CN100348568C - Process for extracting high purity alpha-linolenic acid from pepper category and medicine application thereof - Google Patents
Process for extracting high purity alpha-linolenic acid from pepper category and medicine application thereof Download PDFInfo
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- CN100348568C CN100348568C CNB2005100961936A CN200510096193A CN100348568C CN 100348568 C CN100348568 C CN 100348568C CN B2005100961936 A CNB2005100961936 A CN B2005100961936A CN 200510096193 A CN200510096193 A CN 200510096193A CN 100348568 C CN100348568 C CN 100348568C
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Abstract
The present invention relates to a method and medicine application thereof for extracting high-purity alpha-Linoleic acid from bunge pricklyash seeds, which provides pure traditional Chinese medicine raw medicine and various preparations for treating cancers, thrombus diseases, hyperlipemia, diabetes mellitus and senile dementia symptom. The raw medicine is extracted from the bunge pricklyash seeds which are traditional Chinese medicinal materials. The preparation of the high-purity alpha-Linoleic acid is divided into the four processes of saponification and acid hydrolysis, subzero refrigeration, urea containing and silver nitrate complexation. The content of the alpha-Linoleic acid in the product goes beyond more than 90%, and achieves the No. 1 class new medicine raw medicine standard of traditional Chinese medicine of China; the various designed preparations have the advantages of standard process, low cost, stable quality and convenient application. The present invention has the efficiency of spleen strengthening, stomach militating, liver nourishing, kidney tonifying, qi circulation promotion, stagnation expelling, blood circulation activation, silt removal, sore removal, pleasure and intelligence benefitting. The present invention can effectively prevent and treat the cancers, the thrombus dieasses, the hyperlipemia, the diabetes mellitus and the senile dementia symptom.
Description
Affiliated technical field
Green pepper order of the present invention extracts the method for high-purity alpha-linolenic acid and medicinal application belongs to Chinese medicine material medicine processing technology and new drug is used, and relates in particular to the effective constituent extracted from Chinese medicine, natural drug and the preparation technology of preparation thereof.
Background technology
Alpha-linolenic acid is called punicic acid, belongs to n-3 series polyenoic acid, is called for short α-LXA, formal name used at school: all-cis formula-9,12, and the 15-punicic acid, non-conjugated steric configuration, molecular formula is: C
18H
30O
2It is present in the deep green plant with the form of glyceride, α-Ya is tingle enter human body after, under the effect of enzyme, generate EPA and DHA, this biological process is irreversible, it is the important component that constitutes human tissue cell, be to maintain the indispensable fatty acid that human body is evolved, kept fit, vital role to human body has three aspects: the one, have antithrombotic, anti-blood contrary, regulate blood viscosity, reduce the effect of triglyceride and cholesterol level in the blood, be the important source material of hypotensive, blood lipid-lowering medicine and protective foods; The 2nd, have very strong growth intelligence, vision protection, bring high blood pressure down, delay senility, antianaphylaxis, the generation of inhibition cancer and the effect of transfer; The 3rd, the multiple function that has anti-inflammatory, anti-heart disorder and regulate cerebral nervous system.Modern Chinese herbal medicine research also confirms, alpha-linolenic acid has the effect of invigorating the spleen and regulating the stomach, nourishing liver and kidney, activating QI to alleviate the depression, promoting blood circulation to remove blood stasis, Xiao wei myogenic, the intelligence development of calming the nerves, effectively treatment and preventing cancer, thrombus disease, hyperlipidemia, diabetes and senile dementia.Announcement along with its important physiological function, the alpha-linolenic acid product has become food in last century, medicine, the exploitation focus of field of health care food, as " U.S.'s fish oil capsule and pill ", " the dark Ursine seal fat softgel in the North Sea " etc. all once once becoming hot-sale products, but the said products be with deep sea animal be that raw material processes, production cost height not only, also human body there is certain side effect, the development of raw materials emphasis is transferred to the plant class in recent years, the plant resources that contains alpha-linolenic acid is very abundant, according to present grasp, plant at China's alpha-linolenic acid content＞30% has 53 kinds, what alpha-linolenic acid content was the highest in the domestic edible oil is perilla oil and oleum lini, but as medicinal raw material, its contained toxic side effect but becomes obstacle.The beginning of this century, utilize the Semen zanthoxyli oil of seed (the Chinese medicinal materials green pepper order) extraction of Rutaceae plant pepper, being used for the edible oil approved produces in batches, alpha-linolenic acid content is higher than 30% in its lipid acid, because aboundresources, low production cost, have no side effect, the Application and Development of protective foods and medicine is just carried out multi-faceted, utilizing the processing of Chinese medicinal materials green pepper order and extracting high-purity alpha-linolenic acid and use also becomes the scientific research focus, especially exploitation treatment and preventing cancer, thrombus disease, hyperlipidemia, country's one class tcm product of diabetes and senile dementia has more wide domestic and abroad market prospect.
