CN113521803A - Eutectic solvent, preparation method thereof and application of eutectic solvent in extraction of isofraxidin in acanthopanax senticosus - Google Patents
Eutectic solvent, preparation method thereof and application of eutectic solvent in extraction of isofraxidin in acanthopanax senticosus Download PDFInfo
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- CN113521803A CN113521803A CN202110889827.2A CN202110889827A CN113521803A CN 113521803 A CN113521803 A CN 113521803A CN 202110889827 A CN202110889827 A CN 202110889827A CN 113521803 A CN113521803 A CN 113521803A
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- B01D11/02—Solvent extraction of solids
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- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/06—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 2
- C07D311/08—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 2 not hydrogenated in the hetero ring
- C07D311/16—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 2 not hydrogenated in the hetero ring substituted in position 7
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Abstract
The invention provides a eutectic solvent, a preparation method thereof and application thereof in extracting isofraxidin from acanthopanax, belonging to the technical field of extraction of isofraxidin. The eutectic solvent is prepared from choline chloride, acid and water; the acid is citric acid or malic acid; the dosage ratio of the choline chloride, the acid and the water is (1-2) mol:2mol (200-400) mL. The eutectic solvent can effectively extract isofraxidin in acanthopanax senticosus and improve the yield of isofraxidin. The results of the examples show that the extraction of isofraxidin from acanthopanax senticosus by the eutectic solvent of the invention has higher yield compared with the extraction by ethanol.
Description
Technical Field
The invention relates to the technical field of extraction of isofraxidin, and in particular relates to a eutectic solvent, a preparation method thereof and application of the eutectic solvent in extraction of isofraxidin in acanthopanax senticosus.
Background
Acanthopanax senticosus is a traditional Chinese herbal medicine which is widely used, is always used as a functional food and is prepared into various medicinal preparations, and in the theory of traditional Chinese medicine, acanthopanax senticosus can tonify qi, invigorate spleen, nourish kidney, supplement body vitality, stimulate appetite and improve memory. In the past decades, researchers all over the world have conducted a great deal of chemical, pharmacological and clinical studies on acanthopanax senticosus, and found that acanthopanax senticosus has pharmacological effects on cardiovascular, central nervous and immune systems, and has anti-stress, anti-ulcer, anti-radiation, anti-cancer, anti-inflammatory and liver-protecting effects. Studies have found that acanthopanax contains various compounds, among which syringin, eleutheroside E and isofraxidin are the main pharmacologically active ingredients of acanthopanax, and the extracts thereof have been used for recovery after treatment of severe diseases.
The components in acanthopanax have different properties, different extraction, purification and analysis methods are applied according to different components, the traditional extraction method is an organic solvent extraction method, and different components in acanthopanax are extracted by using organic solvents such as ethanol with different concentrations through the principle of similar compatibility, however, the extraction method has low specificity, the obtained extract has complex components and low yield.
Disclosure of Invention
The invention aims to provide a eutectic solvent, a preparation method thereof and application of the eutectic solvent in extraction of isofraxidin in acanthopanax senticosus, and the solvent provided by the invention can effectively extract isofraxidin in acanthopanax senticosus and improve the yield of isofraxidin.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a eutectic solvent, which is prepared from choline chloride, acid and water; the acid is citric acid or malic acid; the dosage ratio of the choline chloride, the acid and the water is (1-2) mol:2mol (200-400) mL.
Preferably, when the acid is citric acid, the dosage ratio of the choline chloride, the acid and the water is (1-2) mol:2mol (200-400) mL.
Preferably, when the acid is malic acid, the dosage ratio of the choline chloride to the acid to the water is 2mol:2mol (200-400) mL.
The invention provides a preparation method of the eutectic solvent in the scheme, which comprises the following steps: choline chloride, acid and water are mixed, and the obtained mixed solution is stirred for 1.5-2 hours at the temperature of 80-90 ℃ to form a eutectic solvent.
Preferably, the stirring speed is 200-500 r/min.
The invention provides an application of the eutectic solvent or the eutectic solvent prepared by the preparation method in the scheme in the extraction of isofraxidin in acanthopanax senticosus.
