CN113735802B - A method for preparing fucoxanthin extract with eutectic solvent - Google Patents
A method for preparing fucoxanthin extract with eutectic solvent Download PDFInfo
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- CN113735802B CN113735802B CN202111184712.XA CN202111184712A CN113735802B CN 113735802 B CN113735802 B CN 113735802B CN 202111184712 A CN202111184712 A CN 202111184712A CN 113735802 B CN113735802 B CN 113735802B
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Abstract
The invention relates to the technical field of eutectic solvent application, in particular to a method for preparing seaweed fucoxanthin extract by using the eutectic solvent. The method for extracting fucoxanthin from seaweed by using the eutectic solvent specifically comprises the following steps: pulverizing Sargassum, adding eutectic solvent (such as menthol-propionic acid eutectic solvent of different types and proportions), ultrasonic extracting at 25-30 deg.C for 3-30min, centrifuging, and collecting supernatant to obtain fucoxanthin extract. The invention provides an efficient and green method for preparing fucoxanthin extract by utilizing a eutectic solvent, which has the characteristics of short required time, low energy consumption and environmental protection. The fucoxanthin extract is prepared by introducing the natural eutectic solvent, and a new research and development idea is provided for extracting the active ingredients of the seaweed.
Description
Technical Field
The invention relates to a preparation method of a seaweed fucoxanthin extract, in particular to a preparation method of a seaweed fucoxanthin extract by using a eutectic solvent, belonging to the technical field of food processing technology and functional health food.
Background
Fucoxanthin (also called fucoxanthin) is a natural carotenoid extracted from edible brown algae such as Undaria pinnatifida (Alariaceae) and Laminaria japonica (Laminaria japonica Aresch), and has strong biological activity including anti-tumor, anti-inflammatory, anti-oxidant, and weight-reducing effects, since two chemically active 5, 6-epoxy unsaturated allene bond structures are respectively arranged at two ends of rigid all-trans long chain. In recent years, various biological activities of the compound have been proved, and some potential activities are actively researched by scientists, so that the compound is one of the main focus points of research and development of marine medicines at present. At present, the extraction method of fucoxanthin mainly adopts an organic solvent extraction method, which comprises adopting methanol, ethanol, ethyl acetate, chloroform and the like, but most of the methods have low extraction efficiency, and the organic solvent has the defects of certain toxicity, flammability, explosiveness and the like.
The eutectic solvent is generally composed of a hydrogen bond acceptor and a hydrogen bond donor in a stoichiometric ratio, which can be combined with each other through hydrogen bonds to form a eutectic mixture, and has a melting point lower than that of each component. Generally, most eutectic solvents are liquid at room temperature to 70 ℃. Since the physical and chemical properties of the eutectic solvent are very similar to those of ionic liquids, it has also been classified as an ionic liquid or an ionic liquid analogue. Most of the reagents adopted by the eutectic solvent are natural raw materials, have the characteristics of no toxicity, biodegradability, environmental protection and the like, have the advantages which cannot be compared with a plurality of traditional solvents, and are gradually applied to extraction and separation of natural products.
The research mainly invents a green environment-friendly eutectic solvent, is applied to the extraction of fucoxanthin in seaweed, and has the characteristics of simple operation, green environmental protection and high efficiency.
Disclosure of Invention
The invention aims to provide a preparation method for preparing fucoxanthin extract by using a eutectic solvent, which has the characteristics of simple operation, environmental protection, high efficiency and the like.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing seaweed fucoxanthin by using a eutectic solvent comprises the following steps: (1) washing off silt impurities and the like from the seaweed, drying and crushing; (2) adding the seaweed powder into the eutectic solvent for ultrasonic extraction; (3) centrifuging, and collecting supernatant to obtain fucoxanthin extract.
The method for preparing the seaweed fucoxanthin by adopting the eutectic solvent is characterized in that the eutectic solvent is formed by mixing a hydrogen bond donor and a hydrogen bond acceptor and/or ethanol, and the hydrogen bond donor comprises: lactic acid, acetic acid, citric acid, malic acid, propionic acid, the hydrogen bond acceptor includes: menthol, camphor, borneol, geraniol, nerol and citronellol.
The method for preparing the seaweed fucoxanthin by using the eutectic solvent comprises the following steps of (1): 0.5-5, mixing and heating.
The method for preparing the seaweed fucoxanthin by using the eutectic solvent comprises the following steps: mixing the hydrogen bond donor and the hydrogen bond acceptor, and heating and stirring at 60-100 ℃ for 0.5-2h to form a clear and uniform eutectic solvent.
The method for preparing seaweed fucoxanthin by using the deep eutectic solvent is characterized in that the weight ratio of the seaweed powder to the deep eutectic solvent is 1: 5-30.
The method for preparing the seaweed fucoxanthin by using the eutectic solvent comprises the following ultrasonic extraction conditions: extracting with ultrasound at 25-30 deg.C under 50-200W for 3-30 min.
