CN108530397B - Preparation of sargassum horneri algae powder and method for extracting fucoxanthin in sargassum horneri algae powder - Google Patents
Preparation of sargassum horneri algae powder and method for extracting fucoxanthin in sargassum horneri algae powder Download PDFInfo
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Abstract
The invention belongs to the technical field of marine organism natural products, and particularly relates to a preparation method of sargassum horneri algae powder and an extraction method of fucoxanthin in the algae powder; the invention takes the sargassum horneri as raw material, and the sargassum horneri powder is prepared by the steps of cleaning, drying in the shade, drying, pulverizing, sterilizing and the like; adding extractive solution and steel balls into Sargassum horneri powder, extracting under shaking for 3-10min under low light, low temperature and oxygen-free conditions, centrifuging to obtain clear liquid, separating with high performance liquid chromatography, and freeze vacuum drying to obtain fucoxanthin pure product; the method has the advantages of high efficiency, simplicity, low cost and the like, provides a basis for the comprehensive utilization of biological resources of the Sargassum horneri, and has potential important economic value.
Description
Technical Field
The invention belongs to the technical field of marine organism natural products, and particularly relates to a preparation method of sargassum horneri algae powder and an extraction method of fucoxanthin in the algae powder.
Background
The Sargassum horneri (Sargassum horneri) is a large brown algae which grows in a floating way, is widely distributed in the northern sea area of China, has the characteristics of wide adaptability, strong stress resistance, easy cultivation and the like, is not only an important component of an offshore ecosystem, but also an important economic brown algae.
Fucoxanthin (also called fucoxanthin) is a carotenoid substance composed of three elements of carbon, hydrogen and oxygen, and is widely distributed in some diatoms and large-sized brown algae. Because the chemical structure of the nano-composite material has more conjugated double bonds, the nano-composite material has oxidation resistance and can effectively eliminate free radicals in organisms. The fucoxanthin can promote energy consumption of fat cells by inducing the expression of uncoupling protein 1 in cell mitochondria, and has the effect of losing weight. Research shows that fucoxanthin can improve insulin sensitivity and realize the function of resisting type II diabetes. Fucoxanthin can also influence cell cycle regulation and apoptosis through the antioxidant activity of the fucoxanthin, and has potential anticancer effect. Therefore, the biological product rich in the fucoxanthin has wider application in medicines, foods, health care products and formula foods with special medical application.
The industrial development of fucoxanthin as the main active substance is still in the beginning at home. At present, there are microalgae and macroalgae as raw materials for producing fucoxanthin-rich biologicals. Wherein, the characteristics of high requirements of microalgae culture process, high energy consumption for cell harvesting and the like become the bottleneck of the industrialized development. In contrast, the macroalgae is easy to culture and harvest, can purify water quality to a certain extent and restore marine ecological environment, and is an excellent raw material for processing fucoxanthin-rich biological products. The content of fucoxanthin in Sargassum horneri can reach 0.07%, and the Sargassum horneri is easy to be cultivated in northern China. The Sargassum horneri plant is 0.5-2 m high, and has branch structure, stem, leaf, air sac structure, etc. According to the observation of the anatomical structure of Sargassum horneri, the parts where pigments mainly accumulate are located in the epidermal cells of the leaves, the epidermal cells of the air sacs and the stem parts.
At present, most of the research on fucoxanthin at home and abroad is from kelp and undaria pinnatifida, and the extraction of fucoxanthin by using sargassum horneri as a material is reported. Patent CN105859657A discloses a method for extracting fucoxanthin crude products from Sargassum horneri, which extracts fucoxanthin crude products from Sargassum horneri through steps of pretreatment, suction filtration, ultrasonic extraction, extraction and the like, wherein the pretreatment relates to freeze drying of algae bodies, although the activity of fucoxanthin is maintained to a certain degree, the energy consumption of the process is high, and in addition, the method for extracting fucoxanthin crude products is not separated and has low purity.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of sargassum horneri algae powder and an extraction method of fucoxanthin in the algae powder.
