Vitamin E purification method

Abstract

The invention discloses a purification method of vitamin E, and relates to the technical field of bioengineering. Comprising the following steps: extracting a raw material vitamin E with a solvent 1, and filtering to obtain a filter cake; mixing the filter cake, a solvent 2 and silica gel to obtain a mixture; loading the mixture on a silica gel column, eluting with an eluent, and concentrating to obtain a vitamin E crude product; and mixing the vitamin E crude product with the solvent 3, heating, cooling, and taking a vitamin E layer to obtain the purified vitamin E. The vitamin E purification method is simpler and more convenient, the product purity is higher, the yield is higher, the process stability is high, and the repeatability is good.

Description

Technical Field

[0001] The invention relates to the technical field of bioengineering, and in particular to a method for purifying vitamin E, and further to a method for separating and purifying vitamin E from vitamin E powder. Background Art

[0002] Vitamin E (VE) is a fat-soluble vitamin and one of the most important antioxidants. Vitamin E can promote reproduction, promote the secretion of sex hormones, increase the vitality and quantity of sperm in men, increase the concentration of female hormones in women, improve fertility, and prevent miscarriage. At the same time, it delays aging, effectively reduces the formation of wrinkles, and maintains a youthful appearance. Vitamin E is a very important vasodilator and anticoagulant, which can be used to prevent and treat varicose veins, prevent blood coagulation, and reduce the formation of streaky tissue.

[0003] Other functions of vitamin E include: protecting T lymphocytes, protecting red blood cells, resisting free radical oxidation, inhibiting platelet aggregation, thereby reducing the risk of myocardial infarction and cerebral infarction. In addition, it also has a good effect on burns, frostbite, capillary bleeding, menopausal syndrome, and beauty.

[0004] Chinese patent CN105585552A discloses a decolorization and purification method of vitamin E, the method comprising the following steps: (a) providing a composite decolorizing agent to decolorize the vitamin E product; (b) eluting the decolorized vitamin E product obtained in step (a) with an eluent by column chromatography, and collecting the eluate fraction; (c) concentrating the eluate fraction obtained in step (b) to obtain decolorized and purified vitamin E, wherein, in step (a), the composite decolorizing agent is activated white clay: activated carbon: diatomaceous earth: magnesium silicate = 100: 50-100: 30-70: 10-50, by mass. The decolorization and purification method of vitamin E of the invention can not only make the color of vitamin E lighter, reduce viscosity, improve fluidity, but also improve the purity of vitamin E, and has less loss during the decolorization and purification process, and a high recovery rate of vitamin E.

[0005] Chinese patent CN102584769A discloses a method for preparing natural vitamin E with a content of more than 99%, using 40% natural VE, dissolving it in a certain proportion with 99% ethanol, cooling it to about 15°C, filtering to remove ethanol insolubles; then using secondary adsorption, first using macroporous adsorption resin to adsorb acidic impurities and pigments, etc., using anionic strong base resin to adsorb natural VE in the effluent, and then washing the anionic strong base resin with 99% ethanol to remove impurities such as methyl esters that are not adsorbed; then using a release agent to release VE, cooling the eluate to a certain temperature, filtering through micropores to remove ethanol insolubles; adding a specific remover to remove polycyclic aromatic hydrocarbons and adsorb other impurities, filtering to remove the remover, concentrating, desolventizing, and finally refining by three-stage molecular distillation to obtain the product. The content and purity of the product obtained by the invention can meet the quality requirements of EU countries and is a method for preparing natural vitamin E with a content of more than 99%.

[0006] At present, the purification of vitamin E is generally cumbersome and complex, and a simpler and more efficient purification process is needed. Summary of the invention

[0007] The purpose of the present invention is to provide a method for purifying vitamin E, which can separate and purify vitamin E from vitamin E powder, has high yield and high purity, and is simple to operate.

[0008] To achieve the above-mentioned purpose of the invention, the technical solution of the present invention is as follows:

[0009] A method for purifying vitamin E comprises the following steps:

[0010] (1) extracting the raw vitamin E with solvent 1 and filtering to obtain a filter cake;

[0011] (2) mixing the filter cake obtained in step (1), solvent 2, and silica gel to obtain a mixture;

[0012] (3) applying the mixture obtained in step (2) to a silica gel column, eluting with an eluent, and concentrating to obtain a crude vitamin E product;

[0013] (4) mixing the crude vitamin E obtained in step (3) with solvent 3, heating and cooling, taking the vitamin E layer, and obtaining purified vitamin E.