Summary of the invention
The objective of the invention is: utilize Chinese medicinal materials green pepper order to be raw material, adopt the Technology of innovation, the processing and the high-purity alpha-linolenic acid of purifying out, guarantee that content surpasses 90%, become a national class new Chinese medicine bulk drug, and, declare " not the effective constituent of from Chinese medicine, natural drug, extracting and the preparation thereof of list marketing " at home at treatment and preventing cancer, thrombus disease, hyperlipidaemia, diabetes and senile dementia processing injection, soft capsule and tablet and protective foods lays the foundation for taking the lead in.
To achieve these goals, the technical solution used in the present invention is: utilize Chinese medicinal materials green pepper order to be raw material, adopt Semen zanthoxyli oil processing technology and alpha-linolenic acid purification techniques, produce alpha linolenic acid content and be higher than 90% national Chinese medicine one kind new medicine bulk drug, and processing alpha-linolenic acid injection, alpha-linolenic acid soft capsule and alpha-linolenic acid tablet.High-purity alpha-linolenic acid is divided into saponification acidolysis, cryogenic freezing, urea clathration, Silver Nitrate complexing four road technologies, the one, saponification acidolysis: get the 100mL Semen zanthoxyli oil and 120mL10%NaOH solution mixes, reaction is 1 hour under 75 ℃ of conditions, after treating that temperature is reduced to 70 ℃, add 50mL95% ethanol, continue reaction 3 hours, after treating that temperature is reduced to 60 ℃, slowly splash into 50% sulfuric acid, make pH value of solution value to 2～3, isolate upper strata fluid, wash 3 times with separating funnel, isolate oil phase, 4 ℃ of preservations of mixed fatty acid standby; The 2nd, subzero fractionation: get and add 95% ethanol 100ml among the every 100mL of mixed fatty acid of saponification acidolysis gained, descended freezing 8～12 hours at-2 ℃～-5 ℃, filter, wash with water behind the filtrate recycling ethanol 3 times, isolating upper oil phase dewaters with anhydrous magnesium sulfate, filter, 4 ℃ of preservations of mixed fatty acid are standby; The 3rd, urea clathration: in 200mL95% ethanol, add 100g analytical pure urea, after reflux to urea dissolves fully under 70 ℃ of conditions, mixed fatty acid 100mL behind the adding subzero fractionation stirred 30 minutes, and is following freezing 8～12 hours respectively at 5 ℃ ± 2 ℃ ,-6 ℃ ± 2 ℃ ,-12 ℃ ± 2 ℃ successively again, freezing for the third time back is suction filtration fast, reclaim ethanol after washing residuum three times, isolate oil phase, dewater with anhydrous magnesium sulfate, filter, 4 ℃ of preservations of alpha-linolenic acid mixture are standby; The 4th, Silver Nitrate complexing: get 100mL alpha-linolenic acid mixture and join 400mL4mol/LAgNO
3In the solution, 0 ℃ ± 2 ℃ were stirred 1 hour down, and water phase separated and oil phase with the petroleum ether extraction water of 200 mL60～90 boiling ranges, are isolated the sherwood oil phase, reclaim sherwood oil and promptly get content greater than 90% alpha-linolenic acid.
