumes of the pectinase, the cellulase, the hemicellulase and the acid protease are respectively 0.06% -0.08%, 0.05% -0.07%, 0.2% -0.3% and 0.1% -0.3% of the volume of the ultrasonically-pulverized whole fruit pulp;

and/or the enzymolysis temperature is 40-50 ℃, and the enzymolysis time is 30-50 min.

In the above method for preparing citrus whole fruit micropowder, preferably, in the step (2), whole fruit pulp with a particle size of 10 μm to 30 μm is obtained after the colloid mill treatment, and the colloid mill treatment includes: and (3) treating the whole fruit pulp subjected to enzymolysis for 1-2 times by using a colloid mill at the rotating speed of 2500-3000 r/min.

In the above method for preparing ultrafine citrus fruit powder, preferably, in the step (2), the pressure for high-pressure homogenization is 60 to 100 MPa.

In the above method for preparing ultrafine powder of whole citrus fruit, preferably, in the step (3), the spray drying is vacuum freeze spray drying, wherein the cold trap freezing temperature of the vacuum freeze spray drying is-70 ℃ to-60 ℃, and the spray freezing temperature is-30 ℃ to-20 ℃.

In the above method for preparing citrus whole fruit ultrafine powder, preferably, the preparation method further comprises the step (4): carrying out ultra-high pressure sterilization on the whole citrus fruit superfine powder, wherein the pressure of the ultra-high pressure sterilization is 100MPa to 500MPa, and the pressure maintaining time is 5min to 10 min.

As a general inventive concept, the invention also provides the whole citrus fruit superfine powder prepared by the preparation method.

In the preparation method, the enzyme activities of the pectinase, the cellulase, the hemicellulase and the acid protease are 50000U/g, 10000U/g and 50000U/g respectively.

The invention takes whole citrus as a raw material, adopts a novel fruit juice micronizing technology, combines multiple technologies such as complex enzyme enzymolysis, freeze spray drying, cold sterilization and the like, and is processed into full-utilization micronized citrus powder rich in functional components, so that the problems of low raw material utilization rate, high cost, insufficient nutrient substances and the like of the traditional citrus powder are solved, the problems of poor water solubility, poor mouthfeel and the like of processed products of the whole citrus are solved, the full utilization of the whole citrus from peel, tangerine pith and juice cells to citrus seeds is realized, the nutrient components of the citrus are reserved to the maximum extent, the retention rate of flavonoids in the products is more than or equal to 80 percent, and the retention rate of limonoids is more than or equal to 85 percent, and the nutritional value is improved; meanwhile, the method has no peel residue waste, reduces the treatment cost of peel residue, greatly reduces the cost, and is one of the mainstream directions for processing future citrus drinks.

Compared with the prior art, the invention has the advantages that:

(1) the invention firstly carries out full-fruit treatment on the citrus to prepare the superfine powder, thereby realizing full utilization of the citrus. The traditional orange drink processing only utilizes juice in pulp, and peel and residue are not utilized basically, so that the ecological environment is polluted and the resource waste is caused no matter the orange drink is buried or burnt. In fact, the pericarp is rich in nutritional functional components such as natural pigment, pectin, essential oil, flavone, carotenoid and the like, and the fiber and the like in the pomace are also good sources of dietary fiber. The natural functional components can be effectively utilized by adopting the whole citrus to prepare the micronized fruit powder, the natural pigment in the peel increases the color of the superfine powder, the pectin in the peel realizes the stability of the superfine powder in a juice system, and the chemical addition of the natural pigment and a stabilizer is reduced; the essential oil components in the peel increase the flavor of the whole-fruit superfine powder, the peel is also rich in flavonoid compounds, the main components comprise narirutin, hesperidin, neohesperidin and the like which are antioxidant components, and the effective combination of the essential oil and the flavone components not only realizes the effective bacteriostasis of the whole-fruit superfine powder, but also slows down the oxidation of nutrient components; the citrus seeds are rich in triterpenoids such as limonin, nomilin and the like, have the functional activities of resisting inflammation, resisting tumor, resisting cancer and the like, and further enrich the nutritional ingredients and the biological activity of the whole-fruit superfine powder.