Preferably, the method of application comprises the steps of:
mixing acanthopanax powder with a eutectic solvent, performing ultrasonic wall breaking treatment, and stirring in a water bath condition to obtain an initial extraction solution;
centrifuging the primary extract to obtain a supernatant;
and filtering the supernatant to obtain an extract containing isofraxidin.
Preferably, the power of the ultrasonic wall breaking treatment is 400-600W, and the time is 5-10 min; the temperature of the water bath is 80-100 ℃, and the time is 1.5-3 h.
Preferably, the preparation method of the acanthopanax powder comprises the following steps: drying acanthopanax senticosus at 80-100 ℃ for 1-2 h, then crushing and sieving with a sieve of 80-100 meshes, and baking the obtained undersize for 1-2 h at 80-100 ℃.
Preferably, the use amount ratio of the acanthopanax powder to the eutectic solvent is 1 g: (10-20) mL.
The invention provides a eutectic solvent, which is prepared from choline chloride, acid and water; the acid is citric acid or malic acid; the dosage ratio of the choline chloride, the acid and the water is (1-2) mol:2mol (200-400) mL.
The eutectic solvent can effectively extract isofraxidin in acanthopanax senticosus and improve the yield of isofraxidin. The results of the examples show that the extraction of isofraxidin from acanthopanax senticosus by the eutectic solvent of the invention has higher yield compared with the extraction by ethanol.
Drawings
FIG. 1 is a chromatogram of isofraxidin standard.
Detailed Description
The invention provides a eutectic solvent, which is prepared from choline chloride, acid and water; the acid is citric acid or malic acid; the dosage ratio of the choline chloride, the acid and the water is (1-2) mol:2mol (200-400) mL.
In the present invention, when the acid is citric acid, the amount ratio of the choline chloride, the acid and the water is preferably (1-2) mol:2mol (200-400) mL, more preferably 2mol:2mol (200-400) mL, and still more preferably 2mol:2mol:200 mL.
In the invention, when the acid is malic acid, the dosage ratio of the choline chloride, the acid and the water is preferably 2mol:2mol (200-400) mL, and more preferably 2mol:2mol:200 mL.
In the present invention, the acid is preferably citric acid; the water is preferably ultrapure water.
The invention provides a preparation method of the eutectic solvent in the scheme, which comprises the following steps: choline chloride, acid and water are mixed, and the obtained mixed solution is stirred for 1.5-2 hours at the temperature of 80-90 ℃ to form a eutectic solvent.
The invention has no special requirements on the mixing process, and can uniformly mix all the raw materials.
The invention preferably stirs at 80 ℃ for 2 h. Magnetic stirring is preferably employed in the present invention. In the invention, the stirring speed is preferably 200-500 r/min, and more preferably 500 r/min. The stirring is preferably carried out under the condition of a constant-temperature water bath.
The method adopts a constant-temperature heating magnetic stirring method to prepare the eutectic solvent, has the advantages of high sensitivity, strong controllability, simple operation, high heating speed, uniform and stable solution temperature and high stirring efficiency, and accords with the green chemical guiding principle.
The invention provides an application of the eutectic solvent or the eutectic solvent prepared by the preparation method in the scheme in the extraction of isofraxidin in acanthopanax senticosus.
In the present invention, the method of application preferably comprises the steps of:
mixing acanthopanax powder with a eutectic solvent, performing ultrasonic wall breaking treatment, and stirring in a water bath condition to obtain an initial extraction solution;
centrifuging the primary extract to obtain a supernatant;
and filtering the supernatant to obtain an extract containing isofraxidin.
The method comprises the steps of mixing acanthopanax powder with a eutectic solvent, carrying out ultrasonic wall breaking treatment, and then stirring under a water bath condition to obtain an initial extraction solution.
In the present invention, the method for preparing acanthopanax powder preferably comprises: drying acanthopanax senticosus at 80-100 ℃ for 1-2 h, then crushing and sieving with a 80-100 mesh sieve, baking the obtained undersize at 80-100 ℃ for 1-2 h, more preferably drying acanthopanax senticosus at 80 ℃ for 1h, then crushing and sieving with a 80 mesh sieve, and baking the obtained undersize at 80 ℃ for 2 h. The invention removes free water by baking, and ensures the calculation of the subsequent extraction rate.