The method for preparing seaweed fucoxanthin by using the eutectic solvent comprises the step of preparing seaweed from one of Sargassum horneri, kelp and sargassum fusiforme.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the seaweed fucoxanthin is extracted by the eutectic solvent, compared with the traditional organic solvent extraction, the extraction rate of the fucoxanthin is greatly improved, and the eutectic solvent is green and environment-friendly, has strong stability, and can replace the traditional organic solvent to be used as a novel extracting agent of the fucoxanthin;
(2) the extraction method has the advantages of simple operation, less solvent consumption, short extraction time and low production cost, and is suitable for large-scale industrial production.
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FIG. 1 is a high performance liquid chromatography detection of fucoxanthin content of seaweed of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 1
Taking Sargassum horneri, washing off silt impurities, drying, pulverizing, adding 1g eutectic solvent 5mL (menthol-lactic acid molar ratio is 1: 0.3), vortex mixing, ultrasonic extracting for 5min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.58 mg/g.
Example 2
Taking Sargassum horneri, washing off silt impurities, drying, pulverizing, adding 10mL of eutectic solvent (menthol-acetic acid molar ratio is 1: 1) into 1g, vortex mixing, ultrasonic extracting for 5min, centrifuging, collecting supernatant, and detecting fucoxanthin content to be 1.67mg/g by high performance liquid chromatography.
Example 3
Taking Sargassum horneri, washing off silt impurities, etc., drying, pulverizing, adding 1g eutectic solvent 15mL (menthol-citric acid molar ratio is 1: 2), vortex mixing, ultrasonic extracting for 10min, centrifuging, taking supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.79 mg/g.
Example 4
Taking Sargassum horneri, washing off silt impurities, drying, pulverizing, adding 1g of eutectic solvent 20mL (menthol-malic acid molar ratio is 1: 3), vortex mixing, ultrasonic extracting for 15min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.75 mg/g.
Example 5
Taking Sargassum horneri, washing off silt impurities, etc., drying, pulverizing, adding 1g eutectic solvent 30mL (menthol-propionic acid molar ratio is 1: 5), vortex mixing, ultrasonic extracting for 30min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.85 mg/g.
Example 6
Taking the kelp, washing off silt impurities and the like, drying, crushing, adding 5mL of eutectic solvent (the molar ratio of camphor to lactic acid is 1: 0.3) into 1g of kelp, vortex mixing uniformly, carrying out ultrasonic extraction for 5min, centrifuging, taking supernatant, and detecting the fucoxanthin content to be 1.18mg/g by high performance liquid chromatography.
Example 7
Washing herba Zosterae Marinae, removing silt and impurities, drying, pulverizing, adding 1g eutectic solvent 10mL (Camphora-acetic acid molar ratio is 1: 1), vortex mixing, ultrasonic extracting for 5min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.21 mg/g.
Example 8
Taking kelp, washing off silt impurities and the like, drying, crushing, adding 1g of eutectic solvent 15mL (the molar ratio of camphor to citric acid is 1: 2), vortex mixing uniformly, carrying out ultrasonic extraction for 10min, centrifuging, taking supernatant, and detecting the fucoxanthin content to be 1.23mg/g by high performance liquid chromatography.
Example 9
Washing herba Zosterae Marinae, removing silt and impurities, drying, pulverizing, adding eutectic solvent 20mL (Camphora-malic acid molar ratio is 1: 3) into 1g, vortex mixing, ultrasonic extracting for 15min, centrifuging, collecting supernatant, and detecting fucoxanthin content to be 1.27mg/g by high performance liquid chromatography.
Example 10
Taking kelp, washing off silt impurities and the like, drying, crushing, adding 1g of eutectic solvent 30mL (the molar ratio of camphor to propionic acid is 1: 5), vortex mixing uniformly, carrying out ultrasonic extraction for 30min, centrifuging, taking supernatant, and detecting the fucoxanthin content to be 1.36mg/g by high performance liquid chromatography.
Example 11
Washing Cyrtymenia Sparsa, removing silt and impurities, drying, pulverizing, adding eutectic solvent 5mL (borneol-lactic acid molar ratio of 1: 0.3) into 1g, vortex mixing, ultrasonic extracting for 5min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.51 mg/g.
Example 12
Washing Cyrtymenia Sparsa, removing silt and impurities, drying, pulverizing, adding 1g eutectic solvent 10mL (borneol-acetic acid molar ratio of 1: 1), vortex mixing, ultrasonic extracting for 5min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.62 mg/g.
Example 13
Washing Cyrtymenia Sparsa, removing silt and impurities, drying, pulverizing, adding 1g eutectic solvent 15mL (borneol-citric acid molar ratio is 1: 2), vortex mixing, ultrasonic extracting for 10min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.65 mg/g.
Example 14
Washing Cyrtymenia Sparsa, removing silt and impurities, drying, pulverizing, adding eutectic solvent 20mL (Borneolum-malic acid molar ratio of 1: 3) into 1g, vortex mixing, ultrasonic extracting for 15min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.71 mg/g.