[0014] Wherein, the solvent 1, solvent 2 and solvent 3 are organic solvents, and the eluent is at least one of petroleum ether, ethyl acetate, dichloromethane and ethanol.

[0015] Preferably, the solvent 1 is at least one of methanol, petroleum ether, ethyl acetate, dichloromethane, ethanol, n-butanol and acetone, more preferably at least one of methanol, petroleum ether, ethyl acetate, dichloromethane and ethanol, and most preferably methanol.

[0016] Preferably, in step (1), the extraction conditions are: the ratio of solvent 1 to raw vitamin E is 4-10:1, L:kg, extraction is performed 1-3 times, each extraction time is 1-3 hours, and the extraction temperature is 40-80°C. More preferably, the ratio of solvent 1 to raw vitamin E is 5:1, L:kg, extraction is performed 2 times, each extraction time is 1 hour, and the extraction temperature is 50°C.

[0017] Preferably, in step (1), the filtering condition is: cooling to -10 to 10°C and filtering.

[0018] Preferably, the solvent 2 is at least one of petroleum ether, ethyl acetate, dichloromethane, ethanol, n-butanol and acetone; more preferably at least one of petroleum ether, ethyl acetate, dichloromethane and ethanol, and most preferably ethanol.

[0019] Preferably, in step (2), the mass ratio of the filter cake to silica gel is 1-2:1-2, more preferably 1:1.

[0020] Preferably, in step (2), the mesh size of the silica gel is 100-300 mesh, more preferably 200-300 mesh.

[0021] Preferably, in step (3), the mesh size of the silica gel is 100-300 mesh, more preferably 100-200 mesh.

[0022] Preferably, in step (3), the weight ratio of the amount of silica gel to the filter cake is 5-12:1, more preferably 8:1.

[0023] Preferably, the eluent is a mixed solvent of petroleum ether and ethyl acetate, further preferably, the volume ratio of petroleum ether to ethyl acetate is 1:3-10, further preferably 1:6.

[0024] Preferably, in step (3), the elution conditions are: flow rate 1-10V 柱体积 / h, elution volume is 1-5 times V 柱体积 , further preferably: flow rate 3V 柱体积 / h, elution volume 1.5-2 times V 柱体积 .

[0025] Preferably, in step (3), the concentration is concentration to constant weight.

[0026] Preferably, in step (3), the concentration temperature is 30-70°C, more preferably 50°C.

[0027] Preferably, the solvent 3 is an ethanol aqueous solution, more preferably an ethanol aqueous solution with a volume fraction of 70-90%, and more preferably an ethanol aqueous solution with a volume fraction of 80%.

[0028] Preferably, in step (4), the mass ratio of the solvent 3 to the crude vitamin E is 1-5:1, more preferably 3:1.

[0029] Preferably, in step (4), the heating temperature is 40-80°C, and the heating time is 0.5-2h. More preferably, the heating temperature is 60°C, and the heating time is 60min.

[0030] Preferably, in step (4), the cooling temperature is -10 to 10°C, more preferably 0°C.

[0031] Preferably, in step (4), the concentration temperature is 30-70°C, more preferably 60°C.

[0032] The beneficial effects of the present invention are:

[0033] The vitamin E purification method of the present invention is more simple, and by selecting the process and specific solvents and conditions, the obtained vitamin E product has higher purity, higher yield, high process stability and good repeatability. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 It is the chromatogram of vitamin E reference substance of the present invention.

[0035] Figure 2 This is a chromatogram of the vitamin E product after purification in Example 1 of the present invention. DETAILED DESCRIPTION

[0036] Terms and Claims of the Present Invention:

[0037] 1. The articles “a”, “an” and “the” include plural referents unless expressly limited to one or more referents otherwise.

[0038] 2. Numerical range: Unless otherwise expressly stated, all ranges or ratios disclosed herein will be understood to include any and all sub-ranges or sub-ratios contained therein. For example, a range or ratio of 1 to 30 stated should be considered to be included between a minimum value of 1 and a maximum value of 30, and any sub-range or sub-ratio, integer, decimal, or sub-range or sub-ratio consisting of integers or decimals including the end points.

[0039] The following non-limiting examples can enable those skilled in the art to more fully understand the present invention, but do not limit the present invention in any way. The following content is only an exemplary description of the scope of the present invention, and those skilled in the art can make various changes and modifications to the invention of the present invention based on the disclosed content, and they should also fall within the scope of the present application.

[0040] The present invention is further described below by way of specific examples. The various chemical reagents used in the examples of the present invention are obtained through conventional commercial channels unless otherwise specified. Unless otherwise specified, the contents described below are all weight contents. Unless otherwise specified, it is understood that the process is carried out at room temperature.

