Method for extracting 8-hydroxy dictamnine from cortex dictamni

Abstract

The invention provides a method for extracting 8-hydroxy dictamnine from cortex dictamni, and relates to the technical field of preparation of 8-hydroxy dictamnine. The preparation method comprises the following steps: cleaning and drying cortex dictamni, crushing and sieving to obtain cortex dictamni powder for later use; then putting the cortex dictamni powder into an ethanol / glacial acetic acid mixed solution for heating reflux, and filtering to obtain an extracting solution; extracting the extracting solution for multiple times by using an ethyl acetate / n-butyl alcohol mixed solution, and combining the extracting solutions; carrying out reduced pressure distillation on the extract liquor, and obtaining a crude extract after drying by distillation; and finally, recrystallizing the crude extract by using acetone to obtain the 8-hydroxy dictamnine. According to the method, the crude product does not need to be separated and purified by adopting column chromatography, so that the operation difficulty and the cost are reduced, and meanwhile, the time for separating and purifying the 8-hydroxy dictamnine is greatly shortened.

Description

Technical Field

[0001] The invention relates to the field of 8-hydroxydactyline preparation, in particular to a method for extracting 8-hydroxydactyline from Dactyline cortex. Background Art

[0002] Dictamni is a traditional Chinese medicine with the effects of clearing away heat and dampness, dispelling wind and detoxifying. Current research shows that Dictamni has the effects of anti-cancer, anti-gastric ulcer, antibacterial and improving human immunity.

[0003] The chemical components of Dictamni peel mainly include alkaloids, lactones, flavonoids, limonoids, polysaccharides, sesquiterpenes and their glycosides. 8-Hydroxydictamni is an important alkaloid in Dictamni peel. Currently, there are few reports on the methods of extracting and isolating high-purity 8-hydroxydictamni from Dictamni peel. Summary of the invention

[0004] In view of this, the present invention provides a method for extracting 8-hydroxydactyline from Dictamni cortex.

[0005] The present invention is achieved by adopting the following technical solutions:

[0006] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0007] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain the Dictamni cortex powder for standby use;

[0008] (2) placing the Dictamni cortex powder in an ethanol / glacial acetic acid mixture for heating and refluxing, and filtering to obtain an extract;

[0009] (3) extracting the extract multiple times with an ethyl acetate / n-butanol mixture, and combining the extracts;

[0010] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0011] (5) Recrystallizing the crude extract using acetone to obtain 8-hydroxydandruff.

[0012] Preferably, the particle size of the Dictamni cortex powder in step (1) is 200-300 mesh.

[0013] Preferably, the volume ratio of ethanol to glacial acetic acid in the ethanol / glacial acetic acid mixture in step (2) is 3 to 5:1.

[0014] Preferably, in step (2), the solid-to-liquid ratio of the Dictamni cortex powder to the ethanol / glacial acetic acid mixture is 1 g: (15-30) mL.

[0015] Preferably, the heating reflux time in step (2) is 2 h to 5 h.

[0016] Preferably, the volume ratio of ethyl acetate to n-butanol in the ethyl acetate / n-butanol mixture in step (3) is 1-2:1-2.

[0017] Compared with the prior art, the present invention has the following beneficial effects: the present invention provides a method for extracting 8-hydroxy-ducamine from Dictamni cortex, specifically, firstly extracting Dictamni cortex powder with ethanol / glacial acetic acid mixed solution to obtain an extract, then extracting the extract with ethyl acetate / n-butanol mixed solution, and finally evaporating the extract to dry the solvent and recrystallizing, thereby obtaining high-purity 8-hydroxy-ducamine. The present invention does not need to use column chromatography to separate and purify the crude product, reduces the difficulty and cost of operation, and greatly shortens the time for separating and purifying 8-hydroxy-ducamine. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 is the structural formula of 8-hydroxydandruff;

[0019] Figure 2 The present invention is a flowchart of the 8-hydroxy dioscorea alkali extraction process. DETAILED DESCRIPTION

[0020] The present invention will be further described below in conjunction with the embodiments.

