A method for extracting high-purity quebracho alcohol from seabuckthorn leaves
Through simplified water deposition, resin decolorization and low-temperature evaporation solvent purification processes, combined with the gradient elution technology of liquid chromatography, the problems of long time and low transfer rate of high-purity white lemonol in the existing technology have been successfully solved, and the problem of high-purity white lemonol preparation in the existing technology has been achieved. Efficient and simple preparation of high-purity white-sturdy licorice.
Patent Information
- Application Number
- CN202310108904.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Priority Date
- 2022-12-13
- Filing Date
- 2023-02-14
- Publication Date
- 2025-02-18
- Estimated Expiration
- 2043-02-14
AI Technical Summary
The method for preparing high-purity white-clean keratin in the prior art has a long preparation time, cumbersome process, and low transfer rate. It is impossible to obtain more high-purity white-clean keratin in a short time.
By pulverizing and extracting the dried sea buckthorn leaves, decolorizing, decolorizing ADS-17 anion exchange resin, and evaporating solvent at low temperature, gradient elution was performed in the preparation liquid chromatograph, and the fractions for a specific time period were collected. Obtain high purity white-sturdy lichenol.
The preparation cycle is greatly shortened, the process operation is simple and easy to operate, the transfer rate is high, and the product purity reaches ≥99.5%.
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Figure CN116253624B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of extraction and purification of effective components in plants, and in particular to a method for extracting high-purity quebracho alcohol from seabuckthorn leaves. Background Art
[0002] Seabuckthorn (Hippophae rhamnoides Linn.) is a plant resource that can be used as both medicine and food. It is widely planted in the northwest of my country. Seabuckthorn likes light, is cold-resistant, heat-resistant, resistant to wind and sand and drought climate, has strong adaptability to soil, and can survive in saline-alkali environments. Seabuckthorn leaves are usually nearly opposite, similar to paper, and are narrowly lanceolate or rectangular-lanceolate in shape, about 33-85 mm long and about 4-13 mm wide. Seabuckthorn leaves are one of the important nutritional parts of seabuckthorn. Research on the extraction and purification process of the active ingredients in seabuckthorn leaves can enhance the application value of seabuckthorn.
[0003] There are many bioactive substances in seabuckthorn leaves, mainly including flavonoids, polysaccharides, vitamin C and terpenoid components. Pharmacological studies have shown that seabuckthorn leaves have antioxidant, antibacterial, hypoglycemic and liver protection effects. Seabuckthorn leaf extracts are widely used in livestock and poultry feed, medicine and health care products.
[0004] Quebracholic acid, also known as white quebracholic alcohol, is an effective active ingredient in seabuckthorn leaves. Modern medical research shows that quebracholic acid is closely related to the hypoglycemic effect of seabuckthorn leaf extract. At present, high-purity quebracholic acid is mainly obtained through macroporous resin adsorption purification, membrane separation, organic solvent extraction, crystallization, recrystallization, etc., which takes a long time to prepare and has low production efficiency. It is impossible to obtain more high-purity quebracholic acid in a short time. Summary of the invention
[0005] The purpose of the present invention is to provide a method for extracting high-purity quebracho alcohol from seabuckthorn leaves in view of the problems of long preparation time, complicated process and low transfer rate in the existing method for preparing quebracho alcohol in the industry.
[0006] A method for extracting high-purity quebracho alcohol from seabuckthorn leaves of the present invention comprises the following steps:
[0007] (1) Extraction: The dried seabuckthorn leaves were crushed and sieved, dissolved and extracted with ethanol solution, the extract and the residue were collected, and the extract was concentrated under reduced pressure to obtain sample 1;
[0008] (2) Water precipitation: add pure water to sample 1, heat to dissolve, filter, and collect the filtrate;
[0009] (3) Decolorization: The filtrate is passed through an ADS-17 anion exchange resin column, and the decolorized effluent is collected and dried under reduced pressure to obtain a dried product of the effluent, which is Sample 2;
[0010] (4) Preliminary purification: dissolve sample 2 in a glass container using ethanol, evaporate the solvent at low temperature, and collect the dry solid in the glass container to obtain sample 3;
[0011] (5) Purification: Sample 3 was dissolved, filtered, and poured into a preparative liquid chromatograph for gradient elution. The fractions eluting in a specific time period were collected and dried to obtain quebracho alcohol crystals.