(2) The inventor finds that the pericarp, the tangerine pith and the tangerine seed of the whole citrus contain a large amount of macromolecular substances such as fiber, hemicellulose, pectin and the like, and are difficult to dissolve in an aqueous solution, so that fruit powder obtained by processing in a traditional mode is difficult to dissolve in the aqueous solution, and the solubility, the mouthfeel and other qualities of the whole citrus superfine powder are directly influenced. The inventor carries out a long-term and large-scale research in order to solve the technical problems of poor water solubility, more nutrient loss, low retention rate of functional components and the like of whole fruit powder, integrates the six processes of coarse crushing, wet-method superfine crushing, ultrasonic crushing, compound enzymolysis, colloid mill and high-pressure homogenization by establishing a brand-new whole-fruit superfine micronization technology of citrus, changes the physical properties of particles by using the combination of wet-method superfine crushing, ultrasonic crushing, colloid mill and high-pressure homogenization, and hydrolyzes part of macromolecular pectin into galacturonic acid by compound enzymolysis (incomplete enzymolysis and realization by controlling the enzymolysis conditions), thereby separating components such as cellulose, hemicellulose, protein and the like which are closely combined with pectin, promoting the hydrolysis of the macromolecular cellulose and the hemicellulose into oligosaccharides, cellobiose, glucose and reducing sugar with smaller molecular weight, and the macromolecular protein is hydrolyzed into polypeptide or amino acid, the chemical structure of the full-fruit superfine powder is changed, the effective micronization of fruit residue components is realized, the particle size of the full-fruit pulp is reduced, and the particle size of the full-fruit pulp reaches 5-15 mu m, so that the particle size of the full-fruit superfine powder of citrus is greatly reduced, and the instant property and the utilization rate of nutritional ingredients of the full-fruit superfine powder are effectively improved. Meanwhile, the non-enzymatic pectin continuously plays the roles of a thickening agent and a stabilizing agent, the stability of the whole-fruit superfine powder in an aqueous solution system is promoted, a suspension microstructure with the whole-fruit superfine powder uniformly dispersed in an aqueous solution is formed, and the effect of efficiently dissolving and dispersing the whole-fruit superfine powder is realized.

(3) The invention adopts cold sterilization technologies such as ozone cleaning and ultrahigh pressure sterilization technologies, and is matched with cold processing technologies such as freezing spray drying and the like to be cooperated with antioxidant functional components such as essential oil, flavone and the like for synergism, so that not only is high-efficiency bacteriostasis realized for the whole-fruit superfine powder, but also functional nutritional components such as vitamin C, carotenoid, limonin, flavone and the like in the whole fruit are retained to the maximum extent, the original qualities such as aroma, color, taste and the like of the materials are maintained, and the obtained whole-fruit superfine powder for citrus is fine in taste, rich in aroma, bright in color and rich in functional active components. Compared with a freeze dryer, the spray freeze dryer has the advantages of lower energy consumption and accordance with the low-carbon requirement, the dried whole-fruit ultrafine powder is granular, the flowability is very good, the whole-fruit ultrafine powder does not need to be crushed again, the spray freeze dryer has less damage to the nutrient components of the whole-fruit ultrafine powder and does not change the bioactivity, the nutrient components in the whole citrus fruit are retained to the maximum extent, the nutritional value is improved, the retention rate of flavone substances in the product is more than or equal to 80%, and the retention rate of limonin is more than or equal to 85%. The natural bacteriostatic functional components such as essential oil in the citrus peel are combined with ultrahigh pressure sterilization for synergistic interaction, so that effective sterilization of the whole-fruit superfine powder in the later stage is realized, and meanwhile, the original nutritional ingredients in the material can be well reserved in the low-temperature short-time sterilization process.

Drawings

FIG. 1 is a process flow chart of a preparation method of whole citrus fruit superfine powder in the embodiment of the invention.

Detailed Description

The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.

The materials and equipment used in the following examples are commercially available.

Example 1

The invention discloses a preparation method of whole citrus fruit superfine powder, which has a process flow shown in figure 1 and comprises the following steps:

(1) pretreatment of raw materials: selecting fresh, strong-fragrance and high-sugar red sweet oranges, removing rotten and deteriorated oranges, removing orange stems, cleaning mud and other impurities.

(2) Degrading and sterilizing pesticide residues: and (3) placing the pretreated citrus in an ozone tank for high-concentration ozone cleaning, wherein the ozone concentration is 5-15 mg/L, and the treatment time is 15-40 min, so as to degrade and sterilize the pesticide residues of the citrus peel.

