CN113576957A

CN113576957A - Extraction method of sweet orange juice and application of obtained sweet orange juice

Info

Publication number: CN113576957A
Application number: CN202010362790.3A
Authority: CN
Inventors: 张文云; 许显; 蔡少纯; 唐明慧; 朱思阳; 艾勇
Original assignee: Guangdong Heji Biotechnology Co ltd
Current assignee: Guangdong Heji Biotechnology Co ltd
Priority date: 2020-04-30
Filing date: 2020-04-30
Publication date: 2021-11-02

Abstract

The invention discloses a method for extracting sweet orange juice, which comprises the steps of preliminarily extracting sweet oranges by a low-temperature-vacuum (reduced-pressure) technology without adding any solvent, collecting a part of sweet orange cell water and preliminary-extracted sweet orange residues, adding a certain amount of cellulase and pectinase into the preliminary-extracted sweet orange cell water, then pouring the mixture back into the preliminary-extracted sweet orange residues, carrying out secondary extraction by the low-temperature-vacuum (reduced-pressure) technology, and collecting the sweet orange juice. The method has simple process and high extraction rate. The sweet orange juice obtained by the method is colorless, clear and transparent, is rich in more than 60 volatile active ingredients, has strong fruit fragrance and high safety, and has an anti-inflammatory effect; has high utilization value, and can be applied to the fields of skin care products, foods, health care products and the like.

Description

Extraction method of sweet orange juice and application of obtained sweet orange juice

Technical Field

The invention relates to the technical field of agricultural product treatment, in particular to an extraction method of sweet orange juice and application of the obtained sweet orange juice.

Background

Sweet orange is a plant of Citrus of Rutaceae, arbor, and is widely planted in south of Qinling mountain of China. The sweet orange fruit contains abundant vitamin C, and has effects of increasing body resistance, increasing capillary elasticity, and reducing blood cholesterol. Sweet orange also contains abundant hesperidin, narirutin, naringin, limonin, citric acid, and malic acid; the pericarp contains volatile oil, and more than 70 kinds of substances, mainly n-decanal, citral, limonene and octanol. The sweet orange contains abundant vitamin C and carotene, and has effects of inhibiting carcinogen formation, softening and protecting blood vessel, promoting blood circulation, and reducing cholesterol and blood lipid.

At present, the utilization of sweet oranges mainly focuses on pulp juice, sweet orange oil, extract hesperidin and the like. Wherein the sweet orange oil can be prepared by cold grinding fresh whole fruit (oil yield is 0.35-0.37%) or cold pressing fresh pericarp (oil yield is 0.3-0.5%), to obtain cold pressing sweet orange oil; or carrying out steam distillation (the oil yield is 0.4-0.7%) on residues obtained after cold pressing or collected crushed fruit peels to obtain distilled sweet orange oil; the method has the advantages of low oil yield, no reuse of the components except oil, and high cost. The extraction method of hesperidin mostly adopts alcohol extraction, and hesperidin is obtained by column separation after extraction, so that the steps are complicated and the time consumption is long. Therefore, the development of a new process for fully extracting the active ingredients in the sweet oranges and improving the utilization rate of the sweet orange extract have very important significance.

Chinese patent application CN106261332A discloses a method for extracting cell water from lemon, wherein the lemon is peeled, sliced, frozen, put into a vacuum drying oven with the vacuum degree of 0.08-0.095, heated to 40-45 ℃ at a certain speed, and the cell water of the lemon is collected. The method mainly comprises the steps of destroying the structure of lemon cells by freezing, thereby promoting the outflow of cell water; the problem that cell water extraction is affected by large-area collapse in the temperature rising process due to uneven freezing is solved by slow temperature reduction and slow temperature rising, but the extraction time is long (the extraction time is known to be more than 8 hours from the specification), the extraction efficiency is not high, and the method is not suitable for industrial production.