[0012] Preferably, in step (1), the seabuckthorn leaves are crushed and passed through a 30-60 mesh sieve, the mass fraction of the ethanol solution is 60-95%, the mass volume ratio of the seabuckthorn leaves to the ethanol solution is 1-2:6-15, the number of extractions is 1-3 times, the extraction time for each time is 1-4 hours, and the extraction temperature is 10-60°C.
[0013] Preferably, in step (1), the extract is concentrated under reduced pressure to 1 / 5-1 / 4 of the original volume, which is sample 1.
[0014] Preferably, in step (2), the volume ratio of sample 1 to pure water is 1:2-5, and the dissolution temperature is 30-90°C.
[0015] Preferably, in step (3), the mass volume ratio of ADS-17 anion exchange resin to filtrate is 1:2-6, the pressure of reduced pressure drying is -0.08-0.1 MPa, and the temperature is 10-60°C.
[0016] Preferably, in step (4), the mass fraction of the ethanol solution is 60-80%, the mass volume ratio of sample 2 to the ethanol solution is 1:1-5, and the solvent evaporation temperature is 20-50°C.
[0017] Preferably, in step (5), the solvent used to dissolve the sample 3 is pure water or acetonitrile, and the mass volume ratio of the sample 3 to the solvent is 1:2-4.
[0018] Preferably, in step (5), the mobile phase used in the preparative liquid chromatograph is acetonitrile-water, the elution flow rate is 10-30 mL / min, and the detection wavelength is 245 nm.
[0019] Furthermore, in step (5), the mobile phase elution gradient is as follows:
[0020]
[0021] The specific time period for collecting fractions was 1.5-4.0 min.
[0022] Preferably, in step (5), the collected fraction is dried to obtain high-purity quebracho alcohol crystals with a purity of ≥99.5%.
[0023] The beneficial effects produced by the present invention are:
[0024] 1. The process operation is simple and easy, and the production cycle is short: the conventional extraction and purification process of high-purity white quebracho alcohol includes impurity removal, protein removal, organic solvent extraction to remove flavonoids, preliminary purification through membrane, crystallization, and recrystallization. In particular, crystallization and recrystallization take up a lot of time, which seriously slows down the production progress. The present invention directly performs simple water precipitation, resin decolorization, low-temperature evaporation solvent purification, and then prepares the liquid phase for separation and purification to obtain high-purity white quebracho alcohol, which greatly shortens the preparation cycle. At the same time, the mobile phase of the prepared liquid phase only uses a single organic solvent acetonitrile, which has the advantages of cost saving and high drying efficiency.
[0025] 2. High transfer rate: The conventional process for preparing high-purity quebracho alcohol requires the use of deproteinization, organic solvent extraction, macroporous resin purification, membrane purification, crystallization and recrystallization. During macroporous resin purification, the resin will adsorb quebracho alcohol when eluted with an organic solvent, resulting in a low transfer rate; membrane purification will cause a serious drop in transfer rate due to incomplete top washing; a large amount of quebracho alcohol remains in the mother liquor of crystallization and recrystallization and cannot be reused, resulting in a low transfer rate; the water precipitation, resin decolorization and low-temperature evaporation of solvent preliminary purification of the present invention will hardly reduce the transfer rate of quebracho alcohol, and the transfer rate of the preparation liquid phase purification process is relatively high. Therefore, the transfer rate of quebracho alcohol of the present invention is much higher than that of the conventional method.
