CN104672071A - Method for rapid separation and purification of gossypol by using macroporous resin - Google Patents
Method for rapid separation and purification of gossypol by using macroporous resin Download PDFInfo
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- CN104672071A CN104672071A CN201310605604.4A CN201310605604A CN104672071A CN 104672071 A CN104672071 A CN 104672071A CN 201310605604 A CN201310605604 A CN 201310605604A CN 104672071 A CN104672071 A CN 104672071A
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- gossypol
- macroporous resin
- concentration
- ethanol
- purifying
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
Abstract
The invention discloses a method for rapid separation and purification of gossypol by using macroporous resin, and belongs to the field of chemistry. The method includes the steps of crushing, extracting, filtering, resin loading and separating, elution and concentrating crystallization. The method has the advantages of simple process, low cost, high efficiency and environmental protection, allows the adsorption resin to be easy to regenerate and use, and is suitable for industrialized production of gossypol products; an 80% ethanol has relatively good solulbility on gossypol, and is suitably used as an extraction solvent and a chromatography elution solvent; and with adopting of the macroporous resin, gossypol can be effectively enriched, and gossypol with relatively high purity can be obtained after recrystallization.
Description
Technical field
The present invention relates to a kind of method of separation and purification gossypol, particularly a kind of method using macroporous resin fast separating and purifying gossypol, belongs to chemical field.
Background technology
Gossypol (gossypol) is Malvaceae plant cotton, tree cotton or upland cotton mature seed, a kind of polyatomic phenol material of extracting in root skin.There is multiple pharmacological effect, as the restraining effect to hormone receptor, to the restraining effect of hormone sensitive lipase gene enzyme, to the restraining effect that endometrial cell DNA synthesizes, also to ovarian hormone, there is certain regulating effect, to the therapeutic action of former secondary dysmenorrhea, inhibition tumor cell growth etc.In addition, the effect of the generation of gossypol Inhibit sperm and sperm motility, can be used as a kind of effective male contraceptive agent.Extract the method preparing gossypol a lot, mainly contain single solvent lixiviation process, mixed solvent lixiviation process etc.The preparation of current gossypol mainly with cotton seed or cottonseed meal for raw material, take solvent extraction, as Acetone-Benzene amine method, acetone-acid system, ethanol-petroleum naphtha-aniline process etc.These extracting method have obvious deficiency, low if any the organic solvent boiling point used, consumption is large, poisonous, inflammable etc.In order to set up efficient a, environmental protection, the method preparation of safety has the gossypol of higher pharmaceutical use, and we have employed macroporous adsorbent resin and carry out enrichment as parting material to extracting solution.
Summary of the invention
The object of the present invention is to provide a kind of method using macroporous resin fast separating and purifying gossypol.
A kind of method using macroporous resin fast separating and purifying gossypol provided by the present invention, comprises the following steps:
A () is by cottonseed meal flour shape;
(b) adopt concentration be 80% ethanolic soln filter after 50 DEG C of-70 DEG C of lixiviates;
C filtrate is added water by () to be diluted to alcohol concn be 40%;
The upper macroporous resin of (d) filtrate, the weight consumption of macroporous resin is 1-2 times of cottonseed meal weight, take water as solvent-loaded column;
E () first carries out wash-out with the ethanol of 40% concentration, after with 80% concentration ethanol wash-out, collect elutriant;
F elutriant concentrating under reduced pressure is recycled to without ethanol by (), add acetone-Glacial acetic acid mixed solution and carry out recrystallization and obtain high-purity gossypol.Further, adopt in step (b) concentration be 80% ethanolic soln 50 DEG C-70 DEG C lixiviate steps be: the concentration first adding cottonseed meal 15 times of weight be 80% aqueous ethanolic solution filtered after 50 DEG C-70 DEG C lixiviate 2-4 hours, the concentration adding filter residue weight twice in filter residue is the aqueous ethanolic solution washing filter residue of 80%, the alcohol concn adding gained filter residue weight 7 times is again that the aqueous ethanolic solution of 80% was 50 DEG C-70 DEG C lixiviate filter residues 2 hours, after filtering, filtrate merges, further, first wash-out 4BV is carried out with the ethanol of 40% concentration in step (e), after with 80% concentration ethanol wash-out 5BV, further, in step (f), the mixing quality of acetone-Glacial acetic acid mixed solution is than being 1:1, further, ethanol or acetone repetitive scrubbing when described macroporous resin is reused, until water met by washings muddiness does not occur.
