CN102961637A - Method for extracting and purifying general flavones in corn stigma - Google Patents
Method for extracting and purifying general flavones in corn stigma Download PDFInfo
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- CN102961637A CN102961637A CN2012105259189A CN201210525918A CN102961637A CN 102961637 A CN102961637 A CN 102961637A CN 2012105259189 A CN2012105259189 A CN 2012105259189A CN 201210525918 A CN201210525918 A CN 201210525918A CN 102961637 A CN102961637 A CN 102961637A
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Abstract
The invention belongs to the technical field of preparation of general flavones, and in particular relates to a method for extracting and purifying general flavones in corn stigma. The method for extracting and purifying general flavones in corn stigma comprises the following steps of: (1) preparing raw materials; (2) treating the raw materials; (3) recycling ethanol; (4) standing settlement; (5) filtering and concentrating; (6) carrying out alkali wash and acid wash; (7) carrying out resin separation; (8) eluting; (9) recycling ethanol; (10) spraying and drying; and (11) putting finished products into storage. The method for extracting and purifying general flavones in corn stigma has the following advantages: (1) the technology process is simple and short; (2) the product purity is high; and (3) the production cost is lowered.
Description
Technical field
The invention belongs to the technical field of total flavones preparation, be specifically related to the extraction and purification method of total flavones in a kind of Stigma Maydis.
Background technology
Stigma Maydis is style and the stigma of the beautiful administration of grass family plant Semen Maydis, and it contains the number of chemical composition, such as volatile oil, saponin, alkaloid, class total flavones, poly pentose, organic acid etc.Pharmacology activity research shows: extractive of general flavone can reduce the blood pressure of Hypertensive Rats in the Stigma Maydis, and it is down to normal arterial pressure, on the almost not impact of blood pressure with normotensive rat; Extractive of general flavone has the effect of obvious reduction rat blood serum T-CHOL and triglyceride in the Stigma Maydis, and becomes certain dose-effect relationship.
Therefore, the Stigma Maydis total flavones extract is as a kind of biological active substances, uses very extensively, not only can be used as food but also can be used as the configuration raw material of multiple medicine, various health product.Because extractive of general flavone has high using value and prospect in the Stigma Maydis.So, in the last few years, comprised that the expert of many countries of China, scholar have carried out extensive and deep research to the method for the extraction total flavones from Stigma Maydis, had obtained gratifying achievement.But the alcohol extract or the water extract that are summed up the most frequently used method and are Stigma Maydis suspend in water, and use successively different solvent extraction, and solvent commonly used has chloroform, ethyl acetate and saturated n-butyl alcohol.Total flavones in the Stigma Maydis focuses mostly in n-butanol layer, the reclaim under reduced pressure n-butyl alcohol; Extractum concentration is 95% dissolve with ethanol, and makes it pass through activated-charcoal column; Collect effluent and decompression recycling ethanol, make finished product.The total flavones Main Problems that utilizes this method to extract in the Stigma Maydis is: (1) product cost is high, (2) impurity in the product, particularly the content of harmful substance is higher, wherein content of beary metal surpasses 5ppm, persticide residue is greater than 10ppb, surpass prescribed limit, simultaneously residual toxicity solvent, n-butanol etc. inevitably.
In addition, said extracted method complex process, solvent consumption and residual quantity are large, so that cost increases, the part beneficiating ingredient runs off.
Summary of the invention
The object of the invention is to for the defective of above-mentioned existence and the extraction and purification method of total flavones in a kind of Stigma Maydis is provided.
