CN107904016B - Red algae essential oil and preparation method thereof - Google Patents
Red algae essential oil and preparation method thereof Download PDFInfo
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- CN107904016B CN107904016B CN201711105342.XA CN201711105342A CN107904016B CN 107904016 B CN107904016 B CN 107904016B CN 201711105342 A CN201711105342 A CN 201711105342A CN 107904016 B CN107904016 B CN 107904016B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
- C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
- C12P7/06—Ethanol, i.e. non-beverage
- C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
- C12P7/10—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate substrate containing cellulosic material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The invention discloses red algae essential oil and a preparation method thereof, wherein algae of rhodophyta porphyra, multicladium, gracilaria and gelidium during spore maturation are adopted, and after multiple times of enzymolysis, filtrate and residual solid matters are subjected to steam distillation respectively to obtain the red algae essential oil. The invention simplifies the extraction process of the red algae essential oil by the targeted degradation of pectin and cellulose in the red algae. The red algae essential oil provided by the invention has high yield, and the obtained red algae essential oil has aromatic smell and no fishy smell.
Description
Technical Field
The invention relates to a preparation method of essential oil, in particular to red algae essential oil and a preparation method thereof.
Background
Plants of Rhodophyta are 558 genus and 3700 species. About 200 of them are produced in fresh water, and the rest are marine products, which are the main parts of marine algae (the kingdom of protists).
The red algae are mainly filamentous, frond or dendritic, and have few single cells and some groups. Algae often have some tissue differentiation, e.g., some species have "cortex" and marrow. The cell wall is divided into two layers, the inner layer is composed of cellulose, the outer layer is composed of pectic substance containing specific pectin compounds of red algae such as agar and gloiopeltis. The pigment in fructus Jujubae is distributed in asterism shape, belt shape, twisted belt shape or biconvex shape, and contains chlorophyll a and chlorophyll b, carotene and xanthophyll, as well as phycoerythrin and phycocyanin. Phycoerythrin is generally dominant, so that the phycobiont is red or purple red.
The fishy smell of marine products is mainly formed by trimethylamine, delta-aminopentanal (acid) and piperidine compounds. Wherein, the delta-aminopentanal (acid) is generated by the action of basic amino acid lysine through three enzyme systems of deaminase, decarboxylase and oxidase: producing delta-aminopentanoate according to the sequence of deaminase-decarboxylase-oxidase; generating delta-aminopentanal according to the sequence of deaminase-decarboxylase; proceeding in the order of decarboxylase-deaminase, the transition is via the intermediate cadaverine to piperidine. Trimethylamine is formed by oxidizing trimethylamine in large amount under the action of microbe and enzyme.
Disclosure of Invention
Therefore, the invention aims to provide the red algae essential oil and the preparation method thereof.
The technical scheme of the invention is realized as follows:
a red algae essential oil, which has aromatic smell and does not contain fishy smell generated by trimethylamine, delta-aminopentanoic acid and the like.
A preparation method of red algae essential oil comprises the following steps:
step 1: taking fresh and mature red algae, performing irradiation sterilization and enzyme inactivation, cleaning, then crushing the red algae into small blocks of 3-7cm, adding water with the weight 2-4 times that of the red algae, adjusting the pH value to 4.5-6.5 by using hydrochloric acid, and adding an esterification reaction catalyst;
step 2: adding cellulase and yeast into the red algae mixture obtained in the step 1, controlling the temperature at 25-30 ℃, and performing enzymolysis for 5-10 h;
and step 3: in the step 2, adding hydrochloric acid again, adjusting pH to 2-5, adding pectinase, controlling temperature at 30-60 deg.C, and performing enzymolysis for 3-6 h;
and 4, step 4: filtering, respectively collecting filtrate and solid, distilling the filtrate under reduced pressure, collecting fractions with different boiling points, and separating out water and ethanol;
and 5: washing the solid matters in the red algae mixture in the step 4 with clear water, drying, breaking the walls, crushing, distilling under reduced pressure by using a steam distillation method, and collecting fractions;
step 6: and (5) mixing the fractions obtained in the steps (4) and (5) to obtain the red algae essential oil.
Further, in the step 1, the red algae may be algae of porphyra, multicladium, gracilaria and gelidium; the picking time is before and after the red algae spores are mature.
Further, in the step 1, the esterification catalyst is an immobilized heteropoly acid catalyst.
Further, in the step 2, the dosage of the cellulase and the yeast is 0.1-0.2% and 0.05-0.1% of the weight of the red algae respectively.
Further, in the step 3, the dosage of the pectinase is 0.05-0.2% of the weight of the red algae.
The invention can kill deaminase, decarboxylase and oxidase in red algae in time by irradiating red algae, and avoid the continuous generation of trimethylamine, delta-aminopentanal (acid) and piperidine compounds. Adjusting pH to acidity, and neutralizing generated amine substances such as trimethylamine; adding esterification catalyst to convert the residual delta-amino pentanoic acid into esters, and performing enzymolysis for several times to degrade cellulose and pectin in red algae in a targeted manner, thereby reducing extraction difficulty of essential oil and simultaneously obtaining byproduct ethanol.
