CN112314945A - Method for preparing high-activity cranberry extract by sectional extraction method - Google Patents
Method for preparing high-activity cranberry extract by sectional extraction method Download PDFInfo
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Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The invention relates to the field of extraction of effective ingredients of plants, in particular to a method for preparing a high-activity cranberry extract by a sectional extraction method, which comprises the following steps: s1, unfreezing: taking the cranberries out of a refrigerator or a cold storage, then placing the cranberries on a placing disc for natural thawing, and picking and removing impurities such as leaves, branches and the like doped in the cranberries; s2, juicing: placing the cranberries in a juice extractor, starting the juice extractor to extract juice, closing the juice extractor after juice extraction is finished, pouring the cranberry juice onto a filter screen, and filtering the juice extracted from the cranberries by the filter screen to obtain cranberry feed liquid; s3, water extraction: the ratio of cranberry to cranberry feed liquid is 1: 4, extracting for 2 hours at normal temperature by using acid water as a solvent, and then carrying out residue-liquid separation. The cranberry juice has the beneficial effects that the water extract and the alcohol extract are adopted to carry out chromatography, the cranberry adopts the water extract and the alcohol extract to carry out chromatography, the sugar content is very low, and the cranberry juice can be dried directly after being mixed with the fruit juice or after being added with a small amount of excipient.
Description
Technical Field
The invention relates to the field of extraction of effective ingredients of plants, in particular to a method for preparing a high-activity cranberry extract by a sectional extraction method.
Background
The cranberry is very rich in nutrition, contains rich nutrient substances such as vitamin C, flavonoid, pectin, anthocyanin, procyanidine, protein, dietary fiber and the like, and has the main effects of:
preventing urinary tract infection
The cranberry has a good antibacterial effect, can acidify urine, can prevent bacteria from growing in the urethra, can prevent the bacteria from being attached to the urethra, has a good effect of preventing and treating various bacterial infections of the common urinary system of women, and is the best natural diet therapy for urethritis and cystitis.
Second, beauty treatment and face nourishing
The cranberry contains abundant vitamin C, can inhibit melanin deposition and whiten skin, and also contains natural antioxidant substances such as anthocyanin and flavonoid and pectin, and can resist free radicals, delay wrinkle growth, delay skin aging, moisten skin and play a role in maintaining beauty and keeping young. And bioflavonoid of cranberry can also prevent senile dementia.
Protecting heart and blood vessels
According to research and study, the cranberry juice has the effect of reducing blood pressure, and the cranberry contains the components such as flavonol glycosides, unsaturated fatty acids and tocotrienols, so that the cranberry juice is beneficial to regulating the cholesterol level in blood, preventing and treating arteriosclerosis and promoting blood circulation, and is beneficial to certain diseases such as cardiovascular aging, and the cranberry juice is very good for eating by some old people.
Fourthly, protecting intestines and stomach
Many people have bad intestines and stomachs, probably caused by helicobacter pylori, and cranberries are used as natural antibacterial health-care fruits, so that the cranberries are helpful for a urinary system, and can prevent bacteria such as the helicobacter pylori from being attached to the stomach wall, help to relieve symptoms such as gastric ulcer and intestinal ulcer, and help people to protect intestines and stomachs.
Chinese patent No. CN109761946A provides an extraction and separation method of cranberry anthocyanin, which comprises removing seeds from raw materials, drying, pulverizing, extracting with ethanol twice, vacuum concentrating, recovering ethanol, adding pure water, precipitating, removing impurities, and concentrating into soft extract; extracting with supercritical CO2 to obtain anthocyanin product. The extraction rate of procyanidine and anthocyanin in the whole fruit is over 90 percent by combining ethanol extraction with juicing and acid water extraction, and then the whole fruit is further refined and purified, so that the content of procyanidine is over 60 percent; the extraction method has the advantages of high extraction speed, high efficiency and low energy consumption of the anthocyanin, realizes the recycling of the solvent, and is green and environment-friendly; the method efficiently utilizes the residues (pulp and peel) of the cranberries, meets the market demand and improves the utilization value of the cranberries.
