CN114573731B - Extraction process of carrageenan - Google Patents
Extraction process of carrageenan Download PDFInfo
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- CN114573731B CN114573731B CN202210454047.XA CN202210454047A CN114573731B CN 114573731 B CN114573731 B CN 114573731B CN 202210454047 A CN202210454047 A CN 202210454047A CN 114573731 B CN114573731 B CN 114573731B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0036—Galactans; Derivatives thereof
- C08B37/0039—Agar; Agarose, i.e. D-galactose, 3,6-anhydro-D-galactose, methylated, sulfated, e.g. from the red algae Gelidium and Gracilaria; Agaropectin; Derivatives thereof, e.g. Sepharose, i.e. crosslinked agarose
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Abstract
The invention discloses an extraction process of a corrugated wave carrageenan, which comprises the following steps: washing and cutting the carrageenan, adding the carrageenan into an ethanol aqueous solution, stirring at constant temperature, and filtering to obtain a first extract and a first filter residue; freezing the first filter residue, pulverizing into fine powder, adding into ethanol, performing ultrasonic treatment for 0.5-1 hr, adding distilled water containing alkaline substances, performing ultrasonic treatment for 2-4 hr, and filtering to obtain second extractive solution and second filter residue; adding the second filter residue into distilled water, steaming at constant temperature for 2-3h, naturally cooling and press-filtering to obtain a third extract and a third filter residue; mixing the first, second and third extractive solutions, stirring at constant temperature for 2-5 hr to obtain concentrated solution, vacuum distilling the concentrated solution, and freeze drying to obtain herba Chenopodii Aromati extract. The invention solves the problem of residue of the existing corrugated carrageenan filter residue, and improves the extraction quantity by combining the alcohol extraction and the water extraction, thereby achieving the full extraction of active substances.
Description
Technical Field
The invention belongs to the technical field of extraction, and particularly relates to an extraction process of carrageenan.
Background
The carrageenan extract is one of natural polymer materials allowed to be used in the catalogue of national skin care or cosmetic raw materials, is a pure natural marine product, mainly comprises polysaccharide components in seaweed, and has unique skin feel. Has high water solubility, and can promote skin metabolism, stimulate fibroblast to produce more colloid, elastic scleroprotein and mucopolysaccharide, promote epidermal cell growth, promote metabolism, and prevent skin aging. In summary, the Chondrus crispus extract has the effects of expelling toxin, deeply cleaning, removing aged cutin, tightening skin, moistening and removing wrinkles, and the skin becomes fine and bright immediately after use. At present, the extraction process of the carrageenan is mainly based on alkali extraction, but the extracted residues still contain a plurality of active substances, so that the resource waste is caused.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an extraction process of the carrageen, solves the problem of residue of the carrageen, and improves the extraction quantity by combining alcohol extraction and water extraction so as to fully extract active substances.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
an extraction process of carrageenan, comprising the following steps:
step 1, cleaning and chopping the carrageen, then adding the carrageen into an ethanol water solution, stirring at constant temperature, and filtering to obtain a first extract and first filter residues; the volume concentration of the ethanol in the ethanol water solution is 50-70%, and the constant-temperature stirring temperature is 50-60 ℃; the method comprises the steps of chopping the carrageenan, and performing alcohol-water extraction to form primary extraction;
step 2, freezing the first filter residue, crushing into fine powder, putting the fine powder into ethanol, carrying out ultrasonic treatment for 0.5-1h, then adding distilled water containing alkaline substances, carrying out secondary ultrasonic treatment for 2-4h, and filtering to obtain a second extract and a second filter residue, wherein the temperature of the freezing treatment is-10 to-15 ℃, the adding amount of the ethanol is 60-90% of the mass of the first filter residue, the ultrasonic frequency is 40-60kHz, the temperature is 0-5 ℃, the alkaline substances in the distilled water are sodium hydroxide, the pH value is 8, the adding amount of the distilled water is 200-300% of the volume of the ethanol, the temperature of the secondary ultrasonic treatment is 50-60 ℃, and the ultrasonic frequency is 50-80kHz; the step utilizes a low-temperature freezing mode to convert the chopped first filter residues into a frozen state, and pulverizes the first filter residues in the frozen state, so that the whole filter residues can be pulverized under the condition of not damaging active substances; when the ethanol is subjected to first ultrasonic treatment, the low-temperature environment can ensure that the crushed fine powder forms slow thawing from outside to inside, so that the thawing effect of gradual release is achieved, the effect of full alcohol extraction is achieved, after distilled water is added, the alkaline environment can realize alkaline water extraction of the fine powder, and cells produce respiratory effect, so that the internal environment is converted, and the internal alkaline water extraction is realized, so that the full extraction of the inside and the outside is achieved;