The high-purity alpha-linolenic acid that obtains, alpha-linolenic acid content is higher than 90% in the product, no foreign odor, no rancid flavor remains clear and brightly in the time of 10 ℃, and saponification value is 185-200, and iodine number is 79-128, and acid number is lower than 0.56.The technology of processing alpha-linolenic acid injection be: raw material and consumption are that 10 milliliters of high-purity alpha-linolenic acids, 100 milliliters of poloxamers and water for injection add to 1000 milliliters, add and get earlier man-hour in the high-purity alpha-linolenic acid adding dry combustion method cup, add poloxamer again, add in an amount of water for injection after mixing immediately, mixing, add injection water to 1000 milliliter again, 0.22 μ m film degerming, with sterilize after every 2 milliliters of embeddings finished product; The technology of processing alpha-linolenic acid soft capsule is: with high-purity alpha-linolenic acid is feed liquid, and adopting soft capsule processing units direct production to go out loading amount is 0.1～0.6 milliliter of plurality of specifications soft capsule, gets finished product.The technology of processing alpha-linolenic acid tablet is that per 10,000 tablet raw materials and consumption are respectively high-purity alpha-linolenic acid 2.0kg, dextrin 1.25kg, starch 7.25kg, Magnesium Stearate 0.15kg, add and earlier alpha-linolenic acid is added in the mixture of starch, dextrin man-hour, stir, make into softwood, granulate, drying adds Magnesium Stearate again, whole grain back had both got finished product by 1000 milligrams of compressing tablets.
In pilot scale, processed 3 batches in high-purity alpha-linolenic acid sample, alpha-linolenic acid content is between 91%～98%, and as raw material, process alpha-linolenic acid injection, alpha-linolenic acid soft capsule and three kinds of product samples of alpha-linolenic acid tablet respectively, sample quality is stable.
The invention has the beneficial effects as follows: utilize the technology material of processing of Chinese medicinal materials green pepper order and purification alpha-linolenic acid to learn standard, with low cost, steady quality, alpha-linolenic acid content has surpassed 90%, reached a national class Chinese medicine material medicine standard, the formulation samples steady quality has possessed and has declared the primary condition of " not the effective ingredient of extracting and the preparation thereof of list marketing " at home from Chinese medicine, natural drug.
Description of drawings
Fig. 1 extracts the high-purity alpha-linolenic acid process flow sheet for the green pepper order.
Extremely the first time, mixed fatty acid was the saponification acidolysis process flow process stage from Semen zanthoxyli oil among Fig. 1.
Among Fig. 1 from the first time mixed fatty acid to mixed fatty acid for the second time be the cryogenic freezing technical process stage.
Among Fig. 1 from the second time mixed fatty acid to mixed fatty acid for the third time be the urea clathrate process flow process stage.
It is the Silver Nitrate complexing technical process stage from mixed fatty acid to alpha-linolenic acid for the third time among Fig. 1.
Embodiment
1, starting material are standby
(1) Semen zanthoxyli oil is standby: collect the green pepper order in the collecting period at Chinese prickly ash, earlier green pepper order exodermis is broken away from inner casing with corn or wheat debranner machinery, form behind the sticky shape flush away exodermis grease and granulated slag in warm water, and drag for the sky seed, obtain the complete clean benevolence light seed that contains, again the light seed is squeezed equipment with vegetables oil or the critical extraction equipment of carbonic acid gas processes the Semen zanthoxyli oil crude oil, at last with the crude oil depickling, take off flavor, seasoning more than one month under 5 ℃～-10 ℃ cold condition behind the decolorization refining, treat that low temperature is analysed and get supernatant liquid filtering behind the layer to obtain Semen zanthoxyli oil standby that it is standby also can to purchase the edible Semen zanthoxyli oil of one-level.
(2) Semen zanthoxyli oil purification alpha-linolenic acid industrial chemicals is standby: 10% sodium hydroxide, 95% ethanol, 50% sulfuric acid, anhydrous magnesium sulfate, analytical pure urea, Silver Nitrate, and standby in right amount respectively.