[0021] Example 1

[0022] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0023] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain 200 purpose Dictamni cortex powder, for subsequent use;

[0024] (2) placing the Dictamni cortex powder in a 4:1 volume ratio ethanol / glacial acetic acid mixture, wherein the solid-liquid ratio is 1 g:25 mL, heating and refluxing for 3 h, and filtering to obtain an extract;

[0025] (3) extracting the extract three times with a mixture of ethyl acetate and n-butanol in a volume ratio of 2:1, and combining the extracts;

[0026] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0027] (5) The crude extract is recrystallized using acetone to obtain a solid product.

[0028] Example 2

[0029] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0030] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain the Dictamni cortex powder of 300 purposes, for subsequent use;

[0031] (2) placing the Dictamni cortex powder in a 3:1 volume ratio ethanol / glacial acetic acid mixture, wherein the solid-liquid ratio is 1 g:30 mL, heating and refluxing for 2.5 h, and filtering to obtain an extract;

[0032] (3) extracting the extract three times with a mixture of ethyl acetate and n-butanol in a volume ratio of 1:1, and combining the extracts;

[0033] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0034] (5) The crude extract is recrystallized using acetone to obtain a solid product.

[0035] Example 3

[0036] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0037] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain 200 purpose Dictamni cortex powder, for subsequent use;

[0038] (2) placing the Dictamni cortex powder in a mixed solution of ethanol / glacial acetic acid with a volume ratio of 5:1, wherein the solid-liquid ratio is 1 g:25 mL, heating and refluxing for 5 h, and filtering to obtain an extract;

[0039] (3) extracting the extract three times with a mixture of ethyl acetate and n-butanol in a volume ratio of 1:1.5, and combining the extracts;

[0040] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0041] (5) The crude extract is recrystallized using acetone to obtain a solid product.

[0042] Example 4

[0043] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0044] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain 200 purpose Dictamni cortex powder, for subsequent use;

[0045] (2) placing the Dictamni cortex powder in a 3:1 volume ratio ethanol / glacial acetic acid mixture, wherein the solid-liquid ratio is 1 g:25 mL, heating and refluxing for 4 h, and filtering to obtain an extract;

[0046] (3) extracting the extract three times with a mixture of ethyl acetate and n-butanol in a volume ratio of 1:2, and combining the extracts;

[0047] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0048] (5) The crude extract is recrystallized using acetone to obtain a solid product.

[0049] Example 5

[0050] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0051] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain the Dictamni cortex powder of 300 purposes, for subsequent use;

[0052] (2) placing the Dictamni cortex powder in a mixed solution of ethanol / glacial acetic acid with a volume ratio of 3.5:1, wherein the solid-liquid ratio is 1 g:25 mL, heating and refluxing for 4.5 h, and filtering to obtain an extract;

[0053] (3) extracting the extract three times with a mixture of ethyl acetate and n-butanol in a volume ratio of 1:2, and combining the extracts;

[0054] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0055] (5) The crude extract is recrystallized using acetone to obtain a solid product.

[0056] Example 6

[0057] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0058] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain the Dictamni cortex powder of 300 purposes, for subsequent use;

[0059] (2) placing the Dictamni cortex powder in a mixed solution of ethanol / glacial acetic acid with a volume ratio of 5:1 and a solid-liquid ratio of 1 g:25 mL, heating and refluxing for 3 h, and filtering to obtain an extract;

[0060] (3) extracting the extract multiple times with a mixture of ethyl acetate and n-butanol in a volume ratio of 1.5:1, and combining the extracts;

[0061] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0062] (5) The crude extract is recrystallized using acetone to obtain a solid product.