step 3, adding the second filter residue into distilled water, performing constant-temperature cooking for 2-3h, naturally cooling and press-filtering to obtain a third extracting solution and a third filter residue, wherein the mass ratio of the second filter residue to the distilled water is 1:5-10, and the constant-temperature cooking temperature is 80-90 ℃; the pH is adjusted to 8 before constant temperature cooking, and sodium hydroxide is adopted for pH adjustment; the step of curing the second filter residue by utilizing a constant-temperature cooking mode, ensuring the smoothness of the inner side and the outer side of the cell wall, facilitating the extraction of internal substances, simultaneously, completely compressing cured cells by pressure filtration, discharging active substances in the cell wall in the flowing process of liquid, and separating the active substances into a third extracting solution;
step 4, mixing the first extract, the second extract and the third extract, stirring at constant temperature for 2-5 hours to obtain a concentrated solution, then distilling the concentrated solution under reduced pressure, and freeze-drying to obtain the carrageenan extract, wherein the constant temperature stirring temperature is 80-90 ℃, the stirring speed is 1000-2000r/min, the pressure of the reduced pressure distillation is 80-90% of atmospheric pressure, and the temperature is 90-95 ℃; the ethanol is completely removed by stirring at constant temperature to form concentrated solution with water extraction structure, and the extract is completely retained by secondary concentration of reduced pressure distillation to obtain stable active substance.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of residue of the existing corrugated carrageenan filter residue, and improves the extraction quantity by combining the alcohol extraction and the water extraction, thereby achieving the full extraction of active substances.
2. The invention utilizes the change of cell activity and the respiratory effect of the cell thawing process to realize gradient extraction, and fully extracts active substances inside and outside the cell wall, thereby improving the extraction efficiency.
Description of the embodiments
The invention is described in detail with reference to examples, but without any limitation to the claims of the invention.
Examples
An extraction process of carrageenan, comprising the following steps:
step 1, cleaning and chopping the carrageen, then adding the carrageen into an ethanol water solution, stirring at constant temperature, and filtering to obtain a first extract and first filter residues; the volume concentration of the ethanol in the ethanol water solution is 50 percent, and the constant-temperature stirring temperature is 50 ℃;
step 2, carrying out freeze treatment on the first filter residue, crushing the first filter residue into fine powder, putting the fine powder into ethanol, carrying out ultrasonic treatment for 0.5h, then adding distilled water containing alkaline substances, carrying out secondary ultrasonic treatment for 2h, and filtering to obtain second extract and second filter residue, wherein the temperature of the freeze treatment is-10 ℃, the adding amount of the ethanol is 60% of the mass of the first filter residue, the ultrasonic frequency is 40kHz, the temperature is 0 ℃, the alkaline substances in the distilled water are sodium hydroxide, the pH is 8, the adding amount of the distilled water is 200% of the volume of the ethanol, the temperature of the secondary ultrasonic treatment is 50 ℃, and the ultrasonic frequency is 50kHz;
step 3, adding the second filter residue into distilled water, performing constant-temperature cooking for 2 hours, naturally cooling and press-filtering to obtain a third extracting solution and a third filter residue, wherein the mass ratio of the second filter residue to the distilled water is 1:5, and the constant-temperature cooking temperature is 80 ℃; the pH is adjusted to 8 before constant temperature cooking, and sodium hydroxide is adopted for pH adjustment;
and 4, mixing the first extract, the second extract and the third extract, stirring at constant temperature for 2 hours to obtain a concentrated solution, then distilling the concentrated solution under reduced pressure, and freeze-drying to obtain the carrageenan extract, wherein the constant temperature stirring temperature is 80 ℃, the stirring speed is 1000r/min, the pressure of the reduced pressure distillation is 80% of the atmospheric pressure, and the temperature is 90 ℃.