(3) Fruit pulp micronization: conveying the citrus subjected to pesticide residue degradation and sterilization into a GFM-FC-3 fruit and vegetable crusher to crush for 2 times for coarse crushing, wherein the rotating speed is 1500r/min, so as to obtain a citrus juice residue mixture, and the particle size of pulp and peel residue in the citrus juice residue mixture is 3-5 mm. And carrying out wet superfine grinding on the coarsely ground citrus juice residue mixture for 4 times by adopting a QDGP-11 shear type superfine grinder at the rotating speed of 8000r/min to obtain superfine whole fruit pulp with the particle size of 55-80 mu m. And then carrying out ultrasonic crushing for 1 time by adopting an LC-3000N ultrasonic crusher with the ultrasonic power of 2200W for 15min to obtain the ultrasonic crushed whole fruit pulp with the particle size of 40-60 mu m. And then carrying out moderate enzymolysis by adopting complex enzyme, taking the volume of the ultrasonically crushed whole fruit pulp as a reference, sequentially adding 0.06 percent of pectinase (enzyme activity of 50000U/g), 0.05 percent of cellulase (50000U/g), 0.2 percent of hemicellulase (10000U/g) and 0.1 percent of acid protease (50000U/g) into the ultrasonically crushed whole fruit pulp according to volume percentage, and carrying out enzymolysis treatment for 40min at the temperature of 45 ℃. Treating the obtained enzymolysis product for 2 times by adopting a JMS-80 colloid mill at the rotating speed of 2500r/min to obtain the whole fruit pulp with the particle size of 20-30 mu m. Homogenizing for 1 time under 80MPa with APV-1000 high pressure homogenizer to obtain whole fruit pulp with particle size of 10-15 μm, and mixing the solute and solvent in the pulp under high pressure to make the pulp have uniform particle size and improve the stability of the pulp.

(4) Spray drying: and (3) carrying out vacuum freezing spray drying on the whole fruit pulp with the particle size of 10-15 microns obtained in the step (3) by adopting YC-3000 laboratory freezing spray drying equipment, wherein the freezing temperature of a cold trap of the vacuum freezing spray drying is-70-60 ℃, the freezing temperature of the spray is-30-20 ℃, and the freezing drying time is 48h, so as to obtain the citrus whole fruit submicron powder.

(5) Ultra-high pressure sterilization: sterilizing the whole citrus fruit superfine powder under the ultrahigh pressure of 400MPa for 8min to obtain the sterilized whole citrus fruit superfine powder (namely the red orange whole fruit superfine powder) rich in functional components.

The functional components of the red orange whole fruit superfine powder prepared in the embodiment and the traditional red orange fruit powder are compared and measured, and the detection results are shown in the following table 1.

Table 1: comparison table of functional components of traditional fruit powder and whole fruit superfine powder

The data in the table show that the contents of flavonoid substances and limonin substances in the whole fruit superfine powder are obviously higher than those of the traditional fruit powder. The analysis shows that the citrus flavonoid substances mainly exist in citrus peel and citrus collaterals, wherein narirutin, hesperidin, nobiletin and citrinin are used as main representative components; the limonin substances of citrus mainly exist in citrus seeds, wherein limonin and nomilin are taken as main representative components; therefore, the full-fruit superfine powder prepared from the full citrus fruits is used for effectively compounding abundant functional components such as flavonoids, limonin and the like in citrus peel, citrus collaterals and citrus seeds, so that the content of functional nutritional ingredients is obviously improved.

Example 2

(1) pretreatment of raw materials: selecting fresh century tangerine, and removing rotten and deteriorated raw materials, soil and other impurities.

(2) Degrading and sterilizing pesticide residues: and (3) placing the pretreated citrus in an ozone tank for high-concentration ozone cleaning so as to degrade and sterilize the pesticide residues of the citrus peel.

(3) Fruit pulp micronization: and (3) conveying the citrus subjected to pesticide residue degradation and sterilization into a GFM-FC-3 fruit and vegetable crusher for coarse crushing for 3 times at the rotating speed of 1500r/min to obtain a citrus juice residue mixture, wherein the particle size of pulp and peel residue in the citrus juice residue mixture is 3-5 mm. And (3) carrying out superfine grinding on the coarsely ground citrus juice residue mixture for 4 times by adopting a QDGP-11 shear type superfine grinder at the rotating speed of 9000r/min to obtain superfine ground whole fruit pulp with the particle size of 50-75 microns. And then carrying out ultrasonic crushing for 1 time by adopting an LC-3000N ultrasonic crusher with the ultrasonic power of 2400W for 15min to obtain the ultrasonic crushed whole fruit pulp with the particle size of 40-55 microns. And then carrying out moderate enzymolysis by adopting complex enzyme, taking the volume of the ultrasonically crushed whole fruit pulp as a reference, sequentially adding 0.06 percent of pectinase (with the enzyme activity of 50000U/g), 0.05 percent of cellulase (with the enzyme activity of 50000U/g), 0.2 percent of hemicellulase (with the enzyme activity of 10000U/g) and 0.2 percent of acid protease (with the enzyme activity of 50000U/g) into the whole fruit pulp according to the volume percentage, and carrying out enzymolysis treatment for 40min at the temperature of 45 ℃. And then processing for 2 times by adopting a JMS-80 colloid mill at the rotating speed of 2800r/min to obtain the full fruit pulp with the grain diameter of 10-20 mu m. Homogenizing under 100MPa with APV-1000 high pressure homogenizer to obtain whole fruit pulp with particle size of 5-10 μm, mixing solute and solvent in the pulp under high pressure to make the pulp particle size more uniform, and increasing stability of the pulp.

