CN113615780A - Preparation method and application of navel orange concentrated juice rich in various nutritional ingredients - Google Patents

Preparation method and application of navel orange concentrated juice rich in various nutritional ingredients Download PDF

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CN113615780A
CN113615780A CN202110714732.7A CN202110714732A CN113615780A CN 113615780 A CN113615780 A CN 113615780A CN 202110714732 A CN202110714732 A CN 202110714732A CN 113615780 A CN113615780 A CN 113615780A
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navel orange
concentrated juice
microfiltration
juice
concentrated
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刘常青
黄伟明
宋力飞
刘乡乡
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Guangzhou Zeli Pharmtech Co ltd
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Guangzhou Zeli Pharmtech Co ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation containing fruit or vegetable juices
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation containing fruit or vegetable juices
    • A23L2/04Extraction of juices
    • A23L2/06Extraction of juices from citrus fruits
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/385Concentrates of non-alcoholic beverages
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
    • A23L2/72Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • 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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  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Chemical & Material Sciences (AREA)
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  • Polymers & Plastics (AREA)
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Abstract

The invention provides a preparation method and application of navel orange concentrated juice, wherein the preparation method comprises the following steps: (1) pretreating raw materials; (2) extraction: adding water into the navel orange fine crushed materials obtained in the step (1), uniformly mixing, and performing emulsification extraction at the extraction temperature of 20-25 ℃ to obtain a navel orange extracting solution; (3) separating, purifying and microfiltering; (4) concentration: concentrating the obtained elution purified liquid to obtain navel orange concentrated juice A; concentrating the microfiltered clear solution into a navel orange concentrated solution with the solid content of 8-10 percent to obtain a navel orange concentrated juice B; (5) blending: uniformly mixing the microfiltration concentrated solution and the navel orange concentrated juice B according to the mass ratio of 1:1-2 to obtain navel orange concentrated juice C; and uniformly mixing the navel orange concentrated juice A and the navel orange concentrated juice B according to the mass ratio of 1:2-3 to obtain the navel orange concentrated juice D. The method can prepare the navel orange concentrated juice rich in various active ingredients, is a high-efficiency process mode suitable for large-scale production, and has quite wide market prospect.

Description

Preparation method and application of navel orange concentrated juice rich in various nutritional ingredients
Technical Field
The invention relates to the technical field of food and beverage, in particular to a preparation method and application of navel orange concentrated juice.
Background
China is a large country for producing oranges, oranges are one of the main varieties of oranges in China, and the variety resources are rich. Navel orange (Citrus sinensis osb. var. brasiliensis tanaka) is a kind of cultivar of sweet orange of Citrus of Rutaceae, and contains abundant nutrients, wherein VA and VB2The contents of Ca, Fe, sugar and heat are higher than those of other orange varieties, and the essence is the American name of 'the king of oranges', and is the main juice making variety at present. The consumption of Chinese orange juice is increased year by year, the domestic orange juice yield can not meet the demand, the total consumption of domestic concentrated orange juice in 2018 is 9.9 ten thousand t (measured by 65 Brix), and the consumption of the concentrated orange juice is 5.6 ten thousand t (measured by 65 Brix) imported from abroad. The content of Vc in the navel orange peel is extremely higher than that of the flesh. The navel orange peel has bright color, aromatic flavor and extremely high oiliness, and the peel contains a large amount of essential oil with the effects of regulating qi, invigorating spleen, eliminating dampness and reducing phlegm, thymol and other organic matters, and also contains flavonoid glycoside (such as hesperidin), natural carotenoid, pectin and other substances with physiological activity. Polymethoxyflavonoids (PMFs) are flavone compounds only existing in citrus fruits, are rich in citrus peel, and have been identified only from citrus peels so far, so that more than 60 flavonoid monomers exist, wherein the hesperidin content is highest, the distribution is widest and accounts for about 5% of dry weight, and the Polymethoxyflavonoids (PMFs) have physiological functions of resisting cancers, inhibiting tumors, resisting inflammation, resisting mutation, resisting platelet aggregation, reducing cholesterol level, resisting bacteria and the like.
At present, orange juice products on the market are various in types, but part of orange juice is reflected in flavor by adding essence and spice, the difference between the orange juice and the natural source flavor of raw materials is obvious, and the problems of nutrient component loss, rough processing and the like generally exist in part of orange juice by adopting a peeling and squeezing process. Therefore, the preparation method which can furthest retain all nutrient components and original taste of the navel orange concentrated juice, has higher yield and is suitable for large-scale production is imperative.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art. Therefore, the invention provides a preparation method and application of navel orange concentrated juice, and aims to keep full nutritional ingredients of the navel orange concentrated juice and improve the nutritional value.