(3) pharmaceutical adjunct is standby: injection auxiliary material tensio-active agent poloxamer; Additive of tablet is with weighting agent dextrin, starch and magnesium stearate lubricant, and is standby in right amount respectively.
2, Semen zanthoxyli oil purification high-purity alpha-linolenic acid method
Process flow sheet in the by specification accompanying drawing, concrete working method is divided into four-stage:
1. saponification acidolysis: get the 100mL Semen zanthoxyli oil and 120mL 10%NaOH solution mixes, reaction is 1 hour under 75 ℃ of conditions, treat that temperature is reduced to 70 ℃ after, add 50mL 95% ethanol, continue reaction 3 hours, after treating that temperature is reduced to 60 ℃, slowly splash into 50% sulfuric acid, make pH value of solution value to 2～3, isolate upper strata fluid with separating funnel, wash 3 times, isolate oil phase, 4 ℃ of preservations of mixed fatty acid standby;
2. low temperature is cool freezes: get and add 95% ethanol 100ml among the every 100mL of mixed fatty acid of saponification acidolysis gained, descended freezing 8～12 hours at-2 ℃～-5 ℃, filter, wash with water behind the filtrate recycling ethanol 3 times, isolating upper oil phase dewaters with anhydrous magnesium sulfate, filter, 4 ℃ of preservations of mixed fatty acid are standby.
3. urea clathration: in 200mL95% ethanol, add 100g analytical pure urea, after reflux to urea dissolves fully under 70 ℃ of conditions, mixed fatty acid 100mL behind the adding subzero fractionation stirred 30 minutes, and is following freezing 8～12 hours respectively at 5 ℃ ± 2 ℃ ,-6 ℃ ± 2 ℃ ,-12 ℃ ± 2 ℃ successively again, freezing for the third time back is suction filtration fast, reclaim ethanol after washing residuum three times, isolate oil phase, dewater with anhydrous magnesium sulfate, filter, 4 ℃ of preservations of alpha-linolenic acid mixture are standby.
4. Silver Nitrate complexing: get 100mL alpha-linolenic acid mixture and join in the silver nitrate solution of 400mL4mol/L, 0 ℃ ± 2 ℃ were stirred 1 hour down, water phase separated and oil phase, petroleum ether extraction water with 200mL60～90 boiling ranges, isolate the sherwood oil phase, reclaim sherwood oil and promptly get content greater than 90% alpha-linolenic acid, every kilogram of Semen zanthoxyli oil yield is about 250 grams.
3, alpha-linolenic acid process for preparing injection liquid
Accurately measure 10 milliliters of high-purity alpha-linolenic acids, put into the exsiccant beaker, get 100 milliliters of poloxamers again, mix the back and add earlier in an amount of water for injection, mixing adds injection water to 1000 milliliter again, 0.22 μ m film degerming, embedding is in 500 ampoules, and 100 degree were sterilized 40 minutes in the rotating type sterilization device at last, promptly got product.
4, alpha-linolenic acid soft capsule production technique
With high-purity alpha-linolenic acid is feed liquid, adopts the soft capsule processing units, directly is processed into 0.1～0.6 milliliter of plurality of specifications soft capsule and gets product.
5, alpha-linolenic acid tablet manufacturing technology
Per 10,000 tablet raw materials and consumption are respectively height purity alpha-linolenic acid 2.0kg, dextrin 1.25kg, starch 7.25kg, Magnesium Stearate 0.15kg, add and man-hour starch and dextrin are mixed, add alpha-linolenic acid again and stir, make softwood, granulate with 14-16 order nylon mesh, 80 ℃ of left and right sides air seasonings, in dried particle, add Magnesium Stearate, through the whole grain of 14 mesh sieves, mixing, be pressed into 1000 milligrams heavy tablets, promptly get product.