[0063] Comparative Example 1

[0064] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0065] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain 200 purpose Dictamni cortex powder, for subsequent use;

[0066] (2) placing the Dictamni cortex powder in a 4:1 volume ratio ethanol / glacial acetic acid mixture, wherein the solid-liquid ratio is 1 g:25 mL, heating and refluxing for 3 h, and filtering to obtain an extract;

[0067] (3) extracting the extract three times with ethyl acetate and combining the extracts;

[0068] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0069] (5) The crude extract is recrystallized using acetone to obtain a solid product.

[0070] Comparative Example 2

[0071] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0072] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain 200 purpose Dictamni cortex powder, for subsequent use;

[0073] (2) placing the Dictamni cortex powder in a 1:1 volume ratio ethanol / glacial acetic acid mixture, wherein the solid-liquid ratio is 1 g:25 mL, heating and refluxing for 3 h, and filtering to obtain an extract;

[0074] (3) extracting the extract three times with n-butanol and combining the extracts;

[0075] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0076] (5) The crude extract is recrystallized using acetone to obtain a solid product.

[0077] Comparative Example 3

[0078] A method for extracting 8-hydroxydactyline from Dictamni cortex comprises the following steps:

[0079] (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain 200 purpose Dictamni cortex powder, for subsequent use;

[0080] (2) placing the Dictamni cortex powder in ethanol at a solid-liquid ratio of 1 g:25 mL, heating and refluxing for 3 h, and filtering to obtain an extract;

[0081] (3) extracting the extract three times with ethyl acetate and combining the extracts;

[0082] (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness;

[0083] (5) The crude extract is recrystallized using acetone to obtain a solid product.

[0084] The solid products prepared in Examples 1-6 and Comparative Examples 1-3 were tested, and the extraction rate and purity of 8-hydroxydandruff were shown in Table 1, respectively.

[0085] Table 1

[0086] 8-Hydroxydistillate extraction rate 8-Hydroxydistillate purity Example 1 95.4％ 99.8％ Example 2 96.1％ 99.5％ Example 3 95.7％ 99.7％ Example 4 95.5％ 99.3％ Example 5 96.9％ 99.8％ Example 6 96.0％ 99.9％ Comparative Example 1 89.0％ 73.5％ Comparative Example 2 85.4％ 68.3％ Comparative Example 3 58.5％ 55.8％

[0087] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for extracting 8-hydroxydactyline from Dictamni cortex, characterized in that: The following steps are involved: (1) the Dictamni cortex is cleaned and dried, and then pulverized and sieved to obtain the Dictamni cortex powder for standby use; (2) placing the Dictamni cortex powder in an ethanol / glacial acetic acid mixture for heating and refluxing, and filtering to obtain an extract; (3) extracting the extract multiple times with an ethyl acetate / n-butanol mixture, and combining the extracts; (4) distilling the extract under reduced pressure to obtain a crude extract after evaporating to dryness; (5) Recrystallizing the crude extract using acetone to obtain 8-hydroxydandruff.

2. A method for extracting 8-hydroxydactyline from Dictamni cortex as claimed in claim 1, characterized in that: The particle size of the Dictamni cortex powder in step (1) is 200-300 meshes.

3. A method for extracting 8-hydroxydactyline from Dictamni cortex as claimed in claim 1, characterized in that: The volume ratio of ethanol to glacial acetic acid in the ethanol / glacial acetic acid mixture in step (2) is 3 to 5:

1.

4. A method for extracting 8-hydroxydactyline from Dictamni cortex as claimed in claim 1, characterized in that: The solid-to-liquid ratio of the Dictamni cortex powder to the ethanol / glacial acetic acid mixed solution in step (2) is 1 g: (15-30) mL.

5. A method for extracting 8-hydroxydactyline from Dictamni cortex as claimed in claim 1, characterized in that: The heating reflux time in step (2) is 2h to 5h.

6. A method for extracting 8-hydroxydactyline from Dictamni cortex as claimed in claim 1, characterized in that: The volume ratio of ethyl acetate to n-butanol in the ethyl acetate / n-butanol mixture in step (3) is 1-2:1-2.

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