The existing cranberry extract products in the market mainly comprise three types of cranberry juice powder, whole fruit powder and extract. The extract has high content of procyanidin, but poor water solubility. The whole fruit powder contains a large amount of fiber, so that the whole fruit powder is poor in solubility and only suitable for tablets, and a liquid product cannot be used. The fruit juice powder contains organic acid and the like completely, but the contents of procyanidine and anthocyanin are low, and because the sugar content is high, an excipient needs to be added for drying, so that the content of active ingredients of the product is lower, and therefore, the development of a method for preparing the high-activity cranberry extract by a sectional extraction method is urgently needed.
Disclosure of Invention
The invention aims to provide a method for preparing a high-activity cranberry extract by a sectional extraction method, so as to solve the problems that cranberry whole fruit powder and cranberry extract provided in the background art are poor in solubility, only suitable for tablets and cannot be used in liquid products. The cranberry juice powder has low content of procyanidine and anthocyanin, high sugar content, and low content of active ingredients of the product due to the fact that an excipient is required to be added during drying.
The technical scheme of the invention is as follows: a method for preparing a high-activity cranberry extract by a sectional extraction method comprises the following steps:
s1, unfreezing: taking the cranberries out of a refrigerator or a cold storage, then placing the cranberries on a placing disc for natural thawing, and picking and removing impurities such as leaves, branches and the like doped in the cranberries;
s2, juicing: placing the cranberries in a juice extractor, starting the juice extractor for juicing, informing the juice extractor after juicing is finished, pouring the juice onto a filter screen, and filtering the juice squeezed by the cranberries by the filter screen to obtain cranberry feed liquid;
s3, water extraction: the ratio of cranberry to cranberry feed liquid is 1: 4, extracting the mixture for 2 hours at normal temperature by using acid water as a solvent, then carrying out residue-liquid separation, filtering and storing an extracting solution through a screen, and carrying out next extraction on fruit residues;
s4, alcohol extraction: adding an ethanol water solution into the pomace separated in the step S3, then heating the ethanol water solution, extracting for 2 times, 2 hours each time, then carrying out residue-liquid separation, passing the extracted fruits through a screen and storing, and treating the pomace according to a waste treatment standard;
s5, concentrating: pouring the extracting solutions obtained from S3 and S4 into a stirrer, starting the stirrer to fully stir the extracting solutions obtained from S3 and S4, performing membrane filtration or plate-and-frame filter pressing, concentrating, and concentrating until no alcohol exists and the extracting solution is ready to pass through a chromatographic column;
s6, column chromatography: diluting the concentrated solution obtained in the step S5 with water, feeding the diluted solution into macroporous adsorption resin, and treating effluent liquid according to waste liquid; washing with water: standing for 0.5-1h after adsorption, washing with purified water, and washing until effluent is clear; and (3) elution: after the water washing is finished, eluting with 2.5-3Bv of eluent, and then collecting eluent;
s7, concentrating: pouring the eluent in the S6 into a concentrator, and concentrating to obtain the solid content of between 15 and 20 percent;
s8, drying: the solid obtained in S7 is dried in a vacuum drying apparatus or by spray drying, and then dried to obtain a powder.
Further, the rotating speed of the juicer in the S2 is 4000-.
Further, the acid water of S3 is 0.1% citric acid and 0.1% hydrochloric acid, and the normal temperature is 20-30 ℃.
Further, the filter screen in the S2 is 200 meshes, and the filter screen in the S3 is 200 meshes.
Further, the S4 ethanol water solution is 65-75%, and the heating temperature is 65 +/-5 ℃.
Further, the feed-liquid ratio in the S4 is 1: 5,1: 4m/V, and the screen is 200 meshes.
Further, the temperature of S5 is set to 65 +/-5 ℃, and the pressure is set to-0.07 to-0.09 MPa.