In the present invention, the ratio of the acanthopanax powder to the eutectic solvent is preferably 1 g: (10-20) mL, more preferably 1 g: 20 mL.
In the present invention, the mixing of the acanthopanax powder with the eutectic solvent is preferably vortex mixing, and the time of vortex mixing is preferably 2 min.
In the invention, the power of the ultrasonic wall breaking treatment is preferably 400-600W, more preferably 500W, and the time is preferably 5-10 min, more preferably 5 min; the invention improves the dissolving-out amount of isofraxidin by ultrasonic wall breaking treatment.
In the invention, the temperature of the water bath is preferably 80-100 ℃, more preferably 80 ℃, and the time is preferably 1.5-3 h, more preferably 2 h. The present invention does not require any particular speed of agitation, and can employ agitation speeds well known in the art. The method comprises the step of stirring for 2 hours at the temperature of 80 ℃ in a water bath to fully and uniformly mix the solute and the extraction medium, so that the isofraxidin is dissolved out.
After the primary extraction liquid is obtained, the invention centrifuges the primary extraction liquid to obtain supernatant. In the present invention, the rotation speed of the centrifugation is preferably 10000rpm, and the time of the centrifugation is preferably 10 min. The invention removes insoluble impurities by centrifugation to obtain supernatant.
After the supernatant is obtained, the invention filters the supernatant to obtain the extracting solution containing isofraxidin.
The invention preferably adopts a microporous filter membrane with the pore diameter of 0.22 μm for filtration. According to the invention, impurities with large particle size are removed by filtering, so that the chromatographic column is prevented from being blocked during the subsequent measurement of the content of isofraxidin.
The isofraxidin-containing extract solution of the present invention contains various acanthopanax senticosus extracts in addition to isofraxidin, and those skilled in the art can select and purify the isofraxidin-containing extract solution according to actual needs, which is not particularly limited in the present invention.
The eutectic solvent, the preparation method thereof and the application thereof in extracting isofraxidin from acanthopanax senticosus will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Accurately weighing 0.2000mol of choline chloride, 0.2000mol of citric acid and 20mL of ultrapure water, and putting a stirrer for fully mixing; and heating the obtained mixed solution in a water bath at 80 ℃ in a constant-temperature water bath, and stirring at the speed of 500r/min for 2 hours to prepare the eutectic solvent.
Application example 1
The method for extracting the carisopyridazine comprises the following steps:
A. collecting radix Acanthopanacis Senticosi sample, drying in air, placing in an oven, drying at 80 deg.C for 1 hr, pulverizing, sieving with 80 mesh sieve, and baking in 80 deg.C oven for 2 hr to obtain radix Acanthopanacis Senticosi powder;
B. putting 1.0g of acanthopanax powder into a conical flask, adding 20.00mL of the eutectic solvent in example 1, performing ultrasonic wall breaking treatment for 5min after swirling for 2min, and stirring for 2 hours in a water bath at 80 ℃ to obtain a primary extract;
C. centrifuging the primary extract for 10min, precisely sucking 1mL of supernatant after centrifugation, placing in a 100mL volumetric flask, diluting with ultrapure water to constant volume, mixing, and filtering with 0.22 μm microporous membrane to obtain extract containing isofraxidin.
Example 2
Accurately weighing 0.2000mol of choline chloride and malic acid respectively and 20mL of ultrapure water, and adding a stirrer for fully mixing; and heating the obtained mixed solution in a water bath at 80 ℃ in a constant-temperature water bath, and stirring at the speed of 500r/min for 2 hours to prepare the eutectic solvent.
Application example 2
The difference from application example 1 was only in that the extraction was performed using the eutectic solvent prepared in example 2.
Example 3
Accurately weighing 0.1000mol of choline chloride, 0.2000mol of citric acid and 20mL of ultrapure water, and putting a stirrer for fully mixing; and heating the obtained mixed solution in a water bath at 80 ℃ in a constant-temperature water bath, and stirring at the speed of 500r/min for 2 hours to prepare the eutectic solvent.
Application example 3
The difference from application example 1 was only in that the extraction was performed using the eutectic solvent prepared in example 3.
