CN103570517B - A kind of method extracting separating curcumin - Google Patents
A kind of method extracting separating curcumin Download PDFInfo
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- CN103570517B CN103570517B CN201310531265.XA CN201310531265A CN103570517B CN 103570517 B CN103570517 B CN 103570517B CN 201310531265 A CN201310531265 A CN 201310531265A CN 103570517 B CN103570517 B CN 103570517B
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- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
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Abstract
A kind of method extracting separating curcumin, comprises the following steps: (1) extracts: pulverized by Rhizoma Curcumae Longae, adds the potass extraction that mass concentration is 2 10%, obtains potass extraction liquid;(2) defat: add organic solvent petroleum ether, 6# solvent naphtha, hexamethylene, benzene, toluene or ethyl acetate in potass extraction liquid, after stirring extracts 12 hours, stand 12 hours, separate organic layer;(3) acid is heavy: by extracting solution salt acid for adjusting pH to 12, make curcumin separate out, and filters, is dried to constant weight, obtains curcumin crude product;(4) refined: curcumin crude product organic solvent methanol, ethanol, acetone, n-butyl alcohol or isopropanol are dissolved, filter, toward filtrate in, add distilled water, 05 DEG C of freezing crystallizes 28 hours, filter, dry, obtain curcumin product.Production cost of the present invention is low, and gained curcumin product purity is high, up to more than 98.5%.
Description
Technical field
The present invention relates to a kind of method extracting separating curcumin.
Background technology
Rhizoma Curcumae Longae is abounded with in Southeast Asian countries and regions, and diet and medical treatment aspect are all widely used abroad, and the most also there is distribution in the Rhizoma Curcumae Longae place of production.Important component curcumin in Rhizoma Curcumae Longae is a kind of natural pigment, and the method that the producer of domestic production curcumin generally uses is organic solvent extraction.The shortcoming of organic solvent extraction is that consumption of organic solvent is very big, and production cost is higher, and the curcumin content only 95% produced.
Summary of the invention
It is low that the technical problem to be solved is to provide one not only production cost, and the method extracting separating curcumin that in products obtained therefrom, curcumin content is high.
The technical solution adopted for the present invention to solve the technical problems: a kind of method extracting separating curcumin, comprises the following steps:
(1) extract: Rhizoma Curcumae Longae is pulverized, add mass concentration be the preferred 5-9% of 2-10%() potass extraction, aqueous alkali consumption is 1-20 times (preferably 6-12 times) of Rhizoma Curcumae Longae raw material weight, and extraction time is 1-6 hour (preferably 3-5 hour), Extracting temperature is 20-30 DEG C, obtains potass extraction liquid;
(2) defat: add organic solvent petroleum ether, 6# solvent naphtha, hexamethylene, benzene, toluene or ethyl acetate etc. in potass extraction liquid, the consumption of organic solvent is 0.5-2.5 times (preferably 0.7-1.5 times) of aqueous alkali weight, after stirring extraction 1-2 hour, stand 1-2 hour, separate organic layer, remove the liposoluble substance in extracting solution;
(3) acid is heavy: curcumin will be made to separate out through the extracting solution salt acid for adjusting pH after step (2) processes to 1-2, filter, be dried to constant weight, obtain curcumin crude product;
(4) refined: curcumin crude product organic solvent methanol, ethanol, acetone, n-butyl alcohol or isopropanol etc. are dissolved, the consumption of organic solvent is 2-30 times (preferably 8-15 times) of curcumin crude product weight, filter, distilled water is added in filtrate, the consumption of distilled water is 0.5-2.0 times of organic solvent weight, 0-5 DEG C of freezing crystallize 2-8 hour, filters, it is dried, obtains curcumin product.
Further, in step (1), described aqueous alkali is the aqueous solution of the alkaline matters such as sodium hydroxide, potassium hydroxide, calcium hydroxide or sodium carbonate.
Further, in step (2), the organic layer separated is concentrated, obtains side-product-turmeric oil.
Research shows, curcumin dissolubility dissolubility greatly and in organic solvent petroleum ether, 6# solvent naphtha, hexamethylene, benzene, toluene or ethyl acetate etc. in aqueous alkali is less, its impurity dissolubility in aqueous alkali less and in organic solvent dissolubility bigger.
Compared with prior art, the invention have the advantages that first, use cheap aqueous alkali as Extraction solvent, the cost of production can be greatly reduced;Second, use the inventive method can also obtain the turmeric oil in Rhizoma Curcumae Longae as side-product, thus improve resource utilization;3rd, the curcumin product purity using the inventive method to obtain is high, up to more than 98.5%.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The present embodiment comprises the following steps:
(1) extracting: take 100 grams of Rhizoma Curcumae Longae, be crushed to 80 mesh, add the sodium hydrate aqueous solution 800 grams that mass concentration is 5%, under the conditions of 25 DEG C, stirring is extracted 4 hours, filters, obtains potass extraction liquid;
(2) defat: add 600 grams of petroleum ether in potass extraction liquid, after stirring extracts 1.5 hours, stand 1.5 hours, upper strata petroleum ether layer is separated, remove the liposoluble substance (inspissated oil ether layer obtains side-product-turmeric oil 9 grams) in extracting solution;
(3) acid is heavy: curcumin will be made to separate out through the extracting solution salt acid for adjusting pH after step (2) processes to 2, filter, be dried to constant weight, obtain curcumin crude product 6.2 grams, content is 85.6%(efficient liquid phase external standard method);
(4) refined: by 6.2 grams of curcumin crude products with 60 grams of acetone solutions, to filter, toward filtrate in, add 75 grams of distilled water, 0 DEG C of freezing crystallize 6 hours, filtration, dry, obtain curcumin product 5.5 grams, content is 99.10%(efficient liquid phase external standard method).