In order to achieve the purpose, the invention comprises the following technical scheme:
a preparation method of sargassum horneri powder comprises the following steps:
(1) cleaning: collecting fresh Sargassum horneri, and cleaning Sargassum horneri body with seawater and fresh water;
(2) drying in the shade: spreading the washed sargassum horneri, airing in a low-light environment, and manually picking out other sargassum horneri;
(3) drying: transferring the sargassum horneri to a dryer, drying at 55-60 ℃, and continuously introducing nitrogen into the oven in the drying process;
(4) milling: freezing and grinding the dried sargassum horneri, and sieving the sargassum horneri with a 65-90-mesh sieve to obtain sargassum horneri powder;
(5) and (3) sterilization: sterilizing the algae powder by ray irradiation, and storing at normal temperature in a dark place;
wherein, the steps (1), (2), (3) and (4) are operated under the environment that the light intensity does not exceed 200 Lux; the sterilization temperature in the step (5) is not more than 25 ℃, and the ambient light intensity is not more than 10 Lux.
Further, step (1) repeatedly washing fresh Sargassum horneri with clean seawater to quickly remove silt, small plankton, hooked shrimp and other organisms attached to the algae; then clean fresh water is used for rapidly washing the algae in batches, and residual seawater and salt stains are washed.
The salinity of the seawater used for flushing is 30-35 per mill, the flushing water pressure of the seawater and the fresh water is not more than 0.07MPa, and the time for contacting algae with the fresh water is not more than 2 minutes.
Seawater is used for isotonic flushing, so that water loss stress of algae and pigment loss or damage can not be caused; the algae can be quickly washed by fresh water, the residual seawater or salt stains on the algae can be removed, the washing time is not more than 2 minutes, the seawater water loss stress can be reduced to the maximum extent, and the pigment extraction rate is improved. The water pressure of the sea water and the fresh water for cleaning the seaweed is not more than 0.07MPa, and the damage of the water pressure to the parts rich in fucoxanthin, such as frond, air sac and the like, can be prevented.
Further, the process conditions in the step (2) are as follows: the air humidity of the environment is not more than 50%, and the drying time is not more than 12 hours.
Further, the nitrogen gas is introduced at a rate of 0.1-0.2V/min (V is the volume of the oven) in the drying process in the step (3).
Further, the drying time in the step (3) is not more than 24 hours, and the drying process is turned over once every 1-2 hours.
The invention also provides a method for extracting fucoxanthin by using the prepared Sargassum horneri powder, which comprises the following steps:
(1) adding an extracting solution and steel balls into the algae powder, performing oscillation extraction and centrifugation under the environment of weak light, low temperature and no oxygen to obtain a supernatant, wherein the extracting solution is a mixed solvent of methanol and acetone, and the volume ratio of the extracting solution to the acetone is 1: 1;
low-temperature steel ball-added oscillation extraction is adopted, and the high-frequency oscillation of the steel balls is utilized to instantly break the cell walls of the Sargassum horneri, so that the dissolution of fucoxanthin is accelerated, and the extraction rate of the fucoxanthin is improved; fucoxanthin has heat sensitivity, is poor in stability at high temperature and easy to generate geometric isomerism, and is extracted at low temperature, so that fucoxanthin is effectively prevented from being degraded.
(2) Storing the clear liquid obtained by extraction centrifugation in a low-light, low-temperature and anaerobic environment, adding the extracting solution into the centrifuged precipitate, repeatedly extracting, and combining the two supernatants;
(3) separating the supernatant obtained in the step (2) by using high performance liquid chromatography, and collecting an effluent phase;
(4) performing vacuum freeze drying on the fucoxanthin effluent collected in the step (3) to obtain a pure fucoxanthin product;
the column packing of the high performance liquid chromatography in the step (3) is a C18 reverse chromatographic column, the fluidity is a mixture of water, methanol, acetonitrile and ethyl acetate, and the elution procedure is as follows: from 0 to 15 minutes, the mobile phase composition was composed of water (14%): methanol (28%): linear gradient of acetonitrile (58%) to water (0%): methanol (15%): acetonitrile (85%); 15-17 min, linear gradient to water (15%) methanol (15%): acetonitrile (15%): ethyl acetate (35%); 17-40 min, linear gradient to methanol (30%): ethyl acetate (70%), separating for 40 min, and collecting the component between 8-9 min, i.e. fucoxanthin.