Based on the above purpose, the invention provides a preparation method of navel orange concentrated juice, which comprises the following steps:
(1) pretreatment of raw materials: selecting, cleaning and crushing navel oranges to obtain navel orange fine crushed materials;
(2) extraction: adding water into the navel orange fine crushed materials obtained in the step (1), uniformly mixing, and performing emulsification extraction at the extraction temperature of 20-25 ℃ to obtain a navel orange extracting solution;
(3) separation, purification and microfiltration: centrifuging the navel orange extracting solution obtained in the step (2), taking the centrifugate, adsorbing the centrifugate by an AB-8 resin column, washing the column with pure water, eluting with ethanol with the volume fraction of 5-10%, eluting with ethanol solution with the volume fraction of 30-50%, eluting until the solid content is less than 0.5% or colorless each time, collecting the eluent eluted by the ethanol solution with the volume fraction of 30-50%, and removing alcohol until no alcohol smell exists to obtain an eluted and purified solution; additionally taking the centrifugal liquid for microfiltration to obtain a filtrate;
(4) concentration: concentrating the elution purified liquid obtained in the step (3) to obtain navel orange concentrated juice A; concentrating the microfiltration clear liquid obtained in the step (3) into navel orange concentrated solution with the solid content of 8-10 percent to obtain navel orange concentrated juice B;
(5) blending: uniformly mixing the microfiltration concentrated solution obtained in the step (3) with the navel orange concentrated juice B obtained in the step (4) according to the mass ratio of 1:1-2 to obtain navel orange concentrated juice C; uniformly mixing the navel orange concentrated juice A and the navel orange concentrated juice B according to the mass ratio of 1:2-3 to obtain navel orange concentrated juice D; and (4) mixing the microfiltration concentrated solution obtained in the step (3) with the navel orange concentrated juice A and the navel orange concentrated juice B obtained in the step (4) according to the weight ratio of 1: 0.5-1: 1-2 to obtain the navel orange concentrated juice E.
The navel orange fine pulp crushing treatment method comprises the step of crushing navel oranges into blocks before crushing treatment in the step (1), wherein the crushing treatment is to place the crushed navel oranges into blocks in a high-efficiency turbine type crusher provided with a 0.8-1.5mm screen, and add 1-3 times of extraction water for wet crushing to obtain the navel orange fine pulp. The navel orange is firstly crushed into small pieces, so that the subsequent crushing treatment is facilitated. By adopting the wet crushing mode, on one hand, the crushing is convenient, on the other hand, the presoaking treatment of the navel orange crushed aggregates is convenient, and further, the low-temperature instantaneous extraction operation is convenient to be carried out in cooperation with subsequent extraction equipment.
The circulating pressure of the emulsification extraction in the step (2) is 0.4-0.5MPa, and the extraction rate is 30-40L/min.
The rotation speed of the centrifugation is 8000-15000 r/min.
The microfiltration is carried out by adopting a ceramic membrane with the aperture of 300-600nm, the microfiltration temperature is less than or equal to 25 ℃, the microfiltration pressure is 0.15-0.2Mpa, and the flow rate of the microfiltration clear liquid is as follows: 20-25L/min. The microfiltration by adopting the ceramic membrane filter under the condition can realize better refining effect and can effectively remove part of unwanted impurity components.
Concentrating the eluted purified liquid in the step (4) by vacuum concentration, wherein the concentration temperature of the vacuum concentration is less than or equal to 60 ℃, and the vacuum degree is less than-0.07 Mpa; the concentration of the microfiltration clear liquid is membrane concentration, the aperture of the membrane concentration is 100-200nm, the temperature is less than or equal to 25 ℃, the pressure is 0.2-0.7Mpa, and the flow rate of the clear liquid is 0.65-1.2L/min. The membrane concentration has the advantages of low energy consumption, conventional concentration operation and small influence on concentrated juice.
And (3) uniformly mixing the microfiltration concentrated solution and the concentrated solution in the step (5) according to the mass ratio of 1: 1.2. The mixture ratio is the optimal mixture ratio, the taste is relatively better, and the nutrition collocation is more reasonable.
The invention also provides application of the navel orange concentrated juice prepared by the preparation method of the navel orange concentrated juice in preparing raw materials of fruit and vegetable juice.
The invention also provides application of the navel orange concentrated juice prepared by the preparation method of the navel orange concentrated juice in health-care beverage.