[0026] 3. High product purity: The high-purity quebracho alcohol prepared by the method of the present invention has a purity higher than 99.5%. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] FIG1 is the NMR spectrum data of the quebracho alcohol sample prepared in Example 1 of the present invention;
[0028] Figure 1A for 1 H-NMR (500 MHz) spectrum;
[0029] Figure 1B for 13 C-NMR (125 MHz) spectrum;
[0030] Figure 1C is the molecular structure formula of quebracho alcohol;
[0031] Figure 2 This is a preparative liquid chromatogram for determining the time period for collecting the quebracho alcohol fraction in Example 1 of the present invention. DETAILED DESCRIPTION
[0032] A method for extracting high-purity quebracho alcohol from seabuckthorn leaves of the present invention comprises the following steps:
[0033] (1) Extraction: Crush the dried seabuckthorn leaves and pass them through a 30-60 mesh sieve, dissolve the seabuckthorn leaves in an ethanol solution with a mass fraction of 60-95%, and the mass volume ratio of the seabuckthorn leaves to the ethanol solution is 1-2:6-15. Extract 1-3 times at 10-60°C, each extraction time for 1-4 hours, collect the extract and the filter residue, and concentrate the extract under reduced pressure to 1 / 5-1 / 4 of the original volume to obtain sample 1;
[0034] (2) Water precipitation: Dissolve sample 1 and pure water at a volume ratio of 1:2-5 at a temperature of 30-90°C, filter, and collect the filtrate;
[0035] (3) Decolorization: the filtrate is passed through an ADS-17 anion exchange resin column, the mass volume ratio of the resin to the filtrate is 1:2-6, the decolorized effluent is collected, and vacuum dried under the conditions of -0.08- -0.1 MPa and 10-60°C to obtain a dried product of the effluent, which is sample 2;
[0036] (4) Preliminary purification: dissolve sample 2 in a glass container using an ethanol solution with a mass fraction of 60-80%, with the mass volume ratio of sample 2 to the ethanol solution being 1:1-5, evaporate the solvent at 20-50°C, collect the dry solid in the glass container, and obtain sample 3;
[0037] (5) Purification: Sample 3 was dissolved in pure water or acetonitrile, with the mass volume ratio of sample 3 to pure water or acetonitrile being 1:2-4. After dissolution and filtration, the sample was poured into a preparative liquid chromatograph for gradient elution. The mobile phase was acetonitrile-water, the elution flow rate was 10-30 mL / min, and the detection wavelength was 245 nm. The fractions flowing out at 1.5-4.0 min were collected and dried to obtain high-purity quebracho alcohol crystals. The mobile phase elution gradient was performed as shown in the following table:
[0038]
[0039] The present invention is explained in detail below in conjunction with examples, but the following examples do not limit the present invention in any way.
[0040] Example 1
[0041] A method for extracting high-purity quebracho alcohol from seabuckthorn leaves comprises the following steps:
[0042] (1) The dried seabuckthorn leaves were crushed and passed through a 30-mesh sieve. 2000 g of the crushed seabuckthorn leaves were accurately weighed (the content of quebracho alcohol in the seabuckthorn leaves was 5% as determined by ultra-high performance liquid chromatography). The seabuckthorn leaves were extracted with 15 times the volume of a 90% ethanol solution at a mass fraction of 45°C for 3 times, each time for 2 h. The extract and the residue were collected and discarded. The extract was concentrated under reduced pressure to 1 / 5 of the original volume to obtain 355 g of the sample.
[0043] (2) Add 3 times the volume of pure water to sample 1 and heat it to dissolve at 80°C. Filter and collect 1063 mL of the filtrate.
[0044] (3) The filtrate was loaded with 213 g of ADS-17 anion exchange resin column for decolorization, and the decolorized effluent was collected and dried under reduced pressure at -0.08 MPa and 60 °C to obtain 218 g of the dried effluent, i.e., Sample 2.
[0045] (4) Add 2.5 times the volume mass fraction of 80% ethanol solution to sample 2 and dissolve it in a glass container. Evaporate the solvent at 45°C and collect 135 g of dry solid in the glass container to obtain sample 3.