Furthermore, the adsorption speed in the S6 is 1.5-1.7Bv/h, and the adsorption capacity of the macroporous adsorption resin is less than or equal to 30 Bv.
Further, the water washing in the S6 is carried out at a speed of 2.0-2.5Bv/h, the eluent is 65% ethanol water solution and 0.1% citric acid, and the elution flow rate is 1.0-1.2 Bv/h.
Further, the temperature of the concentration in the S7 is 65 + -5 deg.C, and the pressure of the concentration is-0.07-0.09 MPa.
The invention provides a method for preparing a high-activity cranberry extract by improving a sectional extraction method, and compared with the prior art, the method has the following improvements and advantages:
(1) the cranberry juice extracted by the method in a segmented manner contains abundant anthocyanin, procyanidine and organic acid, and can better keep the unique flavor of cranberries. The anthocyanin in the pomace can be completely extracted by acid water extraction, the procyanidin in the pulp can be better extracted by ethanol extraction, and the specific active ingredient combination of the cranberries is better kept by a product prepared by mixing three sections of extracting solutions.
(2) The cranberry juice is prepared by subjecting water extract and alcohol extract to chromatography, and has low sugar content after subjecting the cranberry to chromatography, and can be dried directly or after adding a small amount of excipient. The cranberry extract prepared by the method has good water solubility and high procyanidin content, the total procyanidin content can reach more than 60% by using a health food procyanidin detection method, and the organic acid is completely preserved.
Drawings
The invention is further explained below with reference to the figures and examples:
FIG. 1 is a schematic flow diagram of the present invention.
Detailed Description
The present invention will be described in detail with reference to fig. 1, and the technical solutions in the embodiments of the present invention will be clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A method for preparing a high-activity cranberry extract by a sectional extraction method comprises the following steps:
s1, unfreezing: taking the cranberries out of a refrigerator or a cold storage, then placing the cranberries on a placing disc for natural thawing, and picking and removing impurities such as leaves, branches and the like doped in the cranberries;
s2, juicing: putting the cranberries into a juice extractor, starting the juice extractor, setting the rotation speed of the juice extractor at 5000/min and the rotation time at 15min, extracting juice, closing the juice extractor after the juice extraction is finished, pouring the cranberry juice onto a filter screen, wherein the filter screen is 200 meshes, and filtering the juice extracted from the cranberries by the filter screen to obtain a cranberry feed liquid;
s3, water extraction: the ratio of cranberry to cranberry feed liquid is 1: 4, extracting the mixture for 2 hours at normal temperature of 30 ℃ by using acid water as a solvent and 0.1 percent citric acid and 0.1 percent hydrochloric acid as acid water, then carrying out residue-liquid separation, filtering and storing an extracting solution by using a screen, wherein the screen is 200 meshes, and carrying out next extraction on fruit residues;
s4, alcohol extraction: adding 75% ethanol aqueous solution into the pomace separated in the step S3, heating the ethanol aqueous solution at 65 ℃, extracting for 2 times for 2 hours each time, wherein the material-to-liquid ratio is 1: 5m/V, then carrying out residue-liquid separation, storing the extracted fruits after passing through a screen with 200 meshes, and treating the fruit residues according to a waste treatment standard;
s5, concentrating: pouring the extracting solutions obtained from S3 and S4 into a stirrer, starting the stirrer to fully stir the extracting solutions obtained from S3 and S4, performing membrane filtration or plate-and-frame filter pressing, concentrating, and concentrating until no alcohol is left in the chromatographic column, wherein the temperature is 65 ℃, the pressure is-0.07 MPa;
s6, column chromatography: diluting the concentrated solution obtained in the step S5 with water, putting the diluted solution on macroporous adsorption resin, wherein the adsorption speed is 1.7Bv/h, the adsorption capacity of the macroporous adsorption resin is less than or equal to 30Bv, and treating effluent liquid according to waste liquid; washing with water: standing for 1h after adsorption, washing with purified water at a speed of 2.5Bv/h, and washing until effluent is clear; and (3) elution: after the water washing is finished, 2.5-3Bv of eluent is used, the eluent is 65% ethanol water solution and 0.1% citric acid, the elution flow rate is 1.2Bv/h, then the elution is carried out, and the eluent is collected;
s7, concentrating: pouring the eluent in the S6 into a concentrator, wherein the temperature during concentration is 65 ℃, the pressure during concentration is-0.07 MPa, and the solid content is 15% after concentration;
s8, drying: the solid obtained in S7 is dried in a vacuum drying apparatus or by spray drying, and then dried to obtain a powder.