Further, the ratio of the algae powder to the extract in the step (1) is as follows: 3ml of the extract was added to 1g of algal powder.
Further, the shaking extraction in the step (1) and the step (2) is operated on an ice-water bath, and the process conditions are as follows: the light intensity of the environment is not more than 10Lux, the extraction temperature is 0 ℃, the extraction time is 3-10min, the extraction container is closed, the extracting solution and the steel balls are added, then nitrogen is introduced, and the extraction is immediately carried out in a sealed way.
The nitrogen is introduced to have the following functions: moisture in the interior air is substantially removed and the oxygen-free environment is created.
Further, the optimized separation conditions in the step (3) are as follows: the mobile phase is a mixed solution of water, methanol and acetonitrile, and the mobile phase is water: methanol: the volume ratio of acetonitrile (14:28:58) was linearly eluted to water: methanol: acetonitrile volume ratio (4.67:19.33:76), separation time 10 minutes, and fractions between 7.70 and 8.70 minutes were collected.
The function of ethyl acetate in the mobile phase is to elute the components remaining on the column and to facilitate regeneration of the separation column, the separation time being optimized to 10 minutes.
Further, the temperature of the cold trap for freeze drying in the step (4) is set to be-80 ℃, and the freeze drying time is not more than 3 h.
Compared with the prior art, the invention has the following advantages:
1. the raw material of the invention is the large brown algae in the sea, the biomass is huge, the invention is easy to obtain, and compared with the microalgae material, the invention has low harvesting cost.
2. The energy consumption is low in the material treatment process, and the degradation rate of the fucoxanthin is low. The invention uses fresh Sargassum horneri as raw material, which avoids the degradation of fucoxanthin in the steps of collecting and processing raw material; in the material pretreatment stage, freeze drying and freeze storage treatment are not needed, and the energy consumption is low.
3. In industrial production, factors such as cost, process complexity and the like are considered, so that a drying method is still generally adopted for raw material treatment at present, and fucoxanthin is easily oxidized at high temperature in the drying process. According to the invention, nitrogen is introduced in the drying process to form a low-oxygen environment, so that the high-temperature and oxidative decomposition of fucoxanthin is reduced to the maximum extent.
4. The invention adopts low-temperature steel bead-added oscillation extraction, and has no temperature rise and additive in the process of fucoxanthin extraction, thereby maximally maintaining the activity of fucoxanthin.
5. The fucoxanthin has the characteristics of photosensitivity and heat sensitivity, the invention limits the environmental conditions in the fucoxanthin extraction process, especially the environmental light intensity, and provides a basis for utilizing the biological resources of the Sargassum horneri.
6. The steel balls are oscillated at high frequency at low temperature, so that the extraction time can be shortened to 5 minutes on the premise of not losing the extraction rate and the purity.
Drawings
FIG. 1: the invention discloses a schematic process diagram for preparing sargassum horneri powder and extracting fucoxanthin.
FIG. 2: the invention relates to a linear elution gradient chart used in the process of separating and extracting fucoxanthin.
FIG. 3: the invention separates the spectrogram of the extracted fucoxanthin.
FIG. 4: the high performance liquid chromatogram for fucoxanthin extraction in example 1.
FIG. 5: the high performance liquid chromatogram for fucoxanthin extraction in example 2.
FIG. 6: the high performance liquid chromatogram for fucoxanthin extraction in example 3.
Detailed Description
The present invention will be described in further detail below by way of examples, but the present invention is not limited to the following embodiments.
The invention is based on the early-stage basis of researches such as sargassum horneri field cultivation, activity monitoring, microscopic observation and the like, and develops a series of research contents such as sargassum horneri harvesting, raw material processing, powder making, extraction and the like. The present invention will be described in detail by way of examples, but the present invention is not limited to the following examples.
Example 1
Collecting fresh Sargassum horneri in a time period (early morning or evening) with weak ambient light by adopting a manual salvage mode, and covering the collected Sargassum horneri body by using a sun-shading cloth. After the collection, the sargassum horneri is transferred to a shady and cool factory building with the ambient light of about 180Lux, and fresh sargassum horneri is immediately washed and soaked by clean seawater, the temperature of the seawater is about 20 ℃, and the salinity is 30 per mill, so that the silt, small plankton, hooked shrimp and other organisms attached to the sargassum horneri are fully removed. The Sargassum horneri is quickly washed for 1 minute by using clean fresh water with the temperature of about 20 ℃. The cleaned sargassum horneri is spread on a shelf, the miscellaneous algae are removed manually, and the water is drained and dried in the shade for 12 hours.