Regarding the extraction of plant cell water, the chinese patent application CN109730948A discloses a method for preparing peony flower cell water by combining ultrasonic low-temperature rotary steaming method and enzyme method: firstly, squeezing to obtain juice and residue 1, then carrying out rotary evaporation on the residue 1 to obtain cell water 1 and residue 2, and finally carrying out enzymatic hydrolysis on the residue 2 and then carrying out rotary evaporation to obtain cell water 2. And mixing the juice, the cell water 1 and the cell water 2 to obtain the peony cell water. The method has high extraction efficiency, but has the following defects: (1) the squeezing method is adopted and then mixed with the liquid obtained by the vacuum extraction method, so that polysaccharide, pigment and pungent smell are brought in, and the problems of corrosion prevention and decoloration are caused; (2) the method solves the problem of corrosion resistance by being matched with other plants for distillation at the later stage of the process, but easily changes the original water content and smell of the peony cells, and the quality cannot be controlled in the later-stage production.

Disclosure of Invention

The invention aims to provide a sweet orange fruit water extraction method, which can obtain sweet orange fruit water rich in various volatile active ingredients, and has strong fruit fragrance and high utilization value.

The invention is realized by the following technical scheme:

a method for extracting sweet orange juice comprises the following steps: adding no solvent, primarily extracting sweet orange fruits at the temperature of 30-65 ℃ and under the pressure of-60 kPa to-101 kPa, forming steam in sweet orange cell water, condensing and collecting liquid, extracting for 1.5-2.5 hours to obtain primary cell water and primary sweet orange fruit residues, adding 0.25-0.45 percent of cellulase and 0-0.1 percent of pectinase based on the total weight of the primary sweet orange into the primary cell water, pouring the mixture into the primary sweet orange fruit residues, extracting for 4-6 hours again under the conditions of the temperature of 35-50 ℃ and the pressure of-85 kPa to-101 kPa, and collecting the sweet orange fruit water.

Under the required temperature and pressure conditions, the sweet orange cell water can be well evaporated out and condensed for collection, and meanwhile, the extraction at a lower temperature can reduce the loss of volatile active ingredients and retain the activity of the cell water. Preferably, the temperature of the primary extraction is 35-50 ℃, and the pressure is-85 kPa-101 kPa.

According to the invention, a certain amount of enzyme is added into the primary cell extraction water, and the primary cell extraction water is put into a container to extract the sweet orange fruit residues again, so that the method has the following beneficial advantages: firstly, the surface tension of primary extracted cell water is low, and the permeability is good; secondly, the pH of the primary cell extracting water is 3-7, and the pH does not need to be additionally adjusted, so that the enzyme activity is favorably improved; thirdly, the enzymolysis can accelerate the wall breaking; fourth, low temperature vacuum technique. Through the synergy of the four effects, the enzymolysis speed can be controlled at a lower temperature (35-50 ℃), and the cell sap outflow speed is accelerated. The primary extraction cell water poured back into the container is firstly steamed in about the first 1 hour in the secondary extraction step, the enzymolysis speed is high in the period, the enzymolysis time is controlled by the amount of the primary extraction liquid and the technological conditions of secondary extraction (at the moment, the amount of the primary extraction liquid is important, the enzymolysis time is prolonged, the enzymolysis is excessive, the enzymolysis time is shortened, the enzymolysis is insufficient), and the problems that the extracting solution is diluted due to the fact that a large amount of water is added as an enzymolysis solvent and the odor is stimulated due to the excessive enzymolysis in the traditional enzymolysis method are solved. Therefore, the primary extraction time is one of the key parameters, if the time is too short, the primary extraction cell water is too little, and the cell water is difficult to infiltrate the residues of the sweet orange fruits after the enzyme is added, so that the enzymolysis cannot be normally carried out. If the primary extraction time is too long, cell water flows out too much, so that the enzymolysis time is prolonged, and the risk of excessive enzymolysis is brought; and simultaneously, the subsequent extraction efficiency is reduced.