Examples
An extraction process of carrageenan, comprising the following steps:
step 1, cleaning and chopping the carrageen, then adding the carrageen into an ethanol water solution, stirring at constant temperature, and filtering to obtain a first extract and first filter residues; the volume concentration of the ethanol in the ethanol water solution is 70 percent, and the constant-temperature stirring temperature is 60 ℃;
step 2, carrying out freeze treatment on the first filter residue, crushing the first filter residue into fine powder, putting the fine powder into ethanol, carrying out ultrasonic treatment for 1h, then adding distilled water containing alkaline substances, carrying out ultrasonic treatment for 4h, and filtering to obtain second extract and second filter residue, wherein the temperature of the freeze treatment is-15 ℃, the adding amount of the ethanol is 90% of the mass of the first filter residue, the ultrasonic frequency is 60kHz, the temperature is 5 ℃, the alkaline substances in the distilled water are sodium hydroxide, the pH is 8, the adding amount of the distilled water is 300% of the volume of the ethanol, the temperature of the ultrasonic treatment for the second time is 60 ℃, and the ultrasonic frequency is 80kHz;
step 3, adding the second filter residue into distilled water, performing constant-temperature cooking for 3 hours, naturally cooling and press-filtering to obtain a third extracting solution and a third filter residue, wherein the mass ratio of the second filter residue to the distilled water is 1:10, and the constant-temperature cooking temperature is 90 ℃; the pH is adjusted to 8 before constant temperature cooking, and sodium hydroxide is adopted for pH adjustment;
and 4, mixing the first extract, the second extract and the third extract, stirring at constant temperature for 5 hours to obtain a concentrated solution, then distilling the concentrated solution under reduced pressure, and freeze-drying to obtain the carrageenan extract, wherein the constant temperature stirring temperature is 90 ℃, the stirring speed is 2000r/min, the pressure of the reduced pressure distillation is 90% of the atmospheric pressure, and the temperature is 95 ℃.
Examples
An extraction process of carrageenan, comprising the following steps:
step 1, cleaning and chopping the carrageen, then adding the carrageen into an ethanol water solution, stirring at constant temperature, and filtering to obtain a first extract and first filter residues; the volume concentration of the ethanol in the ethanol water solution is 60 percent, and the constant-temperature stirring temperature is 55 ℃;
step 2, carrying out freeze treatment on the first filter residue, crushing the first filter residue into fine powder, putting the fine powder into ethanol, carrying out ultrasonic treatment for 1h, then adding distilled water containing alkaline substances, carrying out ultrasonic treatment for 3h, filtering to obtain second extract and second filter residue, wherein the temperature of the freeze treatment is-12 ℃, the adding amount of the ethanol is 70% of the mass of the first filter residue, the ultrasonic frequency is 50kHz, the temperature is 2 ℃, the alkaline substances in the distilled water are sodium hydroxide, the pH is 8, the adding amount of the distilled water is 200-300% of the volume of the ethanol, the temperature of the ultrasonic treatment for the second time is 55 ℃, and the ultrasonic frequency is 70kHz;
step 3, adding the second filter residue into distilled water, performing constant-temperature cooking for 3 hours, naturally cooling and press-filtering to obtain a third extracting solution and a third filter residue, wherein the mass ratio of the second filter residue to the distilled water is 1:6, and the constant-temperature cooking temperature is 85 ℃; the pH is adjusted to 8 before constant temperature cooking, and sodium hydroxide is adopted for pH adjustment;
and 4, mixing the first extract, the second extract and the third extract, stirring at constant temperature for 4 hours to obtain a concentrated solution, then distilling the concentrated solution under reduced pressure, and freeze-drying to obtain the carrageenan extract, wherein the constant temperature stirring temperature is 85 ℃, the stirring speed is 1500r/min, the pressure of the reduced pressure distillation is 85% of the atmospheric pressure, and the temperature is 93 ℃.