The half-dried Sargassum horneri which is fully drained in the shade is transferred to an electric heating oven, dried for 20 hours at 55 ℃, turned over once every 1 hour, continuously dried for 12 hours, and introduced with nitrogen at 20L/min. And (4) freezing and grinding the dried sargassum horneri into powder by using liquid nitrogen, and sieving the powder by using a 65-mesh sieve. And (5) performing irradiation sterilization treatment on the algae powder. 1g of algae powder is weighed, 3mL of methanol is added: acetone ═ 1: 1, adding steel balls with the diameter of 3mm into the extracting solution, precooling the steel balls in advance, introducing nitrogen, sealing, and placing the extracting solution in a dark place to perform ice-water bath oscillation extraction for 3 minutes; after taking out the supernatant by centrifugation, 3mL of the above extract was added again to the precipitate, and the extraction was repeated once. The two supernatants were combined.
Filtering with 0.22 μm microporous membrane, separating with high performance liquid chromatography, separating with C18 reverse phase chromatographic column with water, methanol and acetonitrile as mobile phase, wherein the column temperature is 50 deg.C, and the flow rate of the mobile phase is 0.80 mL/min; the procedure for linear gradient elution is shown in fig. 2, and is specifically: from 0 to 15 minutes, the mobile phase composition was composed of water (14%): methanol (28%): linear gradient of acetonitrile (58%) to water (0%): methanol (15%): acetonitrile (85%); 15-17 min, linear gradient to water (15%) methanol (15%): acetonitrile (15%): ethyl acetate (35%); 17-40 min, linear gradient to methanol (30%): ethyl acetate (70%).
The chromatographic separation result is shown in FIG. 4, the outflow substance is fucoxanthin at 8.26 min as shown by an arrow, and the absorption spectrum of 400-800nm (shown as an enlarged region in FIG. 4) is extracted, and the absorption peak is 449 nm. The fucoxanthin standard substance is separated by the same chromatographic separation method, and the absorption spectrum (shown as an amplification area in figure 4) of 400-800nm is extracted, and the absorption peak is 449 nm. The run-out time of the standards was 8.26 minutes. Therefore, it was confirmed that the peak shown by the arrow in FIG. 3 was fucoxanthin, i.e., fucoxanthin flowed out from 7.74 minutes and ended at 8.70 minutes. Collecting the effluent in the time period, freezing and drying in vacuum to obtain pure fucoxanthin. The fucoxanthin extraction rate of the Sargassum horneri extracted by the method without chromatographic separation is calculated to be 2.63%, and the fucoxanthin purity obtained after HPLC chromatographic separation is 97.14%.
Example 2
Fresh sargassum horneri is collected from the cultivation sea area, and the collected sargassum horneri is covered by a sun-shading cloth. Transferring the Sargassum horneri to a shady and cool factory with the ambient light of about 180Lux, immediately washing with clean seawater, soaking fresh Sargassum horneri with the seawater temperature of about 20 deg.C and salinity of 30 ‰, and sufficiently removing silt, small plankton, and Hypoplophora crocea etc. attached on Sargassum horneri. The Sargassum horneri is quickly washed for 1 minute by using clean fresh water with the temperature of about 20 ℃. Spreading the cleaned Sargassum horneri on the shelf, manually removing Sargassum, draining, and drying in shade for 12 hr.
The half-dried Sargassum horneri after draining off water sufficiently is transferred to an electric oven, dried at 60 ℃ for 24 hours, turned over once every 1 hour, and introduced with nitrogen at 20L/min. And (4) freezing and grinding the dried sargassum horneri into powder by using liquid nitrogen, and sieving the powder by using a 90-mesh sieve. And (5) performing irradiation sterilization treatment on the algae powder. 2g of algae powder is weighed, and 6mL of methanol is added: acetone ═ 1: 1, adding steel balls with the diameter of 5mm into the extracting solution, precooling the steel balls in advance, introducing nitrogen, sealing, and placing in a dark place for shaking extraction in an ice-water bath for 5 minutes; after the supernatant was centrifuged, 6mL of the above extract was added again to the precipitate, extraction was repeated once, and the two supernatants were combined.