The invention has the beneficial effects that: according to the invention, by using a complete set of physical low-temperature extraction and concentration equipment, the extraction of related active ingredients of navel oranges is carried out under certain process parameters and conditions, and the concentrated navel orange juice rich in various active ingredients is prepared through centrifugation, purification, microfiltration and concentration, so that the concentrated navel orange juice is rich in various functional ingredients, and meanwhile, the activity of the active ingredients can be greatly reserved through the whole low-temperature extraction, and the nutritional value is high. Can ensure high extraction rate (more than or equal to 90%), simple extraction process, stable process and complete retention of nutrient components. Because the orange juice preparation method of the invention uses whole fruit for extraction, compared with the preparation method of peeling and squeezing, the preparation method of the invention can improve the effective utilization of resources. The orange juice obtained by the preparation method disclosed by the invention has the taste basically consistent with that of the raw material of navel oranges. The defects of low resource utilization rate, nutrient component loss, difference between flavor and raw materials and the like in the existing orange juice preparation process are overcome, and the method has important significance for improving the nutritional value and the taste of the orange juice.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a chromatogram for measuring vitamin C in example 1 of the present invention;
FIG. 2 is a graph showing a standard curve of total flavonoids measured in example 1 of the present invention;
FIG. 3 is a graph showing a standard curve for measuring total phenols in example 1 of the present invention;
FIG. 4 is a chromatogram of hesperidin determination in example 1 according to the present invention;
FIG. 5 is a comparison graph of the emulsification extraction and squeezing processing patterns of navel oranges in accordance with the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific embodiments below.
It is to be noted that technical terms or scientific terms used in the embodiments of the present invention should have the ordinary meanings as understood by those having ordinary skill in the art to which the present disclosure belongs, unless otherwise defined.
The invention relates to a preparation method of navel orange concentrated juice, which comprises the following steps:
(1) pretreatment of raw materials: selecting, cleaning and crushing navel oranges to obtain navel orange fine crushed materials;
(2) extraction: adding water into the navel orange fine crushed materials obtained in the step (1), uniformly mixing, and carrying out low-temperature instant extraction at the extraction temperature of 20-25 ℃ to obtain a navel orange extracting solution;
(3) separation, purification and microfiltration: centrifuging the navel orange extracting solution obtained in the step (2), taking the centrifugate, adsorbing the centrifugate by an AB-8 resin column, washing the column with pure water, eluting with ethanol with the volume fraction of 5-10%, eluting with ethanol solution with the volume fraction of 30-50%, eluting until the solid content is less than 0.5% or colorless each time, collecting the eluent eluted by the ethanol solution with the volume fraction of 30-50%, and removing alcohol until no alcohol smell exists to obtain an eluted and purified solution; additionally taking the centrifugal liquid for microfiltration to obtain a filtrate;
(4) concentration: concentrating the elution purified liquid obtained in the step (3) to obtain navel orange concentrated juice A; concentrating the microfiltration clear liquid obtained in the step (3) into navel orange concentrated solution with the solid content of 8-10 percent to obtain navel orange concentrated juice B;
(5) blending: uniformly mixing the microfiltration concentrated solution obtained in the step (3) with the navel orange concentrated juice B obtained in the step (4) according to the mass ratio of 1:1-2 to obtain navel orange concentrated juice C; uniformly mixing the navel orange concentrated juice A and the navel orange concentrated juice B according to the mass ratio of 1:2-3 to obtain navel orange concentrated juice D; and (4) mixing the microfiltration concentrated solution obtained in the step (3) with the navel orange concentrated juice A and the navel orange concentrated juice B obtained in the step (4) according to the weight ratio of 1: 0.5-1: 1-2 to obtain the navel orange concentrated juice E.
As a preferable embodiment, the step (1) of crushing the navel oranges into blocks is further carried out before the crushing treatment, wherein the crushing treatment is to put the crushed blocks of the navel oranges into a high-efficiency turbine type crusher with a 0.8-1.5mm screen, and add 1-3 times of extraction water for wet crushing to obtain the navel orange fine crushed pulp. The navel orange is firstly crushed into small pieces, so that the subsequent crushing treatment is facilitated. By adopting the wet crushing mode, on one hand, the crushing is convenient, on the other hand, the presoaking treatment of the navel orange crushed aggregates is convenient, and further, the low-temperature instantaneous extraction operation is convenient to be carried out in cooperation with subsequent extraction equipment.
In order to facilitate better low-temperature physical extraction, when homogeneous emulsification extraction equipment is adopted, the extraction parameters are that the circulating pressure is 0.4-0.5MPa, and the extraction rate is 30-40L/min.