Example two
A method for preparing a high-activity cranberry extract by a sectional extraction method comprises the following steps:
s1, unfreezing: taking the cranberries out of a refrigerator or a cold storage, then placing the cranberries on a placing disc for natural thawing, and picking and removing impurities such as leaves, branches and the like doped in the cranberries;
s2, juicing: putting the cranberries into a juice extractor, starting the juice extractor, setting the rotation speed of the juice extractor at 5000/min and the rotation time at 15min, extracting juice, closing the juice extractor after the juice extraction is finished, pouring the cranberry juice onto a filter screen, wherein the filter screen is 200 meshes, and filtering the juice extracted from the cranberries by the filter screen to obtain a cranberry feed liquid;
s3, water extraction: the ratio of cranberry to cranberry feed liquid is 1: 4, extracting the mixture for 2 hours at normal temperature of 30 ℃ by using acid water as a solvent and 0.1 percent citric acid and 0.1 percent hydrochloric acid as acid water, then carrying out residue-liquid separation, filtering and storing an extracting solution by using a screen, wherein the screen is 200 meshes, and carrying out next extraction on fruit residues;
s4, alcohol extraction: adding 75% ethanol aqueous solution into the pomace separated in the step S3, heating the ethanol aqueous solution at 65 ℃, extracting for 2 times for 2 hours each time, wherein the material-to-liquid ratio is 1: 5m/V, then carrying out residue-liquid separation, storing the extracted fruits after passing through a screen with 200 meshes, and treating the fruit residues according to a waste treatment standard;
s5, concentrating: pouring the extracting solutions obtained from S3 and S4 into a stirrer, starting the stirrer to fully stir the extracting solutions obtained from S3 and S4, performing membrane filtration or plate-and-frame filter pressing, concentrating, and concentrating until no alcohol is left in the chromatographic column, wherein the temperature is 65 ℃, the pressure is-0.07 MPa;
s6, column chromatography: diluting the concentrated solution obtained in the step S5 with water, putting the diluted solution on macroporous adsorption resin, wherein the adsorption speed is 1.7Bv/h, the adsorption capacity of the macroporous adsorption resin is less than or equal to 30Bv, and treating effluent liquid according to waste liquid; washing with water: standing for 1h after adsorption, washing with purified water at a speed of 2.5Bv/h, and washing until effluent is clear; and (3) elution: after the water washing is finished, 2.5-3Bv of eluent is used, the eluent is 65% ethanol water solution and 0.1% citric acid, the elution flow rate is 1.2Bv/h, then the elution is carried out, and the eluent is collected;
s7, concentrating: pouring the eluent in the S6 into a concentrator, wherein the temperature during concentration is 65 ℃, the pressure during concentration is 0.07MPa, and the solid content is 18% after concentration;
s8, drying: the solid obtained in S7 is dried in a vacuum drying apparatus or by spray drying, and then dried to obtain a powder.