[0046] (5) Sample 3 was dissolved in 405 mL of pure water, filtered and poured into a preparative liquid chromatograph for gradient elution. The mobile phase was acetonitrile-water, the elution flow rate was 20 mL / min, and the detection wavelength was 245 nm. The fractions eluting at 2.0-3.0 min were collected and dried to obtain 96.2 g of high-purity quebracho alcohol crystals. The mobile phase elution gradient was performed as shown in the following table:
[0047] After testing, the purity of the quebracho alcohol prepared in this embodiment is 99.91%. After calculation, the transfer rate of extracting quebracho alcohol using the method of this embodiment is 96.11%.
[0048] The quebracho alcohol prepared in this example was used for structural identification, fraction time determination, and purity testing, and the results are as follows.
[0049] 1. Take the quebracho alcohol crystal product obtained in Example 1 for structural identification.
[0050] The main instrument used is: DPX-500 nuclear magnetic resonance spectrometer (Bruker, Switzerland). NMR analysis The NMR spectrum data of the white quebracho alcohol sample prepared in Example 1 is shown in Figure 1. In the figure, Figure 1A for 1 H-NMR (500 MHz) spectrum; Figure 1B for 13C-NMR (125 MHz) spectrum; Figure 1C The molecular structure of the obtained quebracho alcohol is shown in FIG.
[0051] As can be seen from the figure: 1 H-NMR (D 2 O, 500 MHz) δ: 3.34(1H, dd, J=3.0, 9.6 Hz, H-2), 3.39(3H, s, H-OMe), 3.55(2H, m, H-3, 4), 3.68(1H, dd, J=9.7, 3.2 Hz, H-5), 4.00(1H, t, J=3.7 Hz, H-6), 4.21(1H, t, J=3.7 Hz, H-1); 13 C-NMR (D 2 O, 125 MHz)δ: 57.5 (Me), 67.6(C-1), 80.8(C-2), 73.3(C-3), 72.6(C-4), 70.9(C-5), 71.9(C-6). The above data were compared with the spectral data information of white quebracho alcohol reported in the literature. The results showed that the spectral data of the product prepared in this embodiment were the same as the spectral data of natural white quebracho alcohol, and it was determined that the product prepared in this embodiment was white quebracho alcohol.
[0052] 2. Use preparative high performance liquid chromatography to locate the time period for collecting the quebracho alcohol fraction.
[0053] The main reagents and instruments used: Quebracho alcohol (C 7 H 14 O 6 ) Reference substance: Chengdu Gelipu Biotechnology Co., Ltd., CAS: 642-38-6, content 99.92%; preparative high performance liquid chromatography was purchased from Agilent Technologies.
[0054] The test results are as follows Figure 2 As shown in the figure, A shows white quebracho alcohol (C 7 H 14 O 6 ) The peak time period of the reference substance fraction is 1.0-4.0 min; B is the peak spectrum of the fraction of sample 3 of this embodiment, Figure 2 It can be seen that the sample 3 prepared in this example also has a peak time of the quebracho alcohol fraction in this section, and high-purity quebracho alcohol can be obtained by simply collecting and drying the fraction in this section.
[0055] 3. The purity of the quebracho alcohol in this example was determined using an ultra-high performance liquid chromatograph, and the transfer rate was calculated.
[0056] Main reagents and instruments: Quebracho alcohol (C 7 H 14 O 6 ) Reference substance: Chengdu Glip Biotechnology Co., Ltd., CAS: 642-38-6, content 99.92%; Waters ACQUITY ultra-high performance liquid chromatograph, AllChrom ELSD6000 evaporative light detector, amide chromatographic column (such as Waters ACQUITY UPLC® BEH Amide 1.7µm 2.1*100mm or equivalent) were purchased from Waters.
[0057] Experimental parameters: mobile phase: acetonitrile: water = 70:30 (V:V), flow rate: 0.5 mL / min, column temperature: 25 °C, injection volume: 1 µL.