Comparative example
Soaking herba Chenopodii with distilled water with pH of 8 adjusted by sodium hydroxide as extractive solution for 6 hr, filtering, and spray drying the filtrate to obtain herba Chenopodii Aromatici extract
| Example 1 | Example 2 | Example 3 | Comparative example | |
| Variation of extraction quantity | 9% | 12% | 11% | - |
| Appearance of | Pale yellow powder | Pale yellow powder | Pale yellow powder | White-like powder |
| Ash content | 9.4% | 9.3% | 9.3% | 9.8% |
| Smell of | No peculiar smell | No peculiar smell | No peculiar smell | Slightly fishy smell of seaweed |
In summary, the invention has the following advantages: 1. the invention solves the problem of residue of the existing corrugated carrageenan filter residue, and improves the extraction quantity by combining the alcohol extraction and the water extraction, thereby achieving the full extraction of active substances.
2. The invention utilizes the change of cell activity and the respiratory effect of the cell thawing process to realize gradient extraction, and fully extracts active substances inside and outside the cell wall, thereby improving the extraction efficiency.
It is to be understood that the foregoing detailed description of the invention is merely illustrative of the invention and is not limited to the embodiments of the invention. It will be understood by those of ordinary skill in the art that the present invention may be modified or substituted for elements thereof to achieve the same technical effects; as long as the use requirement is met, the invention is within the protection scope of the invention.
Claims (1)
1. An extraction process of a carrageenan with a ripple, which is characterized in that: the method comprises the following steps:
step 1, cleaning and chopping the carrageen, then adding the carrageen into an ethanol water solution, stirring at constant temperature, and filtering to obtain a first extract and first filter residues;
step 2, crushing the first filter residue into fine powder after freezing treatment, putting the fine powder into ethanol for ultrasonic treatment for 0.5-1h, then adding distilled water containing alkaline substances for secondary ultrasonic treatment for 2-4h, and filtering to obtain a second extract and second filter residue;
step 3, adding the second filter residue into distilled water, steaming at constant temperature for 2-3 hours, naturally cooling and press-filtering to obtain a third extract and a third filter residue;
step 4, mixing the first extract, the second extract and the third extract, stirring at constant temperature for 2-5 hours to obtain a concentrated solution, and then distilling the concentrated solution under reduced pressure, and freeze-drying to obtain the carrageenan extract;
in the step 1, the volume concentration of ethanol in the ethanol water solution is 50-70%, and the constant-temperature stirring temperature is 50-60 ℃;
in the step 2, the temperature of freezing treatment is-10 to-15 ℃; the addition amount of ethanol is 60-90% of the mass of the first filter residue, the ultrasonic frequency is 40-60kHz, and the temperature is 0-5 ℃; the alkaline substance in the distilled water is sodium hydroxide, the pH value is 8, the adding amount of the distilled water is 200-300% of the volume of ethanol, the temperature of the secondary ultrasonic treatment is 50-60 ℃, and the ultrasonic frequency is 50-80kHz;
in the step 3, the mass ratio of the second filter residue to distilled water is 1:5-10, and the constant-temperature cooking temperature is 80-90 ℃; adjusting the pH value to 8 before constant-temperature cooking, wherein sodium hydroxide is adopted for pH adjustment;
in the step 4, the constant temperature stirring temperature is 80-90 ℃, the stirring speed is 1000-2000r/min, the pressure of reduced pressure distillation is 80-90% of atmospheric pressure, and the temperature is 90-95 ℃.
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| CN112439025A (en) * | 2020-12-16 | 2021-03-05 | 江西和明制药有限公司 | Preparation method of Maiwei rehmannia oral liquid |
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| CN102757509B (en) * | 2011-04-29 | 2014-12-03 | 北京联合大学生物化学工程学院 | Extraction and purification method for Lentian |
| CN102703219B (en) * | 2012-04-19 | 2013-07-03 | 华南理工大学 | Extraction method of pomelo peel essential oil by peel icing and breaking |
| CN114262297A (en) * | 2021-12-29 | 2022-04-01 | 南京先达医药科技有限公司 | Preparation method of ergothioneine |
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| CN112439025A (en) * | 2020-12-16 | 2021-03-05 | 江西和明制药有限公司 | Preparation method of Maiwei rehmannia oral liquid |
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| Title |
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| Chondrus crispus treated with ultrasound as a polysaccharides source with improved antitumoral potential;Torres M D et al;Carbohydrate polymers;第273卷;1-10 * |
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