CN117205599A - Method for efficiently extracting active ingredients of sea fennel - Google Patents
Method for efficiently extracting active ingredients of sea fennel Download PDFInfo
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- CN117205599A CN117205599A CN202311184466.7A CN202311184466A CN117205599A CN 117205599 A CN117205599 A CN 117205599A CN 202311184466 A CN202311184466 A CN 202311184466A CN 117205599 A CN117205599 A CN 117205599A
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- 241000125183 Crithmum maritimum Species 0.000 title claims abstract description 143
- 239000004480 active ingredient Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 118
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 66
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 40
- 239000001257 hydrogen Substances 0.000 claims abstract description 40
- 238000002156 mixing Methods 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 33
- 238000000605 extraction Methods 0.000 claims abstract description 24
- 230000005496 eutectics Effects 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 239000002002 slurry Substances 0.000 claims description 54
- 239000000203 mixture Substances 0.000 claims description 52
- 239000006228 supernatant Substances 0.000 claims description 19
- 241000196324 Embryophyta Species 0.000 abstract description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 18
- 239000000370 acceptor Substances 0.000 description 17
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 13
- 235000019743 Choline chloride Nutrition 0.000 description 13
- 229960003178 choline chloride Drugs 0.000 description 13
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- 239000004310 lactic acid Substances 0.000 description 9
- 235000014655 lactic acid Nutrition 0.000 description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 241000212314 Foeniculum Species 0.000 description 3
- 235000004204 Foeniculum vulgare Nutrition 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- 150000008442 polyphenolic compounds Chemical class 0.000 description 3
- 235000013824 polyphenols Nutrition 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229930003944 flavone Natural products 0.000 description 2
- 150000002212 flavone derivatives Chemical class 0.000 description 2
- 235000011949 flavones Nutrition 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- 230000000971 hippocampal effect Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for efficiently extracting active ingredients of sea fennel, in particular to the technical field of plant active ingredient extraction, which comprises the following steps: step one: preparing a eutectic solvent (DES), namely blending a hydrogen bond acceptor and a hydrogen bond donor in a molar ratio of 1:5-5:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment; step two: adding 0-50% of water into the prepared DES solvent; step three: preparing fresh sea fennel, and cleaning the fresh sea fennel; step four: grinding the cleaned sea fennel. The invention adopts the eutectic solvent (DES), can improve the extraction rate of the active ingredients of the sea fennel on the premise of not damaging the active ingredients, is simple and easy to operate, saves the cost and can meet the market demand.
Description
Technical Field
The invention relates to the technical field of extraction of plant active ingredients, in particular to a method for efficiently extracting fennel active ingredients.
Background
Sea Fennel is named hippocampal teeth and Samphire (Sea Fennel, samphire) and contains various amino acids, polyphenols and flavonoids in vivo, so that the Sea Fennel has high antioxidant activity, free radical scavenging, anti-inflammatory and other effects, and is widely applied to skin care products.
The active ingredients in the sea fennel are generally required to be extracted and then applied, the extraction method which is commonly used at present comprises a water extraction method, an organic solvent (ethyl acetate and methanol) extraction method, a carbon dioxide supercritical extraction method and the like, the water extraction method is safe and environment-friendly, but the extraction is incomplete, the dilution degree is large, the subsequent concentration usually needs high-temperature assistance and high energy consumption, active substances are easy to lose, and organic residues are easy to exist in the organic solvent method; although supercritical extraction can efficiently extract residual organic solvents, special equipment is generally required, the investment of fixed assets is large, and the energy consumption for maintaining the supercritical state is high.
Disclosure of Invention
In order to overcome the above-mentioned drawbacks of the prior art, an embodiment of the present invention provides a method for efficiently extracting active ingredients of fennel, so as to solve the above-mentioned problems in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions: a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending a hydrogen bond acceptor and a hydrogen bond donor in a molar ratio of 1:5-5:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 0-50% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: 10000g of the extracted slurry is centrifuged, and then the supernatant of the obtained centrifuged slurry is taken.
In a preferred embodiment, the temperature in the water bath in the first step is set to 80 ℃.