(4) Spray drying: and (3) carrying out vacuum freezing spray drying on the whole fruit pulp with the particle size of 5-10 microns obtained in the step (3) by adopting YC-3000 laboratory freezing spray drying equipment, wherein the freezing temperature of a cold trap of the vacuum freezing spray drying is-70-60 ℃, the freezing temperature of the spray is-30-20 ℃, and the drying time is 48 hours, so as to obtain the whole citrus fruit submicron powder.

(5) Ultra-high pressure sterilization: sterilizing the whole citrus fruit superfine powder under the ultrahigh pressure of 400MPa for 8min to obtain sterilized whole citrus fruit superfine powder (namely century tangerine superfine powder) rich in functional components.

The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.

Claims

1. The preparation method of the whole citrus fruit superfine powder is characterized by comprising the following steps:

(1) degrading and sterilizing pesticide residues: carrying out ozone cleaning treatment on the pretreated citrus so as to carry out pesticide residue degradation and sterilization on citrus peel;

(2) fruit pulp micronization: carrying out coarse crushing on the citrus treated in the step (1) to obtain a citrus juice residue mixture with the pulp and the peel residue of which the particle sizes are both 3-5 mm, then carrying out wet-method superfine crushing to obtain superfine crushed whole fruit pulp with the particle size of 50-100 mu m, then carrying out ultrasonic crushing to obtain ultrasonic crushed whole fruit pulp with the particle size of 40-70 mu m, and then carrying out enzymolysis, colloid milling and high-pressure homogenization to obtain whole fruit pulp with the particle size of 5-15 mu m; the grain diameter of the whole fruit pulp obtained by the colloid mill is 10-30 mu m; the enzymolysis is incomplete enzymolysis, the complex enzyme preparation used for the enzymolysis comprises pectinase, cellulase, hemicellulase and acid protease, the volumes of the pectinase, the cellulase, the hemicellulase and the acid protease are respectively 0.06% -0.08%, 0.05% -0.07%, 0.2% -0.3% and 0.1% -0.3% of the volume of the ultrasonically crushed whole fruit pulp according to volume percentage, the enzyme activities of the pectinase, the cellulase, the hemicellulase and the acid protease are respectively 50000U/g, 10000U/g and 50000U/g, the enzymolysis temperature is 40-50 ℃, and the enzymolysis time is 30-50 min; the pressure of the high-pressure homogenization is 60 MPa-100 MPa;

(3) preparing whole fruit superfine powder: carrying out spray drying on the whole fruit pulp obtained in the step (2) to obtain whole citrus fruit superfine powder; the spray drying adopts vacuum freezing spray drying;

in the step (2), the ultrasonic crushing is carried out for 1 time, the power of the ultrasonic crushing is 2200 to 3000W, and the time of the ultrasonic crushing is 10 to 20 min;

in the step (2), the colloid mill treatment comprises: treating the whole fruit pulp subjected to enzymolysis for 1-2 times by using a colloid mill at the rotating speed of 2500-3000 r/min;

in the step (3), the freezing temperature of the cold trap of the vacuum freezing spray drying is-70 ℃ to-60 ℃, and the freezing temperature of the spray is-30 ℃ to-20 ℃.

2. The method for preparing whole citrus fruit micropowder according to claim 1, wherein in the step (2), the rotation speed of the coarse grinding is 1500r/min to 2000 r/min.

3. The preparation method of whole citrus fruit ultrafine powder according to claim 1, wherein in the step (2), the wet ultrafine grinding is performed 3 to 4 times, and the rotation speed of the wet ultrafine grinding is 6000 to 9000 r/min.

4. The method for preparing whole citrus fruit micropowder according to any one of claims 1 to 3, characterized by further comprising the step (4): carrying out ultra-high pressure sterilization on the whole citrus fruit superfine powder, wherein the pressure of the ultra-high pressure sterilization is 100MPa to 500MPa, and the pressure maintaining time is 5min to 10 min.

5. An ultrafine citrus fruit powder prepared by the method according to any one of claims 1 to 4.