The microfiltration in the method can be realized by adopting the existing microfiltration equipment, as a preferred embodiment, the microfiltration adopts a ceramic membrane microfiltration with the aperture of 300-600nm, the microfiltration temperature is less than or equal to 25 ℃, the microfiltration pressure is 0.15-0.2Mpa, and the flow rate of the microfiltration clear liquid is as follows: 20-25L/min. The microfiltration by adopting the ceramic membrane filter under the condition can realize better refining effect and can effectively remove part of unwanted impurity components.
Concentrating the eluted purified liquid in the step (4) by vacuum concentration, wherein the concentration temperature of the vacuum concentration is less than or equal to 60 ℃, and the vacuum degree is less than-0.07 Mpa; the concentration of the microfiltration clear liquid is membrane concentration, the aperture of the membrane concentration is 100-200nm, the temperature is less than or equal to 25 ℃, the pressure is 0.2-0.7Mpa, and the flow rate of the clear liquid is 0.65-1.2L/min. The membrane concentration has the advantages of low energy consumption, conventional concentration operation and small influence on concentrated juice.
The following is illustrated by specific examples:
example 1
Cleaning 48kg of navel orange raw materials, coarsely crushing the raw materials into small pieces by using a crusher, performing wet crushing (crushing by using a high-efficiency turbine crusher) by using 2 times of purified water through a 1.2mm screen to obtain navel orange fine crushed pulp, supplementing 8 times of purified water to the navel orange fine crushed pulp, uniformly stirring, and performing low-temperature instantaneous extraction by using an emulsification extraction device, wherein the circulating pressure is 0.4MPa, the temperature is 20 ℃, and the extraction times are 1 time; collecting and centrifuging the navel orange extracting solution, wherein the centrifugal rotating speed is 10000 r/min; adsorbing the centrifugate by an AB-8 resin column, eluting with 10% volume fraction ethanol, eluting with 35% volume fraction ethanol solution until the eluate is colorless or the solid content is less than 0.5%, collecting the eluate after eluting with 35% volume fraction ethanol solution, and removing ethanol until no ethanol smell exists to obtain an eluate; concentrating the eluate under vacuum (vacuum concentration temperature 50 deg.C and vacuum degree of-0.15 MPa) to obtain concentrated juice A; performing 500nm ceramic membrane microfiltration on the centrifugate (the microfiltration temperature is 20 ℃, the microfiltration pressure is 0.18MPa, and the filtration speed of the microfiltration clear liquid is 20L/min) to obtain microfiltration clear liquid and microfiltration concentrated liquid; performing membrane concentration on the microfiltration clear liquid (aperture: 150nm, temperature of 20 ℃, pressure of 0.5Mpa, clear liquid flow rate of 1.0L/min) to obtain navel orange concentrated solution (solid content: 9%), and mixing the microfiltration concentrated solution and the navel orange concentrated solution B according to the mass ratio of 1:1.2 to obtain navel orange concentrated solution C; uniformly mixing the navel orange concentrated juice A and the navel orange concentrated juice B according to the mass ratio of 1:2.5 to obtain navel orange concentrated juice D; mixing the microfiltration concentrated solution obtained in the step (3) with the navel orange concentrated juice A and the navel orange concentrated juice B obtained in the step (4) according to the weight ratio of 1: 0.8: and (5) uniformly mixing the raw materials according to the mass ratio of 1.5 to obtain the navel orange concentrated juice E.
Example 2
Cleaning 30kg of navel orange raw materials, coarsely crushing the raw materials into small pieces by using a crusher, performing wet crushing (crushing by using a high-efficiency turbine crusher) by using 2 times of purified water through a 1.2mm screen to obtain navel orange fine crushed pulp, supplementing 8 times of purified water to the navel orange fine crushed pulp, uniformly stirring, performing low-temperature instantaneous extraction by using an emulsification extraction device, wherein the circulating pressure is 0.45MPa, the temperature is 20 ℃, the extraction frequency is 1 time, collecting an extracting solution, and centrifuging the extracting solution, wherein the centrifuging rotation speed is 10000 r/min; adsorbing the centrifugate by an AB-8 resin column, eluting with ethanol with volume fraction of 8%, eluting with ethanol solution with volume fraction of 30%, each time until the eluate is colorless or the solid content is less than 0.5%, collecting the eluate after the ethanol solution with volume fraction of 30% is eluted, and removing ethanol until no ethanol smell exists to obtain an eluted purified solution; concentrating the eluate under vacuum (vacuum concentration temperature 50 deg.C and vacuum degree of-0.15 MPa) to obtain concentrated juice A; performing 500nm ceramic membrane microfiltration on the centrifugate (the microfiltration temperature is 20 ℃, the microfiltration pressure is 0.18MPa, and the filtration speed of the microfiltration clear liquid is 25L/min) to obtain microfiltration clear liquid and microfiltration concentrated liquid; performing membrane concentration on the microfiltration clear liquid (aperture: 150nm, temperature of 20 ℃, pressure of 0.5Mpa, clear liquid flow rate of 0.7L/min) to obtain navel orange concentrated solution (solid content: 10%), and mixing the microfiltration concentrated solution and the navel orange concentrated solution B according to the mass ratio of 1:1.2 to obtain navel orange concentrated solution C; uniformly mixing the navel orange concentrated juice A and the navel orange concentrated juice B according to the mass ratio of 1:2 to obtain navel orange concentrated juice D; mixing the microfiltration concentrated solution obtained in the step (3) with the navel orange concentrated juice A and the navel orange concentrated juice B obtained in the step (4) according to the ratio of 1:2 to obtain the navel orange concentrated juice E.