With regard to the permeability of the initial extraction of the sweet orange cell water, experimental comparison shows that when the sweet orange fruit residues are extracted by a solvent method, about 60% more flavone and polysaccharide can be extracted by the sweet orange cell water compared with the method that pure water is used as a solvent; it can be shown that the permeability of the water of the orange cells is better than that of pure water.

Preferably, the addition amount of the cellulase is 0.3-0.4%, and the addition amount of the pectinase is 0.02-0.06%. The enzyme is macromolecular protein, can be adsorbed on the cell surface of the sweet orange fruit residue in the required addition range, cannot be volatilized under the low-temperature vacuum condition, and does not need to be subjected to subsequent treatment.

The sweet oranges are fresh sweet orange fruits (full in water).

The sweet orange slices are 1-10 mm in thickness, and are beneficial to extraction of sweet orange cell water.

Stirring is carried out in the extraction process, and the stirring speed is 1-150 revolutions per minute. The sweet orange fruits are uniformly heated, local high temperature is prevented, and meanwhile, the exposure rate of the cut surfaces in a negative pressure environment can be increased, so that the extraction efficiency is improved; and in the secondary extraction step, the primary extraction cell water added with the enzyme can be uniformly mixed with the sweet orange fruit residues by stirring, so that all the sweet orange fruit residues are fully infiltrated, and the enzymolysis is ensured.

Condensing in the collecting process, wherein the condensing temperature is-10-8 ℃.

The extraction method of the invention is also suitable for extracting other citrus fruits.

The extraction method of the invention does not need to add other solvents, and 100% of the obtained sweet orange fruit water is from the sweet orange fruit, green and natural.

The sweet orange juice extracted by the method can be applied to the fields of skin care products, foods, health care products and the like.

Compared with the prior art, the invention has the following beneficial effects:

the sweet orange fruit water is extracted by organically combining a low-temperature vacuum (reduced pressure) technology and an enzymolysis technology, sweet orange fruits are extracted for a period of time to obtain a certain amount of primary cell extraction water, then the sweet orange fruit residues are extracted again after enzyme is added, the high permeability of the cell water is utilized, and the enzymolysis and the low-temperature vacuum (reduced pressure) extraction are carried out simultaneously, so that the cell water extraction efficiency can be accelerated, and the problem of excessive enzymolysis caused by the traditional enzymolysis method is avoided; compared with a single low-temperature-vacuum extraction technology, the extraction rate of cell water is higher, and more volatile active ingredients can be extracted.

The sweet orange juice extracted by the method is colorless, clear and transparent; is rich in more than 60 volatile active ingredients; the fruit flavor is strong, the safety is high, and the anti-inflammatory effect is achieved; has high utilization value, and can be applied to the fields of skin care products, foods, health care products and the like.

Drawings

FIG. 1 is a bar graph of the water safety test data for sweet orange fruit of example 1.

Detailed Description

The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.

In the examples and the comparative examples, fresh and full sweet orange fruits are adopted, washed and drained, sliced to be 3-5 mm in thickness, and subjected to extraction experiments.

Example 1:

putting 50kg sweet orange slices into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 35 ℃ and under the pressure of-90 kPa, forming sweet orange cell water into steam, condensing and collecting liquid, extracting for 1.5 hours to obtain primary extracted cell water and primary extracted residues, adding 200g cellulase and 20g pectinase into the primary extracted cell water, pouring into the primary extracted residues, and extracting for 5 hours again at 35 ℃ and under the pressure of-90 kPa; stirring the mixture in the whole process at 30 revolutions per minute, and condensing the mixture at-5 ℃; 36.82kg of sweet orange juice is obtained, and the sweet orange juice is colorless, clear and transparent and has strong fruit fragrance. The yield of sweet orange fruit juice is 73.6%.