EXAMPLE III
A method for preparing a high-activity cranberry extract by a sectional extraction method comprises the following steps:
s1, unfreezing: taking the cranberries out of a refrigerator or a cold storage, then placing the cranberries on a placing disc for natural thawing, and picking and removing impurities such as leaves, branches and the like doped in the cranberries;
s2, juicing: putting the cranberries into a juice extractor, starting the juice extractor, setting the rotation speed of the juice extractor at 5000/min and the rotation time at 15min, extracting juice, closing the juice extractor after the juice extraction is finished, pouring the cranberry juice onto a filter screen, wherein the filter screen is 200 meshes, and filtering the juice extracted from the cranberries by the filter screen to obtain a cranberry feed liquid;
s3, water extraction: the ratio of cranberry to cranberry feed liquid is 1: 4, extracting the mixture for 2 hours at normal temperature of 30 ℃ by using acid water as a solvent and 0.1 percent citric acid and 0.1 percent hydrochloric acid as acid water, then carrying out residue-liquid separation, filtering and storing an extracting solution by using a screen, wherein the screen is 200 meshes, and carrying out next extraction on fruit residues;
s4, alcohol extraction: adding 75% ethanol aqueous solution into the pomace separated in the step S3, heating the ethanol aqueous solution at 65 ℃, extracting for 2 times for 2 hours each time, wherein the material-to-liquid ratio is 1: 5m/V, then carrying out residue-liquid separation, storing the extracted fruits after passing through a screen with 200 meshes, and treating the fruit residues according to a waste treatment standard;
s5, concentrating: pouring the extracting solutions obtained from S3 and S4 into a stirrer, starting the stirrer to fully stir the extracting solutions obtained from S3 and S4, performing membrane filtration or plate-and-frame filter pressing, concentrating, and concentrating until no alcohol is left in the chromatographic column, wherein the temperature is 65 ℃, the pressure is-0.07 MPa;
s6, column chromatography: diluting the concentrated solution obtained in the step S5 with water, putting the diluted solution on macroporous adsorption resin, wherein the adsorption speed is 1.7Bv/h, the adsorption capacity of the macroporous adsorption resin is less than or equal to 30Bv, and treating effluent liquid according to waste liquid; washing with water: standing for 1h after adsorption, washing with purified water at a speed of 2.5Bv/h, and washing until effluent is clear; and (3) elution: after the water washing is finished, 2.5-3Bv of eluent is used, the eluent is 65% ethanol water solution and 0.1% citric acid, the elution flow rate is 1.2Bv/h, then the elution is carried out, and the eluent is collected;
s7, concentrating: pouring the eluent in the S6 into a concentrator, wherein the temperature during concentration is 65 ℃, the pressure during concentration is-0.07 MPa, and the solid content is between 20% after concentration;
s8, drying: the solid obtained in S7 is dried in a vacuum drying apparatus or by spray drying, and then dried to obtain a powder.
The solid cranberry extracts obtained in the first example, the second example and the third example are different in content and the other conditions are the same, 1g of the solid cranberry extracts obtained in the first example, the second example and the third example are used in 100ml of water to obtain 1g of the solid cranberry extracts in the first example, which can be completely dissolved in 100ml of water, and simultaneously, the water extract and the alcohol extract are used for carrying out a chromatography process, the sugar content of the cranberry after the water extract and the alcohol extract are used for carrying out the chromatography process is low, and the cranberry can be dried directly or by adding a small amount of an excipient after being mixed with fruit juice.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for preparing a high-activity cranberry extract by a sectional extraction method is characterized by comprising the following steps of: the method comprises the following steps:
s1, unfreezing: taking the cranberries out of a refrigerator or a cold storage, then placing the cranberries on a placing disc for natural thawing, and picking and removing impurities such as leaves, branches and the like doped in the cranberries;
s2, juicing: placing the cranberries into a juice extractor, starting the juice extractor, setting the juice extractor at the rotation speed of 4000-;