Filtering with 0.22 μm microporous membrane, and separating with high performance liquid chromatography. Separating with C18 reverse chromatographic column at 50 deg.C and flow rate of 0.80mL/min by using water, methanol and acetonitrile as mobile phase; the procedure for linear gradient elution was: initial mobile phase water: methanol: acetonitrile in a volume ratio (14:28:58) eluted linearly to water: methanol: the volume ratio of acetonitrile is (4.67:19.33:76), and the separation time is 10 min.
The chromatographic separation result is shown in FIG. 5, the outflow substance is fucoxanthin at 8.22 min as shown by an arrow, and the absorption spectrum of 400-800nm (shown as an enlarged region in FIG. 5) is extracted, and the absorption peak is 449 nm. Fucoxanthin flows out from 7.69 minutes and ends at 8.66 minutes, and the outflow in the time period is collected and dried by using freezing vacuum to obtain pure fucoxanthin. The fucoxanthin extraction rate of the Sargassum horneri extracted by the method without chromatographic separation is calculated to be 2.96%, and the fucoxanthin purity obtained after HPLC chromatographic separation is 97.09%.
Example 3
Fresh sargassum horneri is collected from the cultivation sea area, and the collected sargassum horneri is covered by a sun-shading cloth. Transferring the Sargassum horneri to a shady and cool factory with an ambient light of about 100Lux, immediately washing with clean seawater, soaking fresh Sargassum horneri at a temperature of about 20 deg.C and a salinity of 30 ‰, and sufficiently removing silt, small plankton, and Hypoplophora crocea attached to Sargassum horneri. The Sargassum horneri is quickly washed for 1 minute by using clean fresh water at the temperature of about 20 ℃. Spreading the cleaned Sargassum horneri on the shelf, manually removing Sargassum, draining, and drying in shade for 12 hr.
The half-dried Sargassum horneri which is fully drained in the shade is transferred to an electric heating oven, dried for 24 hours at the temperature of 60 ℃, turned over once every 1 hour, and introduced with nitrogen at the rate of 20L/min. And (4) freezing and grinding the dried sargassum horneri into powder by using liquid nitrogen, and sieving the powder by using a 90-mesh sieve. And (5) performing irradiation sterilization treatment on the algae powder. 2g of algae powder is weighed, and 6mL of methanol is added: acetone ═ 1: 1, adding steel balls with the diameter of 5mm into the extracting solution, precooling the steel balls in advance, introducing nitrogen, sealing, and placing in an ice-water bath in a dark place to shake and extract for 10 minutes; after the supernatant was centrifuged, 6mL of the above extract was added to the precipitate again, extraction was repeated once, and the two supernatants were combined.
Filtering with 0.22 μm microporous membrane, and separating with high performance liquid chromatography. Separating with C18 reverse chromatographic column, wherein water, methanol and acetonitrile are used as mobile phase, the column temperature of the chromatographic column is 50 deg.C, and the flow rate of the mobile phase is 0.80 mL/min; the procedure for linear gradient elution was: initial mobile phase water: methanol: acetonitrile in a volume ratio (14:28:58) eluted linearly to water: methanol: the volume ratio of acetonitrile is (4.67:19.33:76), and the separation time is 10 min.