In a preferred embodiment, the stirring time in the water bath in the first step is 6 hours.
In a preferred embodiment, the time for sonicating the mixture of DES solvent and crushed fennel in step five is 20 minutes.
In a preferred embodiment, the temperature of the mixture of the DES solvent and the crushed sea fennel in the fifth step is controlled to 25-65 ℃.
In a preferred embodiment, the slurry after extraction in step six is centrifuged for 20 minutes.
The invention has the technical effects and advantages that:
firstly, mixing a hydrogen bond acceptor and a hydrogen bond donor in a molar ratio of 1:5-5:1, stirring in a water bath kettle, preparing a clear and transparent DES solvent by assistance of ultrasonic treatment, adding 0-50% by weight of water into the prepared DES solvent, preparing fresh sea fennel, cleaning the fresh sea fennel, grinding the clean sea fennel, mixing the DES solvent and the ground sea fennel in a ratio of 5:1-20:1, performing extraction on a mixture of the DES solvent and the ground sea fennel by using 50-200W ultrasonic treatment, taking 10000g of extracted slurry, centrifuging, taking the supernatant of the obtained centrifuged slurry, setting the temperature in the water bath kettle to be 80 ℃, setting the stirring time in the water bath kettle to be 6h, performing ultrasonic treatment on the mixture of the DES solvent and the ground sea fennel for 20min, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled to be 25-65 ℃, the centrifugation treatment time of the extracted slurry is 20min, the eutectic solvent (DES) is formed by mixing different kinds of hydrogen bond donors (alcohols or acids such as oxalic acid and the like) and hydrogen bond acceptors (choline chloride and the like) in different molar ratios, the interaction reduces the anion-cation electrostatic force forming hydrogen bonds, thus obviously reducing the solidifying point of the mixture, the melting point is lower than that of the liquid mixture of a single component, and the dissolution rate of active substances such as polyphenol, flavone and the like can be promoted by adopting the eutectic solvent (DES) under the premise of not damaging the active ingredients, the invention is easy, simple and convenient, saves the cost, and can meet the market demand.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor lactic acid in a molar ratio of 1:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 30% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 2
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor lactic acid in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 30% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 3
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor lactic acid in a molar ratio of 3:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 30% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 4
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor glycerol in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 30% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 5
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor oxalic acid in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 30% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 6
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor citric acid in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 30% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 7
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor lactic acid in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 0% by weight of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 8
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor lactic acid in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 10% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 9
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor lactic acid in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 50% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 10
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor lactic acid in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 30% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 25 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 11
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor choline chloride and hydrogen bond donor lactic acid in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 30% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 65 ℃;
and step six, centrifuging the extracted slurry for 20min.
Example 12
The invention provides a method for efficiently extracting active ingredients of sea fennel, which comprises the following steps:
step one: preparing a eutectic solvent (DES), namely blending hydrogen bond acceptor betaine and hydrogen bond donor lactic acid in a molar ratio of 2:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 30% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: taking 10000g of extracted slurry, centrifuging, and then taking the obtained supernatant of the centrifuged slurry;
the temperature in the water bath kettle in the first step is set to be 80 ℃;
the stirring time in the water bath kettle in the first step is 6 hours;
in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min;
in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled at 40 ℃;
and step six, centrifuging the extracted slurry for 20min.
Table 1 example data table
Comparative example 1
The existing method for extracting the active ingredients of the sea fennel comprises the following steps:
step one: preparing an extract liquid by methanol and water according to the volume ratio of 7:3;
step two: mixing the extractive solution with crushed fructus Foeniculi at a ratio of 5:1-20:1 (loading 5% -20%), and performing ultrasonic treatment at 50-200W for 20min to extract at 40deg.C;
step three: 10000g of the extracted slurry is centrifuged for 20min, and the supernatant of the obtained centrifuged slurry is taken.
Comparative example 2
The existing method for extracting the active ingredients of the sea fennel comprises the following steps:
step one: preparing an extraction liquid by ethanol and water according to the volume ratio of 7:3;
step two: mixing the extractive solution with crushed fructus Foeniculi at a ratio of 5:1-20:1 (loading 5% -20%), and performing ultrasonic treatment at 50-200W for 20min to extract at 40deg.C;
step three: 10000g of the extracted slurry is centrifuged for 20min, and the supernatant of the obtained centrifuged slurry is taken.