Example 4
Accurately weighing 0.2000mol of choline chloride, 0.2000mol of citric acid and 40mL of ultrapure water, and putting a stirrer for fully mixing; and heating the obtained mixed solution in a water bath at 80 ℃ in a constant-temperature water bath, and stirring at the speed of 500r/min for 2 hours to prepare the eutectic solvent.
Application example 4
The difference from application example 1 was only in that the extraction was performed using the eutectic solvent prepared in example 4.
Example 5
Accurately weighing 0.2000mol of choline chloride, 0.2000mol of citric acid and 20mL of ultrapure water, and putting a stirrer for fully mixing; and heating the obtained mixed solution in a water bath at 80 ℃ in a constant-temperature water bath, and stirring at the speed of 500r/min for 2 hours to prepare the eutectic solvent.
Application example 5
The difference from application example 1 is that the extraction was performed using the eutectic solvent of example 5, and the amount of the eutectic solvent used was 10 mL.
Comparative example
The difference from application example 1 is that extraction was performed with 70% ethanol.
And (3) testing:
and detecting the isofraxidin-containing extracting solution obtained in the examples 1-5 and the comparative example by adopting a high performance liquid chromatography-orbital trap mass spectrometry (U hPLC-ESI-Orbitrap-MS/MS) method to test the content of the isofraxidin. The method comprises the following specific steps:
a. the isofraxidin extract is measured by U hPLC-ESI-Orbitrap-MS/MS, and the isofraxidin mass spectrum data is measured by Compound discover 3.1TMAnd (4) identifying the software.
Chromatographic conditions are as follows:
the chemical components of the sample were separated by a Dionex Ultimate 3000 hplc. The chromatograph consists of a vacuum exhaust system, a pump system, a sample tray with a temperature control system, an automatic sample injector, a chromatographic column, a column temperature control system and a DAD detector. The instrument was used in conjunction with a T her mo Scientific hypersil GOLD aQ (2.1 mm. times.100 mm, 1.9 μm) chromatography column (C18, 4.6. times.150 mm, 5 μm). The chromatographic conditions were as follows: formic acid water (0.1%, v/v) and formic acetonitrile (0.1%, v/v) were mobile phases A and B, respectively. Elution gradient procedure: 0-2 minutes, 5% B; 2-42 minutes, 5-95% B; 42-47 minutes, 95% B; 47.1 min, 5% B; 47.1-50 minutes, 5% B. The gradient flow rate was maintained at 0.3mL min-1The column temperature was 40 ℃ and the amount of sample was 5. mu.L.
Mass spectrum conditions:
the high resolution mass spectral parameters were set as follows: sheath gas pressure, 40 psi; the assist gas pressure was 20 psi; purge gas pressure 10 psi; capillary voltage, 3 kV; the ion transfer tube temperature was 320 ℃. AUG gas heating temperature is 350 ℃; collision gas: nitrogen gas; normalized collision energy 20, 40, 60 eV; RF lens amplitude field strength (s-lens): 60. automatic triggering of secondary mass spectrum scanning mode (Fullms-ddms) in combination with selection of primary mass spectrum full scan2). Resolution ratio: the first-level and second-level high-resolution mass spectrum resolutions are respectively as follows: 70000F WhM/17500F WhM; the ion scanning range, m/z is 50-1500; and (3) cycle counting: 3 times; a four-level isolation window, 1.5 m/z; dynamic exclusion time 5 seconds.
b. Accurately weighing 2mg of isofraxidin standard substance, placing the isofraxidin standard substance in a 10mL volumetric flask, adding methanol for dilution and fixing the volume to prepare 0.2mg/mL of isofraxidin standard stock solution. Taking a proper amount of isofraxidin standard stock solution, and diluting with methanol to prepare standard solutions with the concentrations of 0.007mg/mL, 0.005mg/mL, 0.003mg/mL, 0.002mg/mL and 0.001 mg/mL. Shaking up, and measuring the peak area by UhPLC-ESI-Orbitrap-MS/MS according to the method in the step a; the chromatogram of the obtained isofraxidin standard is shown in FIG. 1, and the upper right corner in FIG. 1 is the nucleus ratio of the extracted ions.