Comparative example 1
Cleaning 48kg of navel orange raw materials, coarsely crushing the raw materials into small pieces by using a crusher, performing wet crushing (crushing by using a high-efficiency turbine crusher) by using 2 times of purified water through a 1.2mm screen to obtain navel orange fine crushed pulp, supplementing 8 times of purified water to the navel orange fine crushed pulp, uniformly stirring, and performing low-temperature instantaneous extraction by using an emulsification extraction device, wherein the circulating pressure is 0.4MPa, the temperature is 20 ℃, and the extraction times are 1 time; collecting the extract, and centrifuging at 10000 r/min; then carrying out microfiltration on the collected centrifugate by using a 500nm ceramic membrane (the microfiltration temperature is 20 ℃, the microfiltration pressure is 0.18MPa, and the filtration speed of the microfiltration clear liquid is 30L/min) to obtain microfiltration clear liquid and microfiltration concentrated liquid; and (3) carrying out membrane concentration on the microfiltration clear liquid (aperture: 150nm, temperature of 20 ℃, pressure of 0.5Mpa and clear liquid flow rate of 1.0L/min) to obtain navel orange concentrated solution (solid content: 9%), and compounding the microfiltration concentrated solution and the concentrated solution according to the ratio of 1:0.5 (stirring for 3min) to obtain the navel orange concentrated juice.
Comparative example 2
Cleaning 48kg of navel orange raw materials, coarsely crushing into small pieces by using a crusher, crushing by using the crusher to obtain navel orange fine crushed materials, supplementing purified water which is 5 times of the navel orange fine crushed materials, uniformly stirring, and heating for extraction, wherein the extraction time is 3 hours; collecting the extract, and centrifuging at 10000 r/min; then carrying out microfiltration on the collected centrifugate by using a 500nm ceramic membrane (the microfiltration temperature is 20 ℃, the microfiltration pressure is 0.18MPa, and the filtration speed of the microfiltration clear liquid is 20L/min) to obtain microfiltration clear liquid and microfiltration concentrated liquid; and (3) carrying out membrane concentration on the microfiltration clear liquid (aperture: 150nm, temperature of 20 ℃, pressure of 0.5Mpa and clear liquid flow rate of 1.0L/min) to obtain navel orange concentrated solution (solid content: 9%), and compounding the microfiltration concentrated solution and the concentrated solution according to the ratio of 1:1.2 (stirring for 3min) to obtain the navel orange concentrated juice.
Comparative example 3
Cleaning 48kg of navel orange raw materials, coarsely crushing into small pieces by using a crusher, crushing by using the crusher to obtain navel orange fine crushed materials, supplementing 95% ethanol to the navel orange fine crushed materials, uniformly stirring, and performing reflux extraction for 3 hours; (ii) a Collecting the extract, and centrifuging at 10000 r/min; then carrying out microfiltration on the collected centrifugate by using a 500nm ceramic membrane (the microfiltration temperature is 20 ℃, the microfiltration pressure is 0.18MPa, and the filtration speed of the microfiltration clear liquid is 20L/min) to obtain microfiltration clear liquid and microfiltration concentrated liquid; and (3) carrying out membrane concentration on the microfiltration clear liquid (aperture: 150nm, temperature of 20 ℃, pressure of 0.5Mpa and clear liquid flow rate of 1.0L/min) to obtain navel orange concentrated solution (solid content: 9%), and compounding the microfiltration concentrated solution and the concentrated solution according to the ratio of 1:1.2 (stirring for 3min) to obtain the navel orange concentrated juice.