Technical scheme of the present invention is: the extraction and purification method of total flavones in a kind of Stigma Maydis may further comprise the steps:
(1) preparation of raw material: Stigma Maydis is positioned in the baking oven cured under 70 ℃ 6 hours, make Stigma Maydis lose free water, the length that then Stigma Maydis is cut into 1 ㎝ is stand-by;
(2) processing of raw material: add the ethanol of 5 times of Stigma Maydis weight in the described Stigma Maydis of step (1), wherein the mass fraction of ethanol is 50%, 50～60 ℃ of control temperature, said extracted triplicate, then merge extractive liquid;
(3) Recycled ethanol: the concentrated and Recycled ethanol with the extracting solution distilling under reduced pressure, distilling under reduced pressure concentration of alcohol to the extracting solution obtains concentrated solution less than 2.5%;
(4) staticly settle: the concentrated solution that step (3) is obtained staticly settles 6～8 hours under 20 ℃ of conditions;
(5) filtering and concentrating: after staticly settling, in the supernatant of gained, add the kieselguhr that accounts for supernatant quality 2% and filter clarification, obtain clear liquor;
(6) alkali cleaning, pickling: add mass fraction and be 15% sodium hydroxide solution in the clear liquor of step (5) gained, left standstill after the stirring 1 hour, then add concentration and be 16% hydrochloric acid, the pH value that makes clear liquor is 6～7, and the filtering precipitation obtains filtrate;
(7) resin isolation: with the total flavones in the filtrate usefulness macroporous resin exchange column absorption filtrate of step (6) gained;
(8) eluting: be that 70% ethanol elution is adsorbed on the total flavones in the macroporous resin exchange column with mass fraction, obtain ethanol elution;
(9) Recycled ethanol: ethanol elution is concentrated into concentration of alcohol less than 2.5% and Recycled ethanol, obtains concentrated solution;
(10) spray drying: in spray tower, the resulting concentrated solution of step (9) is dried to powdery, obtains the total flavones powder;
(11) finished product warehouse-in: the total flavones powder is sub-packed in the double-layer plastic bag fitted tube warehouse-in.
The described Stigma Maydis water content of step (1) is 20%.
Beneficial effect of the present invention is: the present invention compares with the existing method of extracting total flavones from Stigma Maydis has following advantage: (1) technological process is brief: technological process of the present invention utilizes the alkali pickling, the protein in the extracting solution, half soluble fiber, tannin have been removed, saved n-butanol extraction, polyamide is refining; (2) product purity is high: because most of impurity has been removed in the alkali pickling, reduced the residual of harmful element in the product, made being improved of total flavones in the product; (3) reduced production cost: owing to do not use expensive food stage n-butyl alcohol solvent and polyamide, and reduced corresponding extraction equipment, therefore reduced the cost of product.
The specific embodiment
The extraction and purification method of total flavones in a kind of Stigma Maydis may further comprise the steps:
(1) preparation of raw material: (milpa grows to the period of maturation in harvesting from corn planting farmland, village, Shandong, Stigma Maydis is sepia, water content is about 20%), Stigma Maydis is positioned in the baking oven under 70 ℃, cured 6 hours, make Stigma Maydis lose free water, the length that then Stigma Maydis is cut into 1 ㎝ is stand-by;
(2) processing of raw material: add the ethanol of 5 times of Stigma Maydis weight in the described Stigma Maydis of step (1), wherein the mass fraction of ethanol is 50%, 50～60 ℃ of control temperature, said extracted triplicate, then merge extractive liquid;
(3) Recycled ethanol: the concentrated and Recycled ethanol with the extracting solution distilling under reduced pressure, distilling under reduced pressure concentration of alcohol to the extracting solution obtains concentrated solution less than 2.5%;
(4) staticly settle: the concentrated solution that step (3) is obtained staticly settles 6～8 hours under 20 ℃ of conditions;
(5) filtering and concentrating: after staticly settling, in the supernatant of gained, add the kieselguhr that accounts for supernatant quality 2% and filter clarification, obtain clear liquor;
(6) alkali cleaning, pickling: add mass fraction and be 15% sodium hydroxide solution in the clear liquor of step (5) gained, left standstill after the stirring 1 hour, then add concentration and be 16% hydrochloric acid, the pH value that makes clear liquor is 6～7, and the filtering precipitation obtains filtrate;
(7) resin isolation: with the total flavones in the filtrate usefulness macroporous resin exchange column absorption filtrate of step (6) gained;
(8) eluting: be that 70% ethanol elution is adsorbed on the total flavones in the macroporous resin exchange column with mass fraction, obtain ethanol elution;
(9) Recycled ethanol: ethanol elution is concentrated into concentration of alcohol less than 2.5% and Recycled ethanol, obtains concentrated solution;
(10) spray drying: in spray tower, resulting concentrated solution in the step (9) is dried to powdery, obtains the total flavones powder;
(11) finished product warehouse-in: the total flavones powder is sub-packed in the double-layer plastic bag fitted tube warehouse-in.