Example 2:

putting 50kg sweet orange slices into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 50 ℃ under the pressure of-80 kPa, forming sweet orange cell water into steam, condensing and collecting liquid, extracting for 2.5 hours to obtain primary extracted cell water and primary extracted residue, adding 135g cellulase and 30g pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting for 4 hours again at 40 ℃ under the pressure of-90 kPa; stirring at 45 r/min in the whole process, and condensing at-5 deg.C; 35.90kg of sweet orange juice is obtained by collection, and the sweet orange juice is colorless, clear and transparent and has strong fruit fragrance. The yield of sweet orange fruit juice is 71.8%.

Example 3:

putting 50kg sweet orange slices into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 65 ℃ and under the pressure of-75 kPa, forming sweet orange cell water into steam, condensing and collecting liquid, extracting for 2 hours to obtain primary extracted cell water and primary extracted residue, adding 170g cellulase and 25g pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting again for 6 hours at 50 ℃ and under the pressure of-85 kPa; stirring at 60 r/min and condensing at-5 deg.c; 35.03kg of sweet orange juice is obtained by collection, and the sweet orange juice is colorless, clear and transparent and has strong fruit fragrance. The yield of sweet orange fruit juice is 70.1%.

Example 4:

putting 50kg sweet orange slices into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 45 ℃ under the pressure of-90 kPa, forming sweet orange cell water into steam, condensing and collecting liquid, extracting for 1.5 hours to obtain primary extracted cell water and primary extracted residue, adding 200g cellulase and 20g pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting for 5 hours again at 45 ℃ under the pressure of-90 kPa; stirring the mixture in the whole process at 30 revolutions per minute, and condensing the mixture at-5 ℃; 37.27kg of sweet orange juice is obtained, and the sweet orange juice is colorless, clear and transparent and has strong fruit fragrance. The yield of sweet orange fruit juice is 74.5%.

Example 5:

putting 50kg sweet orange slices into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 35 ℃ and under the pressure of-95 kPa, forming sweet orange cell water into steam, condensing and collecting liquid, extracting for 1.5 hours to obtain primary extracted cell water and primary extracted residue, adding 200g cellulase and 20g pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting for 5 hours again at 35 ℃ and under the pressure of-95 kPa; stirring the mixture in the whole process at 30 revolutions per minute, and condensing the mixture at-5 ℃; 38.22kg of sweet orange juice is collected, and the sweet orange juice is colorless, clear and transparent and has strong fruit fragrance. The yield of sweet orange fruit juice is 76.4%.

Comparative example 1:

putting 50kg sweet orange slices into 150L low-temperature extraction equipment, adding no solvent, extracting at 35 deg.C and-95 kPa, condensing sweet orange cell water to form vapor, collecting liquid, extracting for 6.5 hr, stirring at 30 rpm, and condensing at-5 deg.C to obtain 29.81kg sweet orange fruit water, which is colorless, clear, transparent, and light in flavor. The yield of sweet orange fruit juice is 59.6%.

Comparative example 2:

50kg of sweet orange slices are put into a 150L low-temperature extraction device, mixed with 5kg of water, 200g of cellulase and 20g of pectinase, stirred for 6.5 hours at 35 ℃ at the stirring speed of 30 r/min, and then filtered (double filtration, namely filtration by a centrifuge and filtration by a 0.22 mu m filter membrane) to obtain 38.65kg of sweet orange juice (containing 5kg of additionally added water), wherein the liquid is light yellow, tiny suspended matters can be seen, and the sweet orange juice is light in flavor and heavy in peculiar smell. The yield of sweet orange fruit juice was 67.3% (minus the weight of 5kg of water).

Comparative example 3:

putting 50kg sweet orange slices into 150L low-temperature extraction equipment, mixing with 5kg water, 200g cellulase and 20g pectinase, stirring for 50 minutes at 35 ℃, extracting for 6.5 hours at 35 ℃, condensing and collecting liquid after sweet orange cell water forms steam, stirring for 30 revolutions per minute in the whole process, condensing at-5 ℃, and collecting 38.24kg sweet orange juice (containing additional 5kg water), wherein the sweet orange juice is colorless, clear and transparent, and has light fragrance and miscellaneous taste. The yield of sweet orange fruit juice was 66.5% (minus the weight of 5kg of water).