Claims (1)
1, a kind of method of from the green pepper order, extracting high-purity alpha-linolenic acid, it is characterized in that: step 1 is the saponification acidolysis: get the 100mL Semen zanthoxyli oil and 120mL10%NaOH solution mixes, reaction is 1 hour under 75 ℃ of conditions, after treating that temperature is reduced to 70 ℃, add 50mL95% ethanol, continue reaction 3 hours, after treating that temperature is reduced to 60 ℃, slowly splash into 50% sulfuric acid, make pH value of solution value to 2～3, isolate upper strata fluid, wash 3 times with separating funnel, isolate oil phase, 4 ℃ of preservations of mixed fatty acid standby; Step 2 is a subzero fractionation: get and add 95% ethanol 100mL among the mixed fatty acid 100mL of saponification acidolysis gained, descended freezing 8～12 hours at-2 ℃～-5 ℃, filter, wash with water behind the filtrate recycling ethanol 3 times, isolating upper oil phase dewaters with anhydrous magnesium sulfate, filter, 4 ℃ of preservations of mixed fatty acid are standby; Step 3 is a urea clathration: add 100g analytical pure urea in 200mL95% ethanol, after reflux to urea dissolves fully under 70 ℃ of conditions, mixed fatty acid 100mL behind the adding subzero fractionation, stirred 30 minutes, following freezing 8～12 hours respectively at 5 ℃ ± 2 ℃ ,-6 ℃ ± 2 ℃ ,-12 ℃ ± 2 ℃ successively again, freezing for the third time back is suction filtration fast, reclaim ethanol after washing residuum three times, isolate oil phase, dewater with anhydrous magnesium sulfate, filter, 4 ℃ of preservations of alpha-linolenic acid mixture are standby; Step 4 is the Silver Nitrate complexing: get 100mL alpha-linolenic acid mixture and join 400mL 4mol/LAgNO
3In the solution, 0 ℃ ± 2 ℃ were stirred 1 hour down, and water phase separated and oil phase with 200mL60～90 boiling range petroleum ether extraction waters, are isolated the sherwood oil phase, reclaim sherwood oil and promptly get content greater than 90% alpha-linolenic acid.
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| CN101530497B (en) * | 2008-03-13 | 2012-05-23 | 成都中医药大学 | Extract and composition of rutaceae zanthoxylum peel, preparing method and application thereof |
| CN103263401B (en) * | 2013-05-23 | 2014-10-08 | 吉林大学 | Pinenut oil pinolenic acid microcapsule and preparation method thereof |
| CN104418726A (en) * | 2013-08-20 | 2015-03-18 | 陕西中鼎华盛农业发展有限公司 | Extraction method of [alpha]-linolenic acid |
| CN104649895B (en) * | 2015-02-12 | 2016-04-06 | 湖北华龙生物制药有限公司 | The preparation method of the alpha-linolenic acid of 98% purity |
| CN107019691A (en) * | 2016-02-02 | 2017-08-08 | 广州中医药大学第二附属医院 | Alpha-linolenic acid as 1 type plasminogen activator inhibitor conditioning agent application |
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| JPH0984590A (en) * | 1995-09-21 | 1997-03-31 | Itouen:Kk | Production of alpha-linolenic acid |
| US5709888A (en) * | 1990-10-30 | 1998-01-20 | Abbott Laboratories | High fat nutritional formula for infants and adults |
| CN1235956A (en) * | 1999-05-04 | 1999-11-24 | 朱铁保 | Method for extracting and separating alpha-linolenic acid |
| CN1386497A (en) * | 2001-05-23 | 2002-12-25 | 上海展望集团有限公司 | Alpha-linolenic acid microcapsule and its preparing process |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5709888A (en) * | 1990-10-30 | 1998-01-20 | Abbott Laboratories | High fat nutritional formula for infants and adults |
| JPH0984590A (en) * | 1995-09-21 | 1997-03-31 | Itouen:Kk | Production of alpha-linolenic acid |
| CN1235956A (en) * | 1999-05-04 | 1999-11-24 | 朱铁保 | Method for extracting and separating alpha-linolenic acid |
| CN1386497A (en) * | 2001-05-23 | 2002-12-25 | 上海展望集团有限公司 | Alpha-linolenic acid microcapsule and its preparing process |
Non-Patent Citations (1)
| Title |
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| 硝酸银—硅胶纯化α-亚麻酸的研究 张汆等.离子交换与吸附，第21卷第1期 2005 * |
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