Comparative example 4
Cleaning 48kg of navel orange raw materials, coarsely crushing the raw materials into small pieces by using a crusher, performing wet crushing (crushing by using a high-efficiency turbine crusher) by using 2 times of purified water through a 1.2mm screen to obtain navel orange fine crushed pulp, supplementing 8 times of purified water to the navel orange fine crushed pulp, uniformly stirring, and performing low-temperature instantaneous extraction by using an emulsification extraction device, wherein the circulating pressure is 0.4MPa, the temperature is 20 ℃, and the extraction times are 1 time; collecting the extract, and centrifuging at 10000 r/min; adsorbing the centrifugate by an AB-8 resin column, eluting by using ethanol with the volume fraction of 10 percent, eluting by using ethanol solution with the volume fraction of 35 percent, collecting eluent after the elution of the ethanol solution with the volume fraction of 35 percent, and then carrying out 500nm ceramic membrane microfiltration (the microfiltration temperature is 20 ℃, the microfiltration pressure is 0.18MPa, and the filtration speed of the microfiltration clear liquid is 20L/min) on the collected eluent to obtain microfiltration clear liquid and microfiltration concentrated liquid; obtaining the navel orange concentrated juice.
Comparative example 5
Cleaning 48kg of navel orange raw materials, squeezing, collecting liquid after squeezing, and centrifuging at the rotation speed of 10000 r/min; adsorbing the centrifugate by an AB-8 resin column, eluting by using ethanol with the volume fraction of 10 percent, eluting by using ethanol solution with the volume fraction of 35 percent, collecting eluent after the elution of the ethanol solution with the volume fraction of 35 percent, and then carrying out 500nm ceramic membrane microfiltration (the microfiltration temperature is 20 ℃, the microfiltration pressure is 0.18MPa, and the filtration speed of the microfiltration clear liquid is 20L/min) on the collected eluent to obtain microfiltration clear liquid and microfiltration concentrated liquid; and (3) carrying out membrane concentration on the microfiltration clear liquid (aperture: 150nm, temperature of 20 ℃, pressure of 0.5Mpa and clear liquid flow rate of 1.0L/min) to obtain navel orange concentrated solution (solid content: 9%), and compounding the microfiltration concentrated solution and the concentrated solution according to the ratio of 1:1.2 (stirring for 3min) to obtain the navel orange concentrated juice.
Verification experiment
(1) Vitamin C is measured by high performance liquid chromatography (GB/T5009.86-2016 first method).
(2) Method for measuring total flavonoids
A. Sample preparation
Precisely weighing 2.0000g of sample in a conical flask with a plug, precisely adding 25mL of 30% ethanol, weighing, ultrasonically treating for 30min, weighing again, supplementing the lost weight with 30% ethanol, shaking up, and collecting the subsequent filtrate.
B. Preparation of Standard Curve
Accurately sucking 0, 1.00, 2.00, 3.00, 4.00 and 6.00mL of rutin standard solution, respectively placing in a 25mL brown volumetric flask, adding water to 6mL, adding 1mL of 5% sodium nitrite solution, uniformly mixing, placing for 6min, adding 1mL of 10% aluminum nitrate solution, shaking up, placing for 6min, adding 10mL of 4.3% sodium hydroxide test solution, adding water to scale, shaking up, placing for 15min, measuring the absorbance value by using a spectrophotometer at 510nm wavelength with a reagent blank solution as a reference and a 1cm cuvette. And drawing a standard curve by taking the concentration of rutin as a horizontal coordinate and the absorbance value as a vertical coordinate.
C. Measurement of
Precisely measuring 1mL of a test sample solution, placing the test sample solution in a 25mL brown volumetric flask, adding water to 6mL, adding 1mL of 5% sodium nitrite solution, uniformly mixing, placing for 6min, adding 1mL of 10% aluminum nitrate solution, shaking up, placing for 6min, adding 10mL of 4.3% sodium hydroxide test solution, adding water to the scale, shaking up, placing for 15min, using a corresponding reagent as a blank, and measuring the light absorption value at the wavelength of 510 nm.
(3) Total phenol determination method
A. Sample preparation
Precisely weighing 2.0000g of a sample into a 250mL brown measuring flask, adding 150mL of water, standing overnight, performing ultrasonic treatment for 10min, cooling, diluting with water to a scale, shaking up, standing (precipitating solids), filtering, discarding 50mL of primary filtrate, precisely weighing 20mL of subsequent filtrate, placing into a 100mL brown measuring flask, diluting with water to a scale, and shaking up to obtain the product.