Claims (2)
1. the extraction and purification method of total flavones in the Stigma Maydis may further comprise the steps:
(1) preparation of raw material: Stigma Maydis is positioned in the baking oven cured under 70 ℃ 6 hours, make Stigma Maydis lose free water, the length that then Stigma Maydis is cut into 1 ㎝ is stand-by;
(2) processing of raw material: add the ethanol of 5 times of Stigma Maydis weight in the described Stigma Maydis of step (1), wherein the mass fraction of ethanol is 50%, 50～60 ℃ of control temperature, said extracted triplicate, then merge extractive liquid;
(3) Recycled ethanol: the concentrated and Recycled ethanol with the extracting solution distilling under reduced pressure, distilling under reduced pressure concentration of alcohol to the extracting solution obtains concentrated solution less than 2.5%;
(4) staticly settle: the concentrated solution that step (3) is obtained staticly settles 6～8 hours under 20 ℃ of conditions;
(5) filtering and concentrating: after staticly settling, in the supernatant of gained, add the kieselguhr that accounts for supernatant quality 2% and filter clarification, obtain clear liquor;
(6) alkali cleaning, pickling: add mass fraction and be 15% sodium hydroxide solution in the clear liquor of step (5) gained, left standstill after the stirring 1 hour, then add concentration and be 16% hydrochloric acid, the pH value that makes clear liquor is 6～7, and the filtering precipitation obtains filtrate;
(7) resin isolation: with the total flavones in the filtrate usefulness macroporous resin exchange column absorption filtrate of step (6) gained;
(8) eluting: be that 70% ethanol elution is adsorbed on the total flavones in the macroporous resin exchange column with mass fraction, obtain ethanol elution;
(9) Recycled ethanol: ethanol elution is concentrated into concentration of alcohol less than 2.5% and Recycled ethanol, obtains concentrated solution;
(10) spray drying: in spray tower, the resulting concentrated solution of step (9) is dried to powdery, obtains the total flavones powder;
(11) finished product warehouse-in: the total flavones powder is sub-packed in the double-layer plastic bag fitted tube warehouse-in.
2. the extraction and purification method of total flavones in the Stigma Maydis according to claim 1 is characterized in that, the described Stigma Maydis water content of step (1) is 20%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012105259189A CN102961637A (en) | 2012-12-10 | 2012-12-10 | Method for extracting and purifying general flavones in corn stigma |
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| CN2012105259189A CN102961637A (en) | 2012-12-10 | 2012-12-10 | Method for extracting and purifying general flavones in corn stigma |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103653177A (en) * | 2013-11-04 | 2014-03-26 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for extracting corn stigma total flavone from corn stigma and application of corn stigma total flavone |
| CN106071323A (en) * | 2016-06-24 | 2016-11-09 | 福建好来屋食品工业有限公司 | A kind of modified mixed method of corn extract |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436785A (en) * | 2002-05-15 | 2003-08-20 | 山西金甲药业有限公司 | Macroporous adsorbing resin process of extracting general flavone from haw leaf |
| CN102309694A (en) * | 2011-08-29 | 2012-01-11 | 安徽农业大学 | Method for extraction and purification of corn silk general flavone, and use of corn silk general flavone |
-
2012
- 2012-12-10 CN CN2012105259189A patent/CN102961637A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436785A (en) * | 2002-05-15 | 2003-08-20 | 山西金甲药业有限公司 | Macroporous adsorbing resin process of extracting general flavone from haw leaf |
| CN102309694A (en) * | 2011-08-29 | 2012-01-11 | 安徽农业大学 | Method for extraction and purification of corn silk general flavone, and use of corn silk general flavone |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103653177A (en) * | 2013-11-04 | 2014-03-26 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for extracting corn stigma total flavone from corn stigma and application of corn stigma total flavone |
| CN106071323A (en) * | 2016-06-24 | 2016-11-09 | 福建好来屋食品工业有限公司 | A kind of modified mixed method of corn extract |
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Application publication date: 20130313 |