[0041] In the following examples, vitamin E powder was purchased from Zhengzhou Zhengyan Biotechnology Co., Ltd. with a product number of 202401112.

[0042] Example 1

[0043] (1) Weigh 10 kg of 50% pure vitamin E powder, extract twice with 50 L of methanol, each extraction temperature is 50° C., the extraction time is 1 hour, and the two extracts are combined; the extract is cooled to 5° C. and filtered to obtain a filter cake;

[0044] (2) 6.5 kg of the filter cake was obtained, dissolved in 6.5 L of ethanol, mixed with 6.5 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0045] (3) Weigh 52 kg of 100-200 mesh silica gel to pack the column, compact it, and elute it with a mixture of petroleum ether and ethyl acetate (volume ratio 1:6) at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 5.5 kg of crude vitamin E;

[0046] (4) The crude vitamin E product was mixed with 3 times the mass of 80% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 4.75 kg of vitamin E product.

[0047] Example 2

[0048] (1) Weigh 100 kg of 50% pure vitamin E powder, extract it twice with 500 L of methanol, each extraction temperature is 50° C., the extraction time is 1 hour, and the two extracts are combined; the extract is cooled to 5° C. and filtered to obtain a filter cake;

[0049] (2) 66.2 kg of the filter cake was obtained, dissolved in 65 L of ethanol, mixed with 66 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0050] (3) Weigh 530 kg of 100-200 mesh silica gel to pack the column, compact it, and elute it with a mixture of petroleum ether and ethyl acetate (volume ratio 1:6) at a flow rate of 1 V. 柱体积 / h, elution volume 2 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 54.8 kg of crude vitamin E;

[0051] (4) The crude vitamin E product was mixed with 1 times the mass of 80% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 47.6 kg of vitamin E product.

[0052] Example 3

[0053] (1) Weigh 500 kg of 50% pure vitamin E powder, extract it twice with 2500 L of methanol, each extraction temperature is 50° C., the extraction time is 1 hour, and the two extracts are combined; the extract is cooled to 5° C. and filtered to obtain a filter cake;

[0054] (2) 325 kg of the filter cake was obtained, dissolved in 325 L of ethanol, mixed with 325 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0055] (3) Weigh 2600 kg of 100-200 mesh silica gel and pack it into the column, compact it, and elute it with a mixture of petroleum ether and ethyl acetate (volume ratio 1:6) at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 276.5 kg of crude vitamin E;

[0056] (4) The crude vitamin E product was mixed with 5 times the mass of 80% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 235.5 kg of vitamin E product.

[0057] Example 4

[0058] (1) Weigh 10 kg of 50% pure vitamin E powder, extract twice with 50 L of methanol, each extraction temperature is 50° C., the extraction time is 1 hour, and the two extracts are combined; the extract is cooled to 5° C. and filtered to obtain a filter cake;

[0059] (2) 6.4 kg of the filter cake was obtained, dissolved in 6.4 L of dichloromethane, mixed with 6.4 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0060] (3) Weigh 51.2 kg of 100-200 mesh silica gel to pack the column, compact it, and elute it with a mixture of petroleum ether and ethyl acetate (volume ratio 1:6) at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 5.8 kg of crude vitamin E;

[0061] (4) The crude vitamin E product was mixed with 3 times the mass of 70% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 4.53 kg of vitamin E product.

[0062] Example 5

[0063] (1) Weigh 10 kg of 50% pure vitamin E powder, extract twice with 50 L of ethyl acetate, each extraction temperature is 50° C., the extraction time is 1 hour, and the two extracts are combined; the extract is cooled to 5° C. and filtered to obtain a filter cake;

[0064] (2) 7.1 kg of the filter cake was obtained, dissolved in 7.1 L of petroleum ether, mixed with 7.1 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0065] (3) Weigh 56.8 kg of 100-200 mesh silica gel to pack the column, compact it, and elute it with a mixture of petroleum ether and ethyl acetate (volume ratio 1:10) at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 5.1 kg of crude vitamin E;

[0066] (4) The crude vitamin E product was mixed with 3 times the mass of 70% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 4.67 kg of vitamin E product.

[0067] Comparative Example 1

[0068] (1) Weigh 10 kg of 50% pure vitamin E powder, extract it once with 50 L of methanol, each extraction temperature is 30° C., the extraction time is 1 hour, the extract is cooled at 5° C., and filtered to obtain a filter cake;

[0069] (2) 4.5 kg of the filter cake was obtained, dissolved in 4.5 L of methanol, mixed with 4.5 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0070] (3) Weigh 36 kg of 100-200 mesh silica gel to pack the column, compact it, and elute it with a mixture of petroleum ether and ethyl acetate (volume ratio 1:6) at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 3.5 kg of crude vitamin E;

[0071] (4) The crude vitamin E product was mixed with 3 times the mass of 80% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 2.8 kg of vitamin E product.