c. B, taking the chromatographic peak area of the isofraxidin standard solution measured in the step b, and calculating a regression equation and a linear coefficient; y is 10060867517.63X +19976535.05, R20.9812, where X is concentration and y is peak area; and performing linear fitting on the concentration by using the peak area by adopting a least square method, and performing linear range and regression analysis.
d. And (c) taking the chromatographic peak area of the isofraxidin standard solution measured in the step b, and calculating to obtain the quantitative limit of the isofraxidin of 27.6407 ng/mL.
e. And (c) taking the chromatographic peak area of the isofraxidin standard solution measured in the step (b) to perform precision investigation, and taking the repeatability test investigation method to investigate the precision, wherein the measured values of the concentrations of the isofraxidin standard solution in the ranges of 0.1mg/mL, 0.01mg/mL and 0.002mg/mL are 0.1083 +/-0.0021 mg/mL, 0.0115 +/-0.00017 mg/mL and 0.0019 +/-0.00004 mg/mL, the RSD% values are 1.93%, 1.47% and 2.11% respectively, the results are all in a limited range, and the system error does not influence the experimental determination result. The method has good precision.
f. And (c) after the step a is finished, taking the isofraxidin standard substance solution of the step b at 0.2mg/mL, 0.01mg/mL and 0.002mg/mL, testing blank recovery rate and sample application recovery rate under different concentrations, and inspecting the accuracy of the method. The result shows that the blank recovery rate of 0.2mg/mL is 85.7%, and the sample recovery rate is 93.1%; the blank recovery rate of 0.01mg/mL is 90.0%, and the sample recovery rate is 82.1%; the blank recovery rate of 0.002mg/mL is 87.2%, the sample recovery rate is 80.7%, the experimental results of the recovery rates of isofraxidin are all within 80% -100%, and the detection method has good accuracy.
g. And c, calculating the content of isofraxidin in the extracting solution by using the regression equation measured in the step c. The results of the content of isofraxidin in application examples 1 to 5 and comparative examples are shown in Table 1.
TABLE 1 Isofraxidin content
As can be seen from the results in table 1, extraction of isofraxidin from acanthopanax senticosus with the eutectic solvent according to the present invention has a higher extraction rate than ethanol.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A eutectic solvent is prepared from choline chloride, acid and water; the acid is citric acid or malic acid; the dosage ratio of the choline chloride, the acid and the water is (1-2) mol:2mol (200-400) mL.
2. The eutectic solvent according to claim 1, wherein when the acid is citric acid, the choline chloride, the acid and water are used in a ratio of (1-2) mol:2mol (200-400) mL.
3. The eutectic solvent as claimed in claim 1, wherein when the acid is malic acid, the choline chloride, the acid and water are used in a ratio of 2mol:2mol (200-400) mL.
4. A method for preparing the eutectic solvent according to any one of claims 1 to 3, comprising the steps of: choline chloride, acid and water are mixed, and the obtained mixed solution is stirred for 1.5-2 hours at the temperature of 80-90 ℃ to form a eutectic solvent.
5. The method according to claim 4, wherein the stirring rate is 200 to 500 r/min.
6. Use of the eutectic solvent according to any one of claims 1 to 3 or the eutectic solvent prepared by the preparation method according to any one of claims 4 to 5 for extracting isofraxidin from Acanthopanax senticosus.
7. The application according to claim 6, characterized in that the method of application comprises the steps of:
mixing acanthopanax powder with a eutectic solvent, performing ultrasonic wall breaking treatment, and stirring in a water bath condition to obtain an initial extraction solution;
centrifuging the primary extract to obtain a supernatant;
and filtering the supernatant to obtain an extract containing isofraxidin.
8. The application of claim 7, wherein the power of the ultrasonic wall breaking treatment is 400-600W, and the time is 5-10 min; the temperature of the water bath is 80-100 ℃, and the time is 1.5-3 h.
9. The use of claim 7, wherein the Acanthopanax senticosus powder is prepared by a method comprising: drying acanthopanax senticosus at 80-100 ℃ for 1-2 h, then crushing and sieving with a sieve of 80-100 meshes, and baking the obtained undersize for 1-2 h at 80-100 ℃.
10. The use of claim 7, wherein the ratio of the acanthopanax senticosus powder to the eutectic solvent is 1 g: (10-20) mL.
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Application publication date: 20211022 |