B. Preparation of Standard Curve
Accurately measuring 0mL, 0.5 mL, 1.0mL, 2.0mL, 4.0 mL and 5.0mL of gallic acid standard solution, respectively placing in a 25mL brown volumetric flask, respectively adding 1mL of phosphomolybdic tungstic acid test solution, respectively adding 12.0mL, 11.5mL, 11.0mL, 10.0mL, 8.0mL and 7.0mL of water, diluting to scale with 29% sodium carbonate solution, shaking uniformly, standing for 30min to blank corresponding reagents, measuring absorbance at 760nm wavelength, and drawing a standard curve.
C. Measurement of
Precisely measuring 1mL of test solution, placing the test solution in a 25mL brown volumetric flask, adding 10mL of water from the step of adding 1mL of phosphomolybdic tungstic acid test solution according to the method under the standard curve preparation, and measuring the absorbance according to the method.
(4) Hesperidin determination method
A. Sample preparation
Weighing two samples in parallel, putting 10g (accurate to 0.01g) of each sample in a 50mL volumetric flask, adding 10mL of ammonium oxalate solution, then adding 10mL of dimethylformamide, mixing uniformly, adding water to a constant volume, pouring into a 100mL conical flask, placing in a 90 ℃ water bath kettle for 10min, cooling to room temperature, taking supernatant, and filtering through a filter membrane (water phase) to obtain a solution to be detected.
B. Reference conditions of the apparatus
A chromatographic column: c18 column (particle size 5 μm,4.6 mm. times.250 mm) or column of equivalent performance.
Mobile phase: acetic acid solution + methanol 65+35
Column temperature: 35 deg.C
Flow rate: 0.80mL/min
Sample introduction amount: 10 μ L
Detection wavelength: 283 nm.
C. Preparation of Standard Curve
Taking the standard stock solution, diluting the stock solution with acetic acid solution and dimethylformamide solution (the volume ratio of the acetic acid solution to the dimethylformamide solution is 8:2) to prepare standard working solutions with the mass concentrations of 1.0mg/L, 5.0mg/L, 10mg/L, 15mg/L, 30mg/L, 60mg/L and 120mg/L, and determining according to the condition B. And calculating a standard curve or solving a linear regression equation by taking the mass concentrations of the hesperidin and the naringin as horizontal coordinates and the corresponding integrated peak areas as vertical coordinates.
D. Measurement of
Two samples were measured in parallel. Sequentially sampling 10 μ L of the solution to be detected and corresponding standard working solution, determining the retention time, and determining the response values of hesperidin and naringin in the sample solution within the quantitative determination range by taking the chromatographic peak area integral value as the quantification.
(5) The results of comparing the retention rates of the effective components by detecting the effective components of the concentrated navel orange juice in each example and each comparative example are shown in the table
TABLE 1 effective component Retention ratio of concentrated juice of navel orange
Figure BDA0003134420160000131
Note: the retention rate of the effective components in the concentrated navel orange juice is divided by the content of the effective components in the concentrated navel orange juice and the content of the effective components in the raw material of the navel orange is multiplied by 100 percent
As can be seen from table 1, the retention rates of the effective components in the navel orange concentrated juice prepared from the raw material of the navel orange are the highest in example 1, wherein the retention rates of the total flavonoids, the total phenols, the hesperidin and the vitamin C in the navel orange concentrated juice E respectively reach 86.7%, 88.7%, 75.3% and 70.9%. Compared with the comparative example 1, the macroporous resin adsorption procedure is not carried out, the retention rate of each effective component is obviously reduced, and particularly the effective components such as flavonoid and the like are reduced. The concentrated juice of navel orange prepared by the hot reflux extraction method in the comparative examples 2 and 3 has obviously damaged mouthfeel and flavor, and the retention rate of heat-sensitive active ingredients such as vitamin C and the like is far lower than that of the emulsification extraction method. The comparison of navel orange emulsification extraction and squeezing treatment maps shows that the squeezing treatment can not fully destroy plant cells, so that nutrient substances in the navel oranges can not be fully released, and the utilization rate of effective components is low.
The macroporous adsorption resin adsorption purification process can obviously improve the content of each effective component in the navel orange concentrated juice, but the process takes longer time; the combined microfiltration and concentration process can control the temperature below 25 ℃ for rapid refining and concentration, effectively removes specific impurities and effectively retains the flavor and taste of the navel oranges. The invention organically combines all working procedures, realizes the consistency of the taste and the flavor of the navel orange concentrated juice with the original materials, and simultaneously improves the retention rate of all effective components to the maximum extent.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, is limited to these examples; within the idea of the invention, also features in the above embodiments or in different embodiments may be combined, steps may be implemented in any order, and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The embodiments of the invention are intended to embrace all such alternatives, modifications and variances that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, substitutions, improvements and the like that may be made without departing from the spirit and principles of the invention are intended to be included within the scope of the invention.