Comparative example 4:

putting 50kg sweet orange slices into 150L low-temperature extraction equipment, adding no solvent, primarily extracting at 35 ℃ and under the pressure of-90 kPa, forming sweet orange cell water into steam, condensing and collecting liquid, extracting for 0.5 h to obtain primary extracted cell water and primary extracted residue, adding 200g cellulase and 20g pectinase into the primary extracted cell water, pouring into the primary extracted residue, and extracting for 5 h again at 35 ℃ and under the pressure of-90 kPa; stirring the mixture in the whole process at 30 revolutions per minute, and condensing the mixture at-5 ℃; 32.54kg of sweet orange juice is collected, and the sweet orange juice is colorless, clear and transparent and has light fruity flavor. The yield of sweet orange fruit juice is 65.1%.

The test methods are as follows:

1. analysis of volatile active ingredients of sweet orange fruit juice: the headspace gas quality was checked at 80 ℃ injection temperature.

(1) Instrument information: agilent 7980A GC; MS 5975C; 50/30 μm CAR/PDMS/DVB extraction fiber head, SUPELCO USA.

(2) GC-MS conditions: the chromatographic column is HP-INNOWAX capillary column (30m × 0.25mm × 0.25 μm); the carrier gas is He, the flow rate is 1mL/min, and the separation ratio is 5: 1; the sample injection temperature is 250 ℃; the temperature raising procedure is that the initial temperature is 40 ℃, the temperature is kept for 5min, the temperature is raised to 250 ℃ at the speed of 8 ℃/min, and the temperature is kept for 5 min.

Mass spectrum conditions: EI ionization source, energy 70 eV; the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, the interface temperature is 250 ℃, and the scanning range is 30-400 m/z.

(3) Sample pretreatment: 5mL of the sample and 1g of NaCl were placed in a 20mL headspace bottle, and the cap was screwed down. After 5min of equilibrium at 80 ℃ in stirring mode, extracting for 5min at 80 ℃ with a solid phase micro-extraction needle, and then resolving for 5min at the sample inlet.

The data of the volatile active ingredient analysis results of the sweet orange fruit juice of example 1 are provided and are shown in table 1.

2. Sweet orange fruit juice anti-inflammatory efficacy test: lipopolysaccharide is the main component of gram-negative bacteria cell wall, and can activate macrophage to release multiple inflammatory cytokines, so Lipopolysaccharide (LPS) is utilized to stimulate mouse mononuclear-macrophage to establish an in vitro inflammatory reaction model, samples are intervened, dexamethasone is used as a positive control, and enzyme-linked immunosorbent assay (ELISA) is used to determine the level change of inflammatory factors IL-6 and TNF-alpha, thereby discussing the in vitro anti-inflammatory action and anti-inflammatory mechanism of the samples. The level of inflammatory factors in normal cells was used as a blank control. The results of the test for the sweet orange fruit water of example 1 are provided in table 2.

3. Sweet orange fruit water safety test: the HaCaT cell is a human immortal epidermal cell line, has cytotoxicity to the HaCaT cell, and can be used as reference data for safety of skin. The normal cells are in vigorous metabolism, succinate dehydrogenase in mitochondria can reduce tetrazolium salt substances into colored crystalline substances and deposit the crystalline substances around the cells, OD values can be read by an enzyme labeling instrument according to the change, and the relative growth condition of the cells can be known by comparing the OD values with a blank control group. The results of the safety tests for sweet orange fruit water of example 1 are provided, see figure 1.

The data in FIG. 1 shows that the sweet orange juice extracted by the method of the present invention has no toxicity to human body skin cells and high safety.