Advantageous Effects of the present invention is: present method technique is simple, cost is low, high-efficiency environment friendly, polymeric adsorbent easily regenerates use, be applicable to suitability for industrialized production gossypol product, 80% ethanol has good solubility property to gossypol, as Extraction solvent and chromatographic elution solvent all more suitable, adopt macroporous resin can effective enrichment gossypol, the gossypol of higher degree after recrystallization, can be obtained.
Embodiment
In order to better understand and implement technical scheme of the present invention, provide some embodiments of the present invention at this, these embodiments, in order to better explain technical solutions according to the invention, are not formed any form restriction of the present invention.Macroporous resin of the present invention adopts the macroporous resin column of H103, and ethanolic soln of the present invention is aqueous ethanolic solution, and the amount in following examples refers to weight.
Use the method for macroporous resin fast separating and purifying gossypol, comprise the following steps:
A () is by cottonseed meal flour shape;
(b) adopt concentration be 80% ethanolic soln filter after 50 DEG C of-70 DEG C of lixiviates;
C filtrate is added water by () to be diluted to alcohol concn be 40%;
The upper macroporous resin of (d) filtrate, the weight consumption of macroporous resin is 1-2 times of cottonseed meal weight, take water as solvent-loaded column;
E () first carries out wash-out with the ethanol of 40% concentration, after with 80% concentration ethanol wash-out, collect elutriant;
F elutriant concentrating under reduced pressure is recycled to without ethanol by (), add acetone-Glacial acetic acid mixed solution and carry out recrystallization and obtain high-purity gossypol.Further, adopt in step (b) concentration be 80% ethanolic soln 50 DEG C-70 DEG C lixiviate steps be: the concentration first adding cottonseed meal 15 times of weight be 80% aqueous ethanolic solution filtered after 50 DEG C-70 DEG C lixiviate 2-4 hours, the concentration adding filter residue weight twice in filter residue is the aqueous ethanolic solution washing filter residue of 80%, the alcohol concn adding gained filter residue weight 7 times is again that the aqueous ethanolic solution of 80% was 50 DEG C-70 DEG C lixiviate filter residues 2 hours, after filtering, filtrate merges, further, first wash-out 4BV is carried out with the ethanol of 40% concentration in step (e), after with 80% concentration ethanol wash-out 5BV, further, in step (f), the mixing quality of acetone-Glacial acetic acid mixed solution is than being 1:1, further, ethanol or acetone repetitive scrubbing when described macroporous resin is reused, until water met by washings muddiness does not occur.
Embodiment 1:
1.50g cotton seed 80% ethanol water of 15 times amount soaks in 60 DEG C and stirs extraction 3h, filters, then uses 80% ethanol water washing filter residue of 2 times amount;
2.7 times amount 80% ethanol water soak in 60 DEG C and stir the filter residue 2h of extraction step 1, filter, then use 80% ethanol water washing filter residue of 2 times amount;
3. merging filtrate, the water adding 2 times amount is diluted to the solution that alcohol concn encloses 40%;
4. the macroporous resin column of the upper H103 of filtrate, the consumption of macroporous resin is 1.5 times of cotton seed meal weight;
5. first use the ethanol water elution 4BV of 40%, then use the ethanol elution 5BV of 80%;
6. be evaporated to without ethanol by elutriant at lower than the temperature of 60 DEG C, the acetone-Glacial acetic acid adding 1:1 dissolves and carries out Gossypol Recrystallized.
Macroporous resin column is with 95% ethanol elution 3BV, and then 40% ethanol elution 5BV can reuse.
Embodiment 2:
1.200g cotton seed 80% ethanol water of 15 times amount soaks in 60 DEG C and stirs extraction 3h, filters, then uses 80% ethanol water washing filter residue of 2 times amount;
2.7 times amount 80% ethanol water soak in 60 DEG C and stir the filter residue 2h of extraction step 1, filter, then use 80% ethanol water washing filter residue of 2 times amount;
3. merging filtrate, the water adding 2 times amount is diluted to the solution that alcohol concn encloses 40%;
4. the macroporous resin column of the upper H103 of filtrate, the consumption of macroporous resin is 2 times of cotton seed meal weight;
5. first use the ethanol water elution 4BV of 40%, then use the ethanol elution 5BV of 80%;
6. be evaporated to without ethanol by elutriant at lower than the temperature of 60 DEG C, the acetone-Glacial acetic acid dissolving adding 1:1 is carried out recrystallization and is obtained highly purified gossypol product.