Comparative example 3
The existing method for extracting the active ingredients of the sea fennel comprises the following steps:
step one: ethyl acetate at 100% concentration was used as the extract;
step two: mixing the extractive solution with crushed fructus Foeniculi at a ratio of 5:1-20:1 (loading 5% -20%), and performing ultrasonic treatment at 50-200W for 20min to extract at 40deg.C;
step three: 10000g of the extracted slurry is centrifuged for 20min, and the supernatant of the obtained centrifuged slurry is taken.
Table 2 comparative example data sheet
Firstly, mixing a hydrogen bond acceptor and a hydrogen bond donor in a molar ratio of 1:5-5:1, stirring in a water bath kettle, preparing a clear and transparent DES solvent by assistance of ultrasonic treatment, adding 0-50% by weight of water into the prepared DES solvent, preparing fresh sea fennel, cleaning the fresh sea fennel, grinding the clean sea fennel, mixing the DES solvent and the ground sea fennel in a ratio of 5:1-20:1, performing extraction on a mixture of the DES solvent and the ground sea fennel by using 50-200W ultrasonic treatment, taking 10000g of extracted slurry, centrifuging, taking the supernatant of the obtained centrifuged slurry, setting the temperature in the water bath kettle to be 80 ℃, setting the stirring time in the water bath kettle to be 6h, performing ultrasonic treatment on the mixture of the DES solvent and the ground sea fennel for 20min, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled to be 25-65 ℃, the centrifugation treatment time of the extracted slurry is 20min, the eutectic solvent (DES) is formed by mixing different kinds of hydrogen bond donors (alcohols or acids such as oxalic acid and the like) and hydrogen bond acceptors (choline chloride and the like) in different molar ratios, the interaction reduces the anion-cation electrostatic force forming hydrogen bonds, thus obviously reducing the solidifying point of the mixture, the melting point is lower than that of the liquid mixture of a single component, and the dissolution rate of active substances such as polyphenol, flavone and the like can be promoted by adopting the eutectic solvent (DES) under the premise of not damaging the active ingredients, the invention is easy, simple and convenient, saves the cost, and can meet the market demand.
Finally: the foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (6)
1. A method for efficiently extracting active ingredients of sea fennel, which is characterized by comprising the following steps:
step one: preparing a eutectic solvent (DES), namely blending a hydrogen bond acceptor and a hydrogen bond donor in a molar ratio of 1:5-5:1, stirring in a water bath kettle, and preparing a clear and transparent DES solvent by assistance of ultrasonic treatment;
step two: adding 0-50% of water into the prepared DES solvent;
step three: preparing fresh sea fennel, and cleaning the fresh sea fennel;
step four: grinding the cleaned sea fennel;
step five: mixing DES solvent and crushed sea fennel at a ratio of 5:1-20:1, and then performing ultrasonic treatment on the mixture of DES solvent and crushed sea fennel at a concentration of 50-200W for extraction;
step six: 10000g of the extracted slurry is centrifuged, and then the supernatant of the obtained centrifuged slurry is taken.
2. The method for efficiently extracting active ingredients of sea fennel according to claim 1, wherein: the temperature in the water bath kettle in the first step is set to be 80 ℃.
3. The method for efficiently extracting active ingredients of sea fennel according to claim 1, wherein: and in the first step, stirring in a water bath kettle for 6 hours.
4. The method for efficiently extracting active ingredients of sea fennel according to claim 1, wherein: and in the fifth step, the time for ultrasonic treatment of the mixture of the DES solvent and the crushed sea fennel is 20min.
5. The method for efficiently extracting active ingredients of sea fennel according to claim 1, wherein: in the fifth step, the temperature of the mixture of the ultrasonic treatment DES solvent and the crushed sea fennel is controlled to be 25-65 ℃.
6. The method for efficiently extracting active ingredients of sea fennel according to claim 1, wherein: and step six, centrifuging the extracted slurry for 20min.
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