Embodiment 2
The present embodiment comprises the following steps:
(1) extracting: take 200 grams of Rhizoma Curcumae Longae, be crushed to 80 mesh, add the aqueous sodium carbonate 2000 grams that mass concentration is 9%, under the conditions of 30 DEG C, stirring is extracted 5 hours, filters, obtains potass extraction liquid;
(2) defat: add 2000 grams of toluene in potass extraction liquid, after stirring extracts 1.5 hours, stand 1.5 hours, separated by upper toluene layer, removes the liposoluble substance in extracting solution (concentrating toluene layer, obtain side-product-turmeric oil 21 grams);
(3) acid is heavy: salt acid for adjusting pH will be used after step (2) processes to 2, and make curcumin separate out, filter, be dried to constant weight, obtain curcumin crude product 12.6 grams, content is 87.5%(efficient liquid phase external standard method);
(4) refined: 12.6 grams of curcumin crude products are dissolved with 150 grams of ethanol, filter, 200 grams of distilled water of addition toward filtrate in, 0 DEG C of freezing crystallize 8 hours, filtration, dry, obtain curcumin fine work 10.8 grams, content is 98.5%(efficient liquid phase external standard method).
Claims (2)
1. the method extracting separating curcumin, it is characterised in that comprise the following steps:
(1) extracting: pulverized by Rhizoma Curcumae Longae, adding mass concentration is the potass extraction of 5-9%, and aqueous alkali consumption is 6-12 times of Rhizoma Curcumae Longae raw material weight, and extraction time is 3-5 hour, and Extracting temperature is 25-30 DEG C, obtains potass extraction liquid;Described aqueous alkali is the aqueous solution of sodium hydroxide or sodium carbonate;
(2) defat: adding organic solvent petroleum ether or toluene in potass extraction liquid, the consumption of organic solvent is 0.7-1.5 times of aqueous alkali weight, after stirring extracts 1-2 hour, stands 1-2 hour, separates organic layer, removes the liposoluble substance in extracting solution;
(3) acid is heavy: curcumin will be made to separate out through the extracting solution salt acid for adjusting pH after step (2) processes to 2, filter, be dried to constant weight, obtain curcumin crude product;
(4) refined: by curcumin crude product organic solvent ethanol or acetone solution, the consumption of organic solvent is 8-15 times of curcumin crude product weight, filter, distilled water is added in filtrate, the consumption of distilled water is 0.5-2.0 times of organic solvent weight, 0-5 DEG C of freezing crystallize 2-8 hour, filters, it is dried, obtains curcumin product.
The method of extraction separating curcumin the most according to claim 1, it is characterised in that in step (2), the organic layer separated is concentrated, obtains side-product-turmeric oil.
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CN104017389A (en) * | 2014-05-30 | 2014-09-03 | 南京工业大学 | Preparation method of turmeric natural dye |
CN104327538A (en) * | 2014-10-23 | 2015-02-04 | 西安莹朴生物科技股份有限公司 | Preparation method of curcumine |
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CN105669409B (en) * | 2016-01-12 | 2018-01-05 | 郭月玲 | A kind of curcumin extracting method |
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CN107805193B (en) * | 2017-11-27 | 2020-11-06 | 晨光生物科技集团股份有限公司 | Production method of low-solubility residual curcumin crystal |
CN108586217A (en) * | 2018-04-02 | 2018-09-28 | 太阳树(厦门)生物工程有限公司 | A method of extracting paradol from paradise green pepper |
CN111153784A (en) * | 2019-12-26 | 2020-05-15 | 湖北回盛生物科技有限公司 | Method for extracting, separating and purifying curcumin |
CN111961560B (en) * | 2020-07-22 | 2023-04-28 | 浙江中医药大学 | Ginger chrysanthemum juice wine and preparation method thereof |
CN112521259B (en) * | 2020-12-24 | 2022-11-18 | 晨光生物科技集团股份有限公司 | Preparation method of natural curcumin without vanillin |
CN113144043A (en) * | 2021-04-24 | 2021-07-23 | 湖州润合医药科技有限公司 | Composition for preventing and improving hypomnesis and senile dementia and preparation method and application thereof |
CN115403457B (en) * | 2022-08-16 | 2023-06-23 | 神威药业集团有限公司 | A method for preparing Curcuma rhizome extract |
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