[0072] Comparative Example 2

[0073] (1) Weigh 10 kg of 50% pure vitamin E powder, extract it with 50 L of methanol for 5 times, each extraction temperature is 40° C., the extraction time is 0.5 hour, the two extracts are combined, the extract is cooled at 5° C., and filtered to obtain a filter cake;

[0074] (2) 6.5 kg of the filter cake was obtained, dissolved in 6.5 L of ethanol, mixed with 6.5 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0075] (3) Weigh 20 kg of 100-200 mesh silica gel to pack the column, compact it, and elute it with a mixture of petroleum ether and ethyl acetate (volume ratio 1:6) at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 3.5 kg of crude vitamin E;

[0076] (4) The crude vitamin E product was mixed with 3 times the mass of 80% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 3.42 kg of vitamin E product.

[0077] Comparative Example 3

[0078] (1) Weigh 10 kg of 50% pure vitamin E powder, extract twice with 50 L of n-butanol, each extraction temperature is 50° C., the extraction time is 1 hour, and the two extracts are combined; the extract is cooled to 5° C. and filtered to obtain a filter cake;

[0079] (2) 5.5 kg of the filter cake was obtained, dissolved in 5.5 L of ethanol, mixed with 5.5 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0080] (3) Weigh 44 kg of 100-200 mesh silica gel to pack the column, compact it, and elute it with a mixture of petroleum ether and ethyl acetate (volume ratio 1:6) at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 4.5 kg of crude vitamin E;

[0081] (4) The crude vitamin E product was mixed with 60% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 3.95 kg of vitamin E product.

[0082] Comparative Example 4

[0083] (1) Weigh 10 kg of 50% pure vitamin E powder, extract twice with 50 L of methanol, each extraction temperature is 50° C., the extraction time is 1 hour, and the two extracts are combined; the extract is cooled to 5° C. and filtered to obtain a filter cake;

[0084] (2) 6.5 kg of the filter cake was obtained, dissolved in 6.5 L of ethanol, mixed with 6.5 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0085] (3) Weigh 52 kg of 100-200 mesh silica gel to pack the column, compact it, and elute it with a mixture of petroleum ether and ethanol in a volume ratio of 1:6 at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 4.6 kg of crude vitamin E;

[0086] (4) The crude vitamin E product was mixed with 80% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 4.05 kg of vitamin E product.

[0087] Comparative Example 5

[0088] (1) Weigh 10 kg of vitamin E powder with a purity of 50%, extract it twice with 30 L of methanol, each time at a temperature of 50° C. for 1 hour, and combine the two extracts; cool the extract to 5° C. and filter to obtain a filter cake;

[0089] (2) 4.5 kg of the filter cake was obtained, dissolved in 4.5 L of ethanol, mixed with 4.5 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0090] (3) Weigh 36 kg of 100-200 mesh silica gel to pack the column, compact it, and elute it with a mixture of petroleum ether and ethyl acetate (volume ratio 1:6) at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 2.9 kg of crude vitamin E;

[0091] (4) The crude vitamin E product was mixed with 80% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 1.75 kg of vitamin E product.

[0092] Comparative Example 6

[0093] (1) Weigh 10 kg of vitamin E powder with a purity of 50%, extract it twice with 50 L of ethanol, each time at a temperature of 50° C. for 1 hour, and combine the two extracts; cool the extract at 5° C. and filter to obtain a filter cake;

[0094] (2) 5.6 kg of the filter cake was obtained, dissolved in 5.6 L of methanol, mixed with 5.6 kg of 200-300 mesh silica gel, and stirred to obtain a mixture;

[0095] (3) Weigh 44.8 kg of 100-200 mesh silica gel to fill the column, compact it, and elute it with a mixture of petroleum ether and methanol (volume ratio 1:6) at a flow rate of 3 V. 柱体积 / h, elution volume 1.5 times V 柱体积 , collect the eluate containing vitamin E, concentrate at 50°C, and obtain 4.5 kg of crude vitamin E;

[0096] (4) The crude vitamin E product was mixed with 80% ethanol, heated at 60°C for 60 min, cooled to 0°C, separated into the vitamin E layer, and then concentrated at 60°C to obtain 3.25 kg of vitamin E product.