The chromatographic separation result is shown in FIG. 6, the outflow substance is fucoxanthin at 8.31 min as shown by an arrow, and the absorption spectrum of 400-800nm (shown as an enlarged region in FIG. 6) is extracted, and the absorption peak is 449 nm. Fucoxanthin flows out from 7.69 minutes and ends at 8.66 minutes, and the outflow in the time period is collected and dried by using freezing vacuum to obtain pure fucoxanthin. The fucoxanthin extraction rate of the Sargassum horneri extracted by the method without chromatographic separation is calculated to be 2.02%, and the fucoxanthin purity obtained after HPLC chromatographic separation is calculated to be 95.27%.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (8)
1. A method for extracting fucoxanthin from Sargassum horneri powder is characterized in that the method for preparing the Sargassum horneri powder comprises the following steps:
(1) cleaning: collecting fresh copper algae, and cleaning algae by combining seawater and fresh water;
(2) drying in the shade: spreading the washed sargassum horneri, airing in a low-light environment, and manually picking out other algae;
(3) drying: transferring the sargassum horneri to a dryer, drying at 55-60 ℃, and continuously introducing nitrogen into the oven in the drying process;
(4) powder preparation: freezing and grinding the dried sargassum horneri, and screening the ground sargassum horneri by using a screen with 65-90 meshes to obtain sargassum horneri powder;
(5) and (3) sterilization: sterilizing the algae powder by ray irradiation, and storing at normal temperature in a dark place;
wherein, the steps (1), (2), (3) and (4) are operated under the environment that the light intensity does not exceed 200 Lux; the sterilization temperature is not more than 25 ℃, and the ambient light intensity is not more than 10 Lux;
the method for extracting fucoxanthin from the algae powder comprises the following steps:
(6) adding an extracting solution and steel balls into the algae powder, performing vibration extraction and centrifugation under the environment of weak light, low temperature and no oxygen to obtain a supernatant, wherein the extracting solution is a mixed solvent of methanol and acetone, and the volume ratio of the extracting solution to the acetone is 1: 1;
(7) repeatedly extracting, and combining the two supernatants;
(8) separating the supernatant obtained in step (7) by high performance liquid chromatography, and collecting the effluent phase;
(9) performing vacuum freeze drying on the fucoxanthin effluent collected in the step (8) to obtain a pure fucoxanthin product;
the column packing of the high performance liquid chromatography in the step (8) is a C18 reverse chromatographic column, the column temperature of the chromatographic column is 50 ℃, the flow rate of a mobile phase is 0.80mL/min, and the mobile phase is a mixed solution of water, methanol, acetonitrile and ethyl acetate; performing linear gradient elution, wherein an initial mobile phase is water-methanol-acetonitrile-ethyl acetate with a volume ratio of 14:28:58:0, and a final mobile phase is water-methanol-acetonitrile-ethyl acetate with a volume ratio of 0:30:70: 0; the separation time is 40 minutes, and the components within 8-9 minutes are collected, namely the fucoxanthin.
2. The method for extracting fucoxanthin from Sargassum horneri powder according to claim 1, wherein in the step (1), fresh Sargassum horneri is washed with clean seawater and then algae are quickly washed with clean fresh water, the salinity of the seawater is 30-35% o, the washing water pressure of the seawater and the fresh water is not more than 0.07MPa, and the time of contacting the algae with the fresh water is not more than 2 minutes.
3. The method for extracting fucoxanthin from Sargassum horneri powder according to claim 1, wherein the operation conditions in step (2) are as follows: the air humidity of the environment is not more than 50%, and the drying time in the shade is not more than 12 hours.
4. The method for extracting fucoxanthin from Sargassum horneri powder according to claim 1, wherein the nitrogen gas is introduced at a rate of 0.1-0.2V/min during the drying process in the step (3), the drying time is not more than 24 hours, and the fucoxanthin is turned over every 1-2 hours during the drying process, wherein V is the volume of the oven.
5. The method for extracting fucoxanthin from Sargassum horneri algae powder according to claim 1, wherein the ratio of the algae powder to the extract liquid in the step (6) is: 3ml of the extract was added to 1g of algal powder.
6. The method for extracting fucoxanthin from Sargassum horneri powder according to claim 1, wherein the diameter of the steel ball in the step (6) is 3-5 mm, and the steel ball is pre-cooled at 0 ℃.
7. The method for extracting fucoxanthin from Sargassum horneri meal according to claim 5, wherein the process conditions of the shaking extraction in the steps (6) and (7) are as follows: the light intensity of the environment is not more than 10Lux, the extraction temperature is 0 ℃, the extraction time is 3-10min, the sealed extraction is carried out, and nitrogen is introduced before the sealed extraction.
8. The method for extracting fucoxanthin from Sargassum horneri powder according to claim 1, wherein the temperature of the cold trap of the freeze-drying in the step (9) is set to-80 ℃ and the freeze-drying time is not more than 3 h.
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