[0058] The transfer rate of quebracho alcohol was calculated according to formula 1. The calculation formula is as follows:
[0059] Y=(A×B) / (C×D) Formula 1
[0060] Wherein: Y: quebracho transfer rate, %; A: mass of high-purity quebracho obtained in each embodiment, g; B: purity of high-purity quebracho obtained in each embodiment, %; C: mass of seabuckthorn leaves used in the experiment, g; D: content of quebracho in seabuckthorn leaves in the experiment, %.
[0061] The experimental results show that the mass percentage of the quebracho alcohol prepared in this embodiment is 99.91%. According to formula 1, the transfer rate of the quebracho alcohol in this embodiment is 96.11%.
[0062] Example 2
[0063] A method for extracting high-purity quebracho alcohol from seabuckthorn leaves comprises the following steps:
[0064] (1) The dried seabuckthorn leaves were crushed and passed through a 40-mesh sieve. 2000 g of the crushed seabuckthorn leaves were accurately weighed (the content of quebracho alcohol in the seabuckthorn leaves was 5% as determined by ultra-high performance liquid chromatography). The seabuckthorn leaves were extracted with 6 volumes of 95% ethanol solution at a temperature of 40°C for 2 times, each time for 3 h. The extract and the residue were collected and discarded. The extract was concentrated under reduced pressure to 1 / 5 of the original volume to obtain 352 g of the sample.
[0065] (2) Add 3 times the volume of pure water to sample 1 and heat to dissolve it at 80°C. Filter and collect 1052 mL of the filtrate.
[0066] (3) The filtrate was loaded with 500 g of ADS-17 anion exchange resin column for decolorization, and the decolorized effluent was collected and dried under reduced pressure at -0.08 MPa and 50 °C to obtain 212 g of the dried effluent, i.e., Sample 2.
[0067] (4) Add 2.5 times the volume mass fraction of 70% ethanol solution to sample 2 and dissolve it in a glass container. Evaporate the solvent at 40°C and collect 132 g of dry solid in the glass container to obtain sample 3.
[0068] (5) Sample 3 was dissolved in 400 mL of pure water, filtered and poured into a preparative liquid chromatograph for gradient elution. The mobile phase was acetonitrile-water. The elution flow rate was 20 mL / min and the detection wavelength was 245 nm. The fraction flowing out from 2.0-3.0 min was collected and dried to obtain 95.3 g of high-purity quebracho alcohol crystals. The mobile phase elution gradient was carried out according to Example 1.
[0069] After testing, the purity of the quebracho alcohol prepared in this embodiment is 99.87%. After calculation, the transfer rate of quebracho alcohol extracted by the method of this embodiment is 95.18%.
[0070] Example 3
[0071] A method for extracting high-purity quebracho alcohol from seabuckthorn leaves comprises the following steps:
[0072] (1) The dried seabuckthorn leaves were crushed and passed through a 60-mesh sieve. 2000 g of the crushed seabuckthorn leaves were accurately weighed (the content of quebracho alcohol in the seabuckthorn leaves was 5% as determined by ultra-high performance liquid chromatography). The leaves were extracted with 8 times the volume mass fraction of 90% ethanol solution at 30°C for 3 times, each time for 2 h. The extract and the residue were collected, and the extract was concentrated under reduced pressure to 1 / 4 of the original volume to obtain 360 g of the sample.
[0073] (2) Then add 2 times the volume of pure water to sample 1 and heat it to dissolve at 70°C, filter it, and collect 720 mL of the filtrate;
[0074] (3) The filtrate was loaded with 300 g of ADS-17 anion exchange resin column for decolorization, and the decolorized effluent was collected and dried under reduced pressure at -0.08 MPa and 55 °C to obtain 215 g of the dried effluent, i.e., Sample 2.