Example 15
Washing Cyrtymenia Sparsa, removing silt and impurities, drying, pulverizing, adding 1g eutectic solvent 30mL (borneol-propionic acid molar ratio is 1: 5), vortex mixing, ultrasonic extracting for 30min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.70 mg/g.
Example 16
Taking Sargassum horneri, washing off silt impurities, drying, pulverizing, taking 1g, adding 20mL of eutectic solvent (geraniol-lactic acid molar ratio is 1: 3), vortex mixing, ultrasonic extracting for 10min, centrifuging, taking supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.65 mg/g.
Example 17
Taking Sargassum horneri, washing off silt impurities, etc., drying, pulverizing, adding 1g eutectic solvent 20mL (nerol-acetic acid molar ratio is 1: 3), vortex mixing, ultrasonic extracting for 10min, centrifuging, taking supernatant, and detecting fucoxanthin content to be 1.69mg/g by high performance liquid chromatography.
Example 18
Taking Sargassum horneri, washing off silt impurities, drying, pulverizing, adding 20mL of eutectic solvent (nerol-malic acid molar ratio is 1: 3) into 1g, vortex mixing, ultrasonic extracting for 10min, centrifuging, taking supernatant, and detecting fucoxanthin content to be 1.51mg/g by high performance liquid chromatography.
Example 19
Taking Sargassum horneri, washing off silt impurities, etc., drying, pulverizing, adding 1g eutectic solvent 20mL (mole ratio of citronellol-lactic acid is 1: 3), vortex mixing, ultrasonic extracting for 10min, centrifuging, collecting supernatant, and detecting fucoxanthin content by high performance liquid chromatography to be 1.78 mg/g.
Example 20
Taking Sargassum horneri, washing off silt impurities, drying, pulverizing, adding eutectic solvent 20mL (citronellol-propionic acid molar ratio is 1: 3) into 1g, vortex mixing, ultrasonic extracting for 10min, centrifuging, taking supernatant, and detecting fucoxanthin content to be 1.83mg/g by high performance liquid chromatography.
Comparative example 1
Taking Sargassum horneri, washing off silt impurities, etc., drying, pulverizing, taking 1g, adding 20mL (v/v) of 90% ethanol water solution, mixing uniformly by vortex, ultrasonically extracting for 10min, centrifuging, taking supernatant, and detecting fucoxanthin content to be 1.13mg/g by high performance liquid chromatography.
Comparative example 2
Taking kelp, washing off silt impurities and the like, drying, crushing, adding 20mL (v/v) of 90% ethanol aqueous solution into 1g, uniformly mixing by vortex, ultrasonically extracting for 10min, centrifuging, taking supernatant, and detecting the fucoxanthin content to be 0.95mg/g by high performance liquid chromatography.
Comparative example 3
Washing Sargassum fusiforme, removing silt impurities, drying, pulverizing, adding 90% ethanol water solution 20mL (v/v) 1g, mixing, performing ultrasonic extraction for 10min, centrifuging, collecting supernatant, and detecting fucoxanthin content to be 1.17mg/g by high performance liquid chromatography.
The fucoxanthin content of the examples 1 to 20 and the comparative examples 1 to 3 is shown in fig. 1, and it can be seen that the extraction rate of fucoxanthin is greatly improved by using the eutectic solvent compared with the conventional organic solvent extraction, and the eutectic solvent is green, environment-friendly and strong in stability, and can replace the conventional organic solvent to be used as a novel fucoxanthin extracting agent.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for preparing seaweed fucoxanthin by using a eutectic solvent is characterized by comprising the following steps: (1) washing off silt and impurities from the seaweed, drying and crushing; (2) adding the seaweed powder into the eutectic solvent for ultrasonic extraction; (3) centrifuging, and collecting supernatant to obtain fucoxanthin extract; the eutectic solvent is formed by mixing a hydrogen bond donor and a hydrogen bond acceptor and/or ethanol, wherein the hydrogen bond donor comprises: lactic acid, acetic acid, citric acid, malic acid, propionic acid, the hydrogen bond acceptor includes: menthol, borneol, geraniol, nerol, citronellol; the eutectic solvent is prepared by mixing a hydrogen bond donor and a hydrogen bond acceptor in a ratio of the amount of substances of 1: 0.55, mixing and heating.
2. The method for preparing algal fucoxanthin of claim 1 using a eutectic solvent, wherein the eutectic solvent is prepared by the following method: and (3) mixing the hydrogen bond donor and the hydrogen bond acceptor, and heating and stirring at 60100 ℃ for 0.52 h to form a clear and uniform eutectic solvent.
3. The method for preparing algal fucoxanthin of claim 1, wherein the ratio of the algal powder weight to the eutectic solvent is 1: 530.
4. The method for preparing algal fucoxanthin of claim 1 using the eutectic solvent, wherein the ultrasonic extraction conditions are as follows: extracting with ultrasound at 2530 deg.C and 50200W for 330 min.
5. The method for preparing algal fucoxanthin of claim 1 using the eutectic solvent, wherein the algal is one of Sargassum horneri, Laminaria japonica and Hizikia fusiforme.
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