Compared with the prior art, the invention has the beneficial effects that:
1) the red algae essential oil prepared by the invention has aromatic smell and does not have fishy smell;
2) the oil yield of the preparation method of the red algae essential oil provided by the invention is high and can reach 0.113%;
3) according to the preparation method provided by the invention, a byproduct ethanol can be obtained.
Detailed Description
For clear and complete description of the technical solutions in the present invention, it is obvious that the inventor combines the embodiments to describe, but the following embodiments describe only some embodiments of the present invention, 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.
A red algae essential oil free of fishy smell generated by trimethylamine, delta-aminopentanoic acid and the like is prepared by the following steps:
step 1: taking fresh and mature red algae, performing irradiation sterilization and enzyme inactivation, cleaning, then crushing the red algae into small blocks of 3-7cm, adding water with the weight 2-4 times that of the red algae, adjusting the pH value to 4.5-6.5 by using hydrochloric acid, and adding an esterification reaction catalyst;
step 2: adding cellulase and yeast into the red algae mixture obtained in the step 1, controlling the temperature at 25-30 ℃, and performing enzymolysis for 5-10 h;
and step 3: in the step 2, adding hydrochloric acid again, adjusting pH to 2-5, adding pectinase, controlling temperature at 30-60 deg.C, and performing enzymolysis for 3-6 h;
and 4, step 4: filtering, respectively collecting filtrate and solid, distilling the filtrate under reduced pressure, collecting fractions with different boiling points, and separating out water and ethanol;
and 5: washing the solid matters in the red algae mixture in the step 4 with clear water, drying, breaking the walls, crushing, distilling under reduced pressure by using a steam distillation method, and collecting fractions;
step 6: and (5) mixing the fractions obtained in the steps (4) and (5) to obtain the red algae essential oil.
Further, in the step 1, the red algae may be algae of porphyra, multicladium, gracilaria and gelidium; the picking time is before and after the red algae spores are mature.
Further, in the step 1, the esterification catalyst is an immobilized heteropoly acid catalyst.
Further, in the step 2, the dosage of the cellulase and the yeast is 0.1-0.2% and 0.05-0.1% of the weight of the red algae respectively.
Further, in the step 3, the dosage of the pectinase is 0.05-0.2% of the weight of the red algae.
Examples and comparative examples were designed as shown in table 1:
table 1, examples 1-4, comparative examples 1-5 preparation method parameters:
the oil production and fishy smell of examples 1-4 and comparative examples 1-5 were measured as shown in Table 2:
table 2:
it can be seen that according to the preparation method provided by the invention, the red algae essential oil which has no fishy smell and has high oil yield can be obtained, the oil yield is obviously reduced beyond the range of the preparation parameters provided by the invention, wherein the oil yield is maximum when the pH value is too low. In addition, the obtained essential oil has fishy smell without adding enzyme or using esterification reaction catalyst, which affects the quality of the essential oil.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (3)
1. The red algae essential oil is characterized by being aromatic in smell, free of trimethylamine and delta-aminopentanoic acid which can generate fishy smell, and the preparation method comprises the following steps:
step 1: taking fresh and mature red algae, performing irradiation sterilization and enzyme inactivation, cleaning, then crushing the red algae into small blocks of 3-7cm, adding water with the weight 2-4 times that of the red algae, adjusting the pH value to 4.5-6.5 by using hydrochloric acid, and adding an esterification reaction catalyst;
step 2: adding cellulase and yeast into the red algae mixture obtained in the step 1, wherein the dosage of the cellulase and the yeast is 0.1-0.2 percent and 0.05-0.1 percent of the weight of the red algae respectively, controlling the temperature at 25-30 ℃, and performing enzymolysis for 5-10 hours;
and step 3: in the step 2, adding hydrochloric acid again, adjusting pH to 2-5, adding pectase, wherein the dosage of pectase is 0.05-0.2% of the weight of red algae, controlling the temperature at 30-60 deg.C, and performing enzymolysis for 3-6 h;
and 4, step 4: filtering, respectively collecting filtrate and solid, distilling the filtrate under reduced pressure, collecting fractions with different boiling points, and separating out water and ethanol;
and 5: washing the solid matters in the red algae mixture in the step 4 with clear water, drying, breaking the walls, crushing, distilling under reduced pressure by using a steam distillation method, and collecting fractions;
step 6: and (5) mixing the fractions obtained in the steps (4) and (5) to obtain the red algae essential oil.
2. The red algae essential oil according to claim 1, wherein in the step 1, the red algae are algae of porphyra, multiclada, gracilaria and gelidium; the picking time is before and after the red algae spores are mature.
3. The essential oil of red algae according to claim 1, wherein in step 1, the esterification catalyst is an immobilized heteropoly acid catalyst.
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| CN201711105342.XA CN107904016B (en) | 2017-11-10 | 2017-11-10 | Red algae essential oil and preparation method thereof |
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| CN107904016B true CN107904016B (en) | 2021-04-20 |
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| CN113245343B (en) * | 2021-04-26 | 2022-08-12 | 菏泽尧舜牡丹生物科技有限公司 | Efficient utilization method of squeezed peony residues |
| CN113444578B (en) * | 2021-06-24 | 2023-03-21 | 日照职业技术学院 | Extraction process of nannochloropsis oculata essential oil |
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