[0075] (4) Add 2.0 times the volume mass fraction of 80% ethanol solution to sample 2 and dissolve it in a glass container. Evaporate the solvent at 35°C and collect 128 g of dry solid in the glass container to obtain sample 3.
[0076] (5) Sample 3 was dissolved in 395 mL of acetonitrile, filtered and poured into a preparative liquid chromatograph for gradient elution. The mobile phase was acetonitrile-water. The elution flow rate was 25 mL / min and the detection wavelength was 245 nm. The fractions eluting at 2.2-3.4 min were collected and dried to obtain 95.70 g of high-purity quebracho alcohol crystals. The mobile phase elution gradient was the same as that in Example 1.
[0077] After testing, the purity of the quebracho alcohol prepared in this embodiment is 99.74%. After calculation, the transfer rate of quebracho alcohol extracted by the method of this embodiment is 95.45%.
[0078] Example 4
[0079] A method for extracting high-purity quebracho alcohol from seabuckthorn leaves comprises the following steps:
[0080] (1) The dried seabuckthorn leaves were crushed and passed through a 30-mesh sieve. 2000 g of the crushed seabuckthorn leaves were accurately weighed (the content of quebracho alcohol in the seabuckthorn leaves was 5% as determined by ultra-high performance liquid chromatography). The seabuckthorn leaves were extracted with 10 times the volume of 80% ethanol solution at a temperature of 60°C. The extraction was repeated for 4 hours each time. The extract and the residue were collected and discarded. The extract was concentrated under reduced pressure to 1 / 4 of the original volume to obtain 350 g of the sample.
[0081] (2) Add 5 times the volume of pure water to sample 1 and heat it to dissolve at 60°C. Filter and collect 1746 mL of the filtrate.
[0082] (3) The filtrate was loaded with 500 g of ADS-17 anion exchange resin column for decolorization, and the decolorized effluent was collected and dried under reduced pressure at -0.1 MPa and 60 °C to obtain 215 g of the dried effluent, i.e., Sample 2.
[0083] (4) Add 5 times the volume mass fraction of 60% ethanol solution to sample 2 and dissolve it in a glass container. Evaporate the solvent at 50°C and collect 133 g of dry solid in the glass container to obtain sample 3.
[0084] (5) Sample 3 was dissolved in 280 mL of pure water, filtered and poured into a preparative liquid chromatograph for gradient elution. The mobile phase was acetonitrile-water. The elution flow rate was 15 mL / min and the detection wavelength was 245 nm. The fractions flowing out from 1.5 to 3.0 min were collected and dried to obtain 95.31 g of high-purity quebracho alcohol crystals. The mobile phase elution gradient was performed according to Example 1.
[0085] After testing, the purity of the quebracho alcohol prepared in this embodiment is 99.89%. After calculation, the transfer rate of extracting quebracho alcohol using the method of this embodiment is 95.21%.
[0086] Example 5
[0087] A method for extracting high-purity quebracho alcohol from seabuckthorn leaves comprises the following steps:
[0088] (1) The dried seabuckthorn leaves were crushed and passed through a 50-mesh sieve. 2000 g of the crushed seabuckthorn leaves were accurately weighed (the content of quebracho alcohol in the seabuckthorn leaves was 5% as determined by ultra-high performance liquid chromatography). The seabuckthorn leaves were extracted with 7.5 times the volume of a 70% ethanol solution at a mass fraction of 50°C. The extraction was repeated twice, each time for 1 h. The extract and the residue were collected and discarded. The extract was concentrated under reduced pressure to 1 / 5 of the original volume to obtain 354 g of the sample.
[0089] (2) Add 4 times the volume of pure water to sample 1 and heat to dissolve it at 90°C. Filter and collect 1412 mL of the filtrate.
[0090] (3) The filtrate was loaded with 400 g of ADS-17 anion exchange resin column for decolorization, and the decolorized effluent was collected and dried under reduced pressure at -0.1 MPa and 45 °C to obtain 214 g of the dried effluent, i.e., Sample 2.