Claims (9)

1. A preparation method of navel orange concentrated juice is characterized by comprising the following steps:
(1) pretreatment of raw materials: selecting, cleaning and crushing navel oranges to obtain navel orange fine crushed materials;
(2) extraction: adding water into the navel orange fine crushed materials obtained in the step (1), uniformly mixing, and performing emulsification extraction at the extraction temperature of 20-25 ℃ to obtain a navel orange extracting solution;
(3) separation, purification and microfiltration: centrifuging the navel orange extracting solution obtained in the step (2), taking the centrifugate, adsorbing the centrifugate by an AB-8 resin column, washing the column with pure water, eluting with ethanol with the volume fraction of 5-10%, eluting with ethanol solution with the volume fraction of 30-50%, eluting until the solid content is less than 0.5% or colorless each time, collecting the eluent eluted by the ethanol solution with the volume fraction of 30-50%, and removing alcohol until no alcohol smell exists to obtain an eluted and purified solution; additionally taking the centrifugal liquid for microfiltration to obtain a filtrate and a microfiltration concentrated solution;
(4) concentration: concentrating the elution purified liquid obtained in the step (3) to obtain navel orange concentrated juice A; concentrating the microfiltration clear liquid obtained in the step (3) into navel orange concentrated solution with the solid content of 8-10 percent to obtain navel orange concentrated juice B;
(5) blending: uniformly mixing the microfiltration concentrated solution obtained in the step (3) with the navel orange concentrated juice B obtained in the step (4) according to the mass ratio of 1:1-2 to obtain navel orange concentrated juice C; uniformly mixing the navel orange concentrated juice A and the navel orange concentrated juice B according to the mass ratio of 1:2-3 to obtain navel orange concentrated juice D; and (4) mixing the microfiltration concentrated solution obtained in the step (3) with the navel orange concentrated juice A and the navel orange concentrated juice B obtained in the step (4) according to the weight ratio of 1: 0.5-1: 1-2 to obtain the navel orange concentrated juice E.
2. The method for preparing concentrated juice of navel orange according to claim 1, wherein the step of crushing navel orange into pieces is further included before the crushing treatment in step (1), and the crushing treatment is carried out by putting the crushed pieces of navel orange into a high-efficiency turbine type crusher with a 0.8-1.5mm screen, adding 1-3 times of extraction water, and carrying out wet crushing to obtain the fine pulp of navel orange.
3. The method for preparing concentrated juice from navel orange according to claim 1, wherein the circulation pressure of the emulsification extraction in step (2) is 0.4-0.5MPa, and the extraction rate is 30-40L/min.
4. The method for preparing concentrated juice from navel orange according to claim 1, wherein the rotation speed of the centrifugation is 8000-.
5. The method for preparing concentrated juice of navel orange according to claim 1, wherein the microfiltration is performed by using a ceramic membrane with a pore size of 600nm and a microfiltration temperature of less than or equal to 25 ℃, a microfiltration pressure of 0.15-0.2Mpa, a microfiltration clear liquid flow rate: 20-25L/min.
6. The method for preparing the concentrated juice of navel orange according to claim 1, wherein the concentration of the elution purified liquid in the step (4) adopts vacuum concentration, the concentration temperature of the vacuum concentration is less than or equal to 60 ℃, and the vacuum degree is less than-0.07 Mpa; the concentration of the microfiltration clear liquid is membrane concentration, the aperture of the membrane concentration is 100-200nm, the temperature is less than or equal to 25 ℃, the pressure is 0.2-0.7Mpa, and the flow rate of the clear liquid is 0.65-1.2L/min.
7. The method for preparing the navel orange concentrated juice according to claim 1, wherein the microfiltration concentrated solution and the concentrated solution are uniformly mixed according to the mass ratio of 1:1.2 in the step (5).
8. Use of the navel orange juice concentrate produced by the method of any one of claims 1 to 7 in fruit and vegetable juice formulations.
9. Use of the navel orange juice concentrate produced by the method of any one of claims 1 to 7 in a health beverage.
CN202110714732.7A 2021-06-25 2021-06-25 Preparation method and application of navel orange concentrated juice rich in various nutritional ingredients Pending CN113615780A (en)

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