Macroporous resin column is with 95% ethanol elution 3BV, and then 40% ethanol elution 5BV can reuse.
After describing various specific embodiment of the present invention above in detail, those of ordinary skill in the art should be well understood to, according to the various common practise of this area, can carry out various equivalent variations, equivalent replacement according to thinking of the present invention or simply revise, these all should belong to the scope of technical solution of the present invention.
Claims (5)
1. use the method for macroporous resin fast separating and purifying gossypol, it is characterized in that: comprise the following steps:
A () is by cottonseed meal flour shape;
(b) adopt concentration be 80% ethanolic soln filter after 50 DEG C of-70 DEG C of lixiviates;
C filtrate is added water by () to be diluted to alcohol concn be 40%;
The upper macroporous resin of (d) filtrate, the weight consumption of macroporous resin is 1-2 times of cottonseed meal weight, take water as solvent-loaded column;
E () first carries out wash-out with the ethanol of 40% concentration, after with 80% concentration ethanol wash-out, collect elutriant;
F elutriant concentrating under reduced pressure is recycled to without ethanol by (), add acetone-Glacial acetic acid mixed solution and carry out recrystallization and obtain high-purity gossypol.
2. the method for use macroporous resin fast separating and purifying gossypol according to claim 1, it is characterized in that: adopt in step (b) concentration be 80% ethanolic soln 50 DEG C-70 DEG C lixiviate steps be: the concentration first adding cottonseed meal 15 times of weight be 80% aqueous ethanolic solution filtered after 50 DEG C-70 DEG C lixiviate 2-4 hours, the concentration adding filter residue weight twice in filter residue is the aqueous ethanolic solution washing filter residue of 80%, the alcohol concn adding gained filter residue weight 7 times be again the aqueous ethanolic solution of 80% 50 DEG C-70 DEG C lixiviate filter residues 2 hours, after filtering, filtrate merges.
3. the method for use macroporous resin fast separating and purifying gossypol according to claim 1, is characterized in that: first carries out wash-out 4BV with the ethanol of 40% concentration in step (e), after with 80% concentration ethanol wash-out 5BV.
4. the method for use macroporous resin fast separating and purifying gossypol according to claim 1, is characterized in that: in step (f), the mixing quality of acetone-Glacial acetic acid mixed solution is than being 1:1.
5. the method for use macroporous resin fast separating and purifying gossypol according to claim 1, is characterized in that: ethanol or acetone repetitive scrubbing when described macroporous resin is reused, until water met by washings muddiness does not occur.
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| CN201310605604.4A CN104672071A (en) | 2013-11-26 | 2013-11-26 | Method for rapid separation and purification of gossypol by using macroporous resin |
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| CN201310605604.4A CN104672071A (en) | 2013-11-26 | 2013-11-26 | Method for rapid separation and purification of gossypol by using macroporous resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106363733A (en) * | 2016-09-29 | 2017-02-01 | 阜南县星光工艺品有限公司 | Green mould-proof insecticide for wood materials |
| CN106928042A (en) * | 2017-04-14 | 2017-07-07 | 华中农业大学 | A kind of method of Solid phase extraction separation gossypol in solution from gossypol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1966483A (en) * | 2006-11-03 | 2007-05-23 | 暨南大学 | Production process of medicinal gossypol acetic acid |
| CN101139269A (en) * | 2007-08-30 | 2008-03-12 | 季萍 | Method for producing male contraceptive raw material medicine-gossypol acetate |
-
2013
- 2013-11-26 CN CN201310605604.4A patent/CN104672071A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1966483A (en) * | 2006-11-03 | 2007-05-23 | 暨南大学 | Production process of medicinal gossypol acetic acid |
| CN101139269A (en) * | 2007-08-30 | 2008-03-12 | 季萍 | Method for producing male contraceptive raw material medicine-gossypol acetate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106363733A (en) * | 2016-09-29 | 2017-02-01 | 阜南县星光工艺品有限公司 | Green mould-proof insecticide for wood materials |
| CN106928042A (en) * | 2017-04-14 | 2017-07-07 | 华中农业大学 | A kind of method of Solid phase extraction separation gossypol in solution from gossypol |
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Application publication date: 20150603 |