Table 1: example 1 analysis of volatile active ingredients from orange fruit juice (Low match and relative content of ingredients not shown)

Table 2: example 1 orange fruit juice anti-inflammatory efficacy test results

Sweet orange fruit Water concentration	IL-6(pg/mL)	TNF-α(pg/mL)
			100％	31	151
80％	34	154
			40％	37	160
15％	42	193
			10％	44	215
5％	47	234
			Blank space	25	150
LPS stimulation	50	260
			Dexamethasone	45	206

As can be seen from the data in Table 2, the concentration of 15% sweet orange fruit water can cause the IL-6 expression factor to be obviously reduced after the skin is stimulated by LPS; the orange juice with the concentration of 100 percent can reduce the TNF-alpha expression factor of the skin after being stimulated by LPS to be in a normal range; the sweet orange juice extracted by the method has certain anti-inflammatory effect.

Table 3: the main volatile active ingredient content of the sweet orange fruit water of the examples and comparative examples and the results of the preservation challenge test

Continuing with Table 3:

analysis of the process results of the examples and comparative examples:

compared with the comparative example, the sweet orange juice is extracted by organically combining a low-temperature vacuum (reduced pressure) technology and an enzymatic hydrolysis method, the extraction rate is high, and the obtained sweet orange juice is rich in volatile active ingredients and high in utilization value.

In particular, the comparative example 1 adopts a single low-temperature-vacuum extraction technology, has low extraction rate, less components and light fragrance. As can be seen from the comparative example 2, the sweet orange fruit water obtained by the single enzyme extraction method contains more impurities and has heavy peculiar smell, the extracting solution is diluted due to the additional addition of water as an enzymolysis solvent, and meanwhile, the volatile active ingredients extracted are few, so that the fragrance is light, and the utilization value is not high. Comparative example 3 the sweet orange slices are firstly subjected to enzymolysis for a period of time and then extracted by adopting a low-temperature-vacuum (reduced pressure) technology, so that the problem of foreign flavor caused by excessive enzymolysis can be caused; and water is used as an enzymolysis solvent, and due to poor water permeability and dilution of the extracting solution by additional water, the defects of low extraction rate, light cell water flavor and the like are caused. As can be seen from comparative example 4, since the initial extraction time was too short, the initial extraction cell water was too small, resulting in too low a degree of enzymatic hydrolysis, and the extraction rate was lower and the content of active ingredient was less resulting in less flavor than that of example 1.

Claims

1. The extraction method of the sweet orange juice is characterized by comprising the following steps: adding no solvent, primarily extracting sweet orange fruits at the temperature of 30-65 ℃ and under the pressure of-60 kPa to-101 kPa, forming steam in sweet orange cell water, condensing and collecting liquid, extracting for 1.5-2.5 hours to obtain primary cell water and primary sweet orange fruit residues, adding 0.25-0.45 percent of cellulase and 0-0.1 percent of pectinase based on the total weight of the primary sweet orange into the primary cell water, pouring the mixture into the primary sweet orange fruit residues, extracting for 4-6 hours again under the conditions of the temperature of 35-50 ℃ and the pressure of-85 kPa to-101 kPa, and collecting the sweet orange fruit water.

2. The method for extracting sweet orange fruit water as claimed in claim 1, wherein the preliminary extraction temperature is 35-50 ℃ and the pressure condition is-85 kPa-101 kPa.

3. The method for extracting sweet orange fruit water as claimed in claim 1, wherein the adding amount of cellulase is 0.3% -0.4%, and the adding amount of pectinase is 0.02% -0.06%.

4. The extraction method of sweet orange fruit water as claimed in claim 1, wherein stirring is carried out during the extraction process, and the stirring speed is 1-150 rpm.

5. The method of claim 1, wherein the condensing is performed during the collection process, wherein the condensing temperature is between-10 ℃ and 8 ℃.

6. The extraction method of sweet orange fruit water as claimed in claim 1, wherein the sweet orange fruit slices have a thickness of 1-10 mm.

7. Application of the sweet orange juice obtained by the extraction method of any one of claims 1 to 6 in the fields of skin care products, foods and health care products.