[0097] Results

[0098] Determined according to high performance liquid chromatography (General Rule 0512);

[0099] Chromatographic conditions and system suitability test:

[0100] Column: C18 5μm 150x 4.6mm;

[0101] Chromatographic conditions:

[0102] Mobile phase: methanol-water (volume ratio 98:2);

[0103] Flow rate: 1 mL / min;

[0104] Injection volume: 20 μL;

[0105] Column temperature: 25°C;

[0106] The number of theoretical plates calculated based on peaks should not be less than 2000.

[0107] Preparation of reference solution: Accurately weigh an appropriate amount of vitamin E reference substance and add methanol to make a solution containing 0.1 mg per 1 mL.

[0108] Preparation of test solution: Take 2 portions of vitamin E prepared in each of the above examples and comparative examples (precisely weighed, placed in a stoppered conical flask, accurately add 10 mL of methanol, weigh the weight, ultrasonically treat (power 250 W, frequency 25 kHz) for 15 minutes, cool, weigh again, make up the lost weight with methanol, shake well, filter, and obtain;

[0109] Determination method: Accurately pipette 10 μL of reference solution and test solution respectively, inject into liquid chromatograph, and determine.

[0110] The content test results and vitamin E yield results are shown in Table 1 below:

[0111] Table 1

[0112] Sample name content Quality product rate Example 1 99.1％ 95.0％ Example 2 99.5％ 95.2％ Example 3 99.2％ 94.2％ Example 4 99.1％ 90.6％ Example 5 98.9％ 93.4％ Comparative Example 1 98.9％ 56.0％ Comparative Example 2 99.1％ 68.4％ Comparative Example 3 98.12％ 79.5％ Comparative Example 4 97.25％ 81.0％ Comparative Example 5 98.53％ 35.0％ Comparative Example 6 99.12％ 65.0％

[0113] The results show that the determination results are relatively stable, the vitamin E product of the embodiment has high purity, high yield of vitamin E product, high process stability and good repeatability. Comparative Examples 1 and 2 show that the extraction conditions and the amount of silica gel used will significantly affect the yield of fine products. Comparative Examples 3, 4 and 6 show that the types of solvent and eluent have a great influence on purity and yield. Comparative Example 5 verifies that when the amount of solvent used in step (1) is reduced, the yield will decrease significantly.

[0114] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to specific details.

Claims

1. A method for purifying vitamin E, characterized in that: The following steps are involved: (1) extracting the raw vitamin E with solvent 1 and filtering to obtain a filter cake; (2) mixing the filter cake obtained in step (1), solvent 2, and silica gel to obtain a mixture; (3) applying the mixture obtained in step (2) to a silica gel column, eluting with an eluent, and concentrating to obtain a crude vitamin E product; (4) mixing the crude vitamin E obtained in step (3) with solvent 3, heating and cooling, taking the vitamin E layer, and obtaining purified vitamin E. Wherein, the solvent 1, solvent 2 and solvent 3 are organic solvents, and the eluent is at least one of petroleum ether, ethyl acetate, dichloromethane and ethanol.

2. The purification method according to claim 1, characterized in that The solvent 1 is at least one of methanol, petroleum ether, ethyl acetate, dichloromethane and ethanol.

3. The purification method according to claim 2, characterized in that The solvent 1 is methanol.

4. The purification method according to claim 1, characterized in that In step (1), the extraction conditions are: the ratio of the amount of the solubilizer to the vitamin is 4-10, L:kg, extraction is performed 1-3 times, each extraction time is 1-3 hours, the extraction temperature is 40-80°C, and the extraction is cooled to -10 to 10°C and filtered.

5. The purification method according to claim 1, characterized in that The solvent 2 is at least one of petroleum ether, ethyl acetate, dichloromethane and ethanol.

6. The purification method according to claim 1, characterized in that In step (2), the mass ratio of the filter cake to the silica gel is 1-2:1-2.

7. The purification method according to claim 1, characterized in that In step (2), the mesh size of the silica gel is 100-300 meshes; in step (3), the mesh size of the silica gel is 100-300 meshes, and the weight ratio of the amount of silica gel to the filter cake is 5-12:

1.

8. The purification method according to claim 1, characterized in that The volume ratio of petroleum ether to ethyl acetate is 1:3-10.

9. The purification method according to claim 1, characterized in that In step (3), the elution conditions are: flow rate 1-10V 柱体积 / h, elution volume is 1-5 times V 柱体积 .

10. The purification method according to claim 1, characterized in that: The solvent 3 is an ethanol aqueous solution with a volume fraction of 70-90%.

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