s3, water extraction: the ratio of cranberry to cranberry feed liquid is 1: 4, extracting the mixture for 2 hours at normal temperature, wherein the solvent is acid water, the acid water is 0.1% citric acid and 0.1% hydrochloric acid, separating residues and liquids at the normal temperature of 20-30 ℃, filtering and storing the extracting solution through a screen, and the screen is 200 meshes, and extracting the pomace in the next step;
s4, alcohol extraction: adding an ethanol aqueous solution into the pomace separated in the step S3, wherein the ethanol aqueous solution is 65-75%, heating the ethanol aqueous solution at 65 +/-5 ℃, extracting for 2 times, 2 hours each time, and the material-liquid ratio is 1: 5,1: 4m/V, then carrying out residue-liquid separation, storing the extracting solution after passing through a screen mesh, wherein the screen mesh is 200 meshes, and treating the fruit residues according to a waste treatment standard;
s5, concentrating: pouring the extracting solutions obtained from S3 and S4 into a stirrer, starting the stirrer to fully stir the extracting solutions obtained from S3 and S4, performing membrane filtration or plate-and-frame filter pressing, concentrating, and concentrating until no alcohol exists and the extracting solution is ready to pass through a chromatographic column;
s6, column chromatography: diluting the concentrated solution obtained in the step S5 with water, loading the diluted solution on macroporous adsorption resin, wherein the adsorption speed is 1.5-1.7Bv/h, the adsorption capacity of the macroporous adsorption resin is less than or equal to 30Bv, and treating the effluent liquid according to waste liquid; washing with water: standing for 0.5-1h after adsorption, washing with purified water at 2.0-2.5Bv/h, and washing until effluent is clear; and (3) elution: after the water washing is finished, 2.5-3Bv of eluent is used, the eluent is 65% of ethanol water solution and 0.1% of citric acid, the elution flow rate is 1.0-1.2Bv/h, then the elution is carried out, and the eluent is collected;
s7, concentrating: pouring the eluent in the S6 into a concentrator, wherein the concentration temperature is 65 +/-5 ℃, the concentration pressure is-0.09-0.07 MPa, and the solid content is 15-20% after concentration;
s8, drying: the solid obtained in S7 is dried in a vacuum drying apparatus or by spray drying, and then dried to obtain a powder.
2. The method for preparing the cranberry extract in a segmented extraction manner according to claim 1, wherein the method comprises the following steps: in the S2, the rotating speed of the juicer is 4000-.
3. The method for preparing the cranberry extract in a segmented extraction manner according to claim 1, wherein the method comprises the following steps: the acid water of S3 is 0.1 percent of citric acid and 0.1 percent of hydrochloric acid, and the normal temperature is 20-30 ℃.
4. The method for preparing the cranberry extract in a segmented extraction manner according to claim 1, wherein the method comprises the following steps: the filter screen in the S2 is 200 meshes, and the filter screen in the S3 is 200 meshes.
5. The method for preparing the cranberry extract in a segmented extraction manner according to claim 1, wherein the method comprises the following steps: the S4 ethanol water solution is 65-75%, and the heating temperature is 65 +/-5 ℃.
6. The method for preparing the cranberry extract in a segmented extraction manner according to claim 1, wherein the method comprises the following steps: the feed-liquid ratio in the S4 is 1: 5,1: 4m/V, and the screen is 200 meshes.
7. The method for preparing the cranberry extract in a segmented extraction manner according to claim 1, wherein the method comprises the following steps: the temperature of S5 is set at 65 + -5 deg.C, and the pressure is set at-0.09 MPa to-0.07 MPa.
8. The method for preparing the cranberry extract in a segmented extraction manner according to claim 1, wherein the method comprises the following steps: the adsorption speed in S6 is 1.5-1.7Bv/h, and the adsorption capacity of the macroporous adsorption resin is less than or equal to 30 Bv.
9. The method for preparing the cranberry extract in a segmented extraction manner according to claim 1, wherein the method comprises the following steps: the water washing in the S6 is carried out at the speed of 2.0-2.5Bv/h, the eluent is 65% ethanol water solution and 0.1% citric acid, and the elution flow rate is 1.0-1.2 Bv/h.
10. The method for preparing the cranberry extract in a segmented extraction manner according to claim 1, wherein the method comprises the following steps: the temperature of S7 during concentration is 65 + -5 deg.C, and the pressure during concentration is-0.09-0.07 MPa.
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