[0091] (4) Add 1 volume mass fraction of 75% ethanol solution to sample 2 and dissolve it in a glass container. Evaporate the solvent at 20°C and collect 135 g of dry solid in the glass container to obtain sample 3.
[0092] (5) Sample 3 was dissolved in 405 mL of pure water, filtered and poured into a preparative liquid chromatograph for gradient elution. The mobile phase was acetonitrile-water. The elution flow rate was 10 mL / min and the detection wavelength was 245 nm. The fractions eluting at 1.7-3.2 min were collected and dried to obtain 95.72 g of high-purity quebracho alcohol crystals. The mobile phase elution gradient was performed according to Example 1.
[0093] After testing, the purity of the quebracho alcohol prepared in this embodiment is 99.68%. After calculation, the transfer rate of quebracho alcohol extracted by the method of this embodiment is 95.41%.
[0094] The above embodiments are only examples of the preferred embodiments of the present invention and do not include all the implementation scope of the invention. Various changes and modifications made by ordinary technicians in this field without departing from the spirit and scope of the present invention are considered to be within the scope of protection of the claims of the present invention.
Claims
1. A method for extracting high-purity quebracho alcohol from seabuckthorn leaves, characterized in that The steps include: (1) Extraction: the dried seabuckthorn leaves are crushed and sieved, dissolved and extracted with an ethanol solution, the extract and the filter residue are collected, and the extract is concentrated under reduced pressure to obtain sample 1; the seabuckthorn leaves are crushed and sieved with a 30-60 mesh sieve, the mass fraction of the ethanol solution is 60-95%, the mass volume ratio of the seabuckthorn leaves to the ethanol solution is 1-2:6-15, the number of extractions is 1-3, the extraction time for each extraction is 1-4 hours, and the extraction temperature is 10-60°C; (2) Water precipitation: add pure water to sample 1, heat to dissolve, filter, and collect the filtrate; the volume ratio of sample 1 to pure water is 1:2-5, and the dissolution temperature is 30-90°C; (3) Decolorization: the filtrate is passed through an ADS-17 anion exchange resin column, the decolorized load effluent is collected and dried under reduced pressure to obtain a dry load effluent, which is sample 2; the mass volume ratio of the ADS-17 anion exchange resin to the filtrate is 1:2-6, the pressure of the reduced pressure drying is -0.08-0.1MPa, and the temperature is 10-60°C; (4) Preliminary purification: dissolve sample 2 in a glass container using ethanol, evaporate the solvent at low temperature, and collect the dry solid in the glass container to obtain sample 3; (5) Purification: After dissolving and filtering the sample 3, pour it into a preparative liquid chromatograph for gradient elution, collect the fractions flowing out in a specific time period and dry them to obtain white quebracho alcohol crystals; the solvent used to dissolve the sample 3 is pure water or acetonitrile, and the mass volume ratio of the sample 3 to the solvent is 1:2-4; the mobile phase used in the preparative liquid chromatograph is acetonitrile-water, the elution flow rate is 10-30 mL / min, the detection wavelength is 245 nm, and the mobile phase elution gradient is as follows: ; The specific time period for collecting fractions was 1.5-4.0 min.
2. A method for extracting high-purity quebracho alcohol from seabuckthorn leaves according to claim 1, characterized in that: In the step (1), the extract is concentrated under reduced pressure to 1 / 5-1 / 4 of the original volume, which is sample 1.
3. A method for extracting high-purity quebracho alcohol from seabuckthorn leaves according to claim 1, characterized in that: In the step (4), the mass fraction of the ethanol solution is 60-80%, the mass volume ratio of the sample 2 to the ethanol solution is 1:1-5, and the solvent evaporation temperature is 20-50°C.
4. A method for extracting high-purity quebracho alcohol from seabuckthorn leaves according to claim 1, characterized in that: In the step (5), the collected fraction is dried to obtain high-purity quebracho alcohol crystals, the purity of which is ≥99.5%.
Citation Information
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