CN101735234B - Preparation process for obtaining high purity sesamin from sesame cake meal - Google Patents

Preparation process for obtaining high purity sesamin from sesame cake meal Download PDF

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CN101735234B
CN101735234B CN 200910245011 CN200910245011A CN101735234B CN 101735234 B CN101735234 B CN 101735234B CN 200910245011 CN200910245011 CN 200910245011 CN 200910245011 A CN200910245011 A CN 200910245011A CN 101735234 B CN101735234 B CN 101735234B
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sesamin
cake meal
sesame
sesame cake
oil
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CN101735234A (en
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陈伟强
李树田
潘秀萍
赵小玲
李红梅
邓斌
徐廷丽
王冬兰
程义勇
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Institute of Hygiene and Environmental Medicine Academy of Military Medical Sciences of Chinese PLA
Cofco Northsea Oils and Grains Industries Tianjin Co Ltd
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Institute of Hygiene and Environmental Medicine Academy of Military Medical Sciences of Chinese PLA
Cofco Northsea Oils and Grains Industries Tianjin Co Ltd
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Abstract

The invention provides a preparation process for obtaining high purity sesamin from sesame cake meal. A series of extracting and purifying treatments are carried out on the sesame cake meal by using organic solvents such as normal hexane and the like under a certain condition to obtain the sesamin with high purity finally; raw materials used by the preparation process are solid waste materials of the sesame cake meal which are obtained after preparing sesame oil by squeezing, and the sesamin extracted by separating has higher extraction ratio which reaches about 90%; the obtained sesamin has higher purity which reaches 95.6% by HPLC detection, thereby a good basis for function development and application of the sesamin is established. The invention realizes the comprehensive utilization of the waste materials, greatly increases the additional value of farm products, has very considerable economic benefits, and is suitable for the needs of scale industrial production.

Description

A kind of preparation technology who from sesame cake meal, obtains high purity sesamin
Technical field
The present invention relates to a kind of preparation technology of sesamin, especially a kind of preparation technology who from sesame cake meal, obtains high purity sesamin.
Background technology
Sesamin (sesamin) is subject to people's attention just day by day as a kind of crude substance of biologically active, and it in the application in fields such as healthcare products, foodstuffs industry and medical and health more and more widely.Sesamin is one of important biological composition in the sesame (sesamum indicum), is a kind of of lignan compounds, and lignan content in sesame is 0.5%~1%, and sesamin accounts for more than 50% in this compounds.Sesame has been planted a lot of centuries as important oil crops, extensively plant in the developing country in Asia and Africa especially, the planted area of China's sesame is more extensive, rises gradually from output over 1997, calendar year 2001 reaches 810,000 tons, and also has very big development potentiality.Along with Japan and other countries is goed deep into the research of sesamin, people have also obtained remarkable progress to the effect and the Application and Development of sesamin.Physiological actions such as that many studies show that, sesamin have is anti-ageing, anti-oxidant, anti-inflammatory, reducing cholesterol, protection liver, hypertension, anticancer and immuno-stimulating.The human senility free-radical theory is thought: human body produces free radical in the metabolic process of vital movement, under normal circumstances, the generation and the elimination of the free radical of human body are in equilibrium state, but when the too much overbalance of free radical, will cause multiple disease and body aging.The Japan scholar experiment showed, that sesamin has very strong anti-oxidant activity in body, can effectively eliminate free radical, superoxide and hydroxy radical qiao.Scholars have studied the effect that sesamin is removed hydroxy radical qiao at the rat liver tissue, and the result shows, the liver organization 4-hydroxyl-2,2,6 of the sesamin group of ingesting, and 6-methyl piperidine-1-oxygen base disappearance speed is significantly accelerated.In addition, they have also detected the anti-oxidant activity of sesamin metabolite in bile, show that the metabolite of sesamin has the very strong removing superoxide anion and the activity of hydroxy radical qiao.Sesamin has stronger antioxygenation than vitamin-E; can stop and produce lipid peroxide in the body; thereby the microbial film of protective tissue cell effectively; improve the surrounding blood vessel blood circulation; improve volume of blood flow; increase the hemotrophic nutrition effect of histoorgan, the enhancing body immunologic function is resisted the harm of objectionable impurities to human tissue cell.And sesamin can effectively remove free radical, delays the aging of cell.In addition; sesamin can suppress the activation of microglia; neuroprotective unit avoids the infringement of excitatory toxicity; and; sesamin also can reduce lipopolysaccharide-induced cytokine and generate by the activation that suppresses p38 MAPK signal transduction pathway and NF-κ B, thereby neurocyte is played a protective role.
Sesamin is obtained from the sesame oil treating process by Japanese scholar the earliest.The separating and extracting method of sesamin mainly contains two big classes: a class is to use organic solvent such as methyl alcohol, ether etc. directly to extract sesamin from sesame oil, and then crystallization purifying.As far back as 1949, Allen just extracts sesamin with methyl alcohol from sesame oil, and its product was used to sterilant at that time.When Liu Yuanfa etc. utilize the sesame oil extraction sesamin, behind Ethanol Treatment acquisition raw product, carry out purifying with acetone-Virahol as solvent again, can obtain 0.24% sesamin, its purity is analyzed through HPLC can reach relative content 94%.Li Jiaoshe etc. use 2 crystallization processs of different solvents, obtain pure product sesamin, and yield reaches 0.15%.But as a whole, this class methods rate of recovery is low, simultaneously also because of not removing residual organic solvent in the sesame oil fully, to the formation of the utilization again potential Hazard Factor of sesame oil.The 2nd, adopt low-pressure distillation sesame oil, then its overhead product is carried out processing such as molecular distillation, resin absorption.The method of reduced steam distillation extraction sesamin has successively been proposed as Tatsuhiko Ozaki and Masato Sugiura etc., but its product is the sesame lignan class mixture of (comprising sesamin, episesamin, sesamol and sesamolin), this class methods extraction cost height has certain difficulty on the suitability for industrialized production.Therefore, seeking a kind of more effective, cheap sesamin preparation method has been imperative.
At present, the domestic machine of employing basically press for extracting juice method and water are got sesame oil for legal system.The solid substance that machine press for extracting juice legal system is got behind the sesame oil is sesame cake meal, and oily factory is to abandon or as fertilizer sources to the processing of sesame cake meal basically, and utility value is very low.A domestic large-scale sesame oil factory can produce 1400 tons to 1500 tons in sesame oil every year at present, need to consume 4000 tons sesame, wherein the sesame cake meal of Chan Shenging just has more than 2000 ton, if it is carried out deep processing Application and Development in addition, not only can realize the comprehensive utilization of waste material, and can also make additional value of farm products be ten times, tens times increase, produce considerable economic benefit.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation technology who obtains high purity sesamin from sesame cake meal.Described sesame cake meal is the dry thing of solid shape, and utility value is very low at present; Described high purity sesamin is meant that purity reaches the sesamin more than 95%, realizes the separation and Extraction of high purity sesamin in the sesame cake meal, can improve the utility value of sesame cake meal greatly, realizes the cycling and reutilization of waste material, improves additional value of farm products.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of preparation technology who from sesame cake meal, obtains high purity sesamin, concrete steps are:
(1) be that raw material extracts by normal hexane with the solid substance sesame cake meal;
(2) remove normal hexane and obtain oil-like extracts (sesame oil), press solid-liquid ratio (oil-like extracts: organic solvent, g/ml) 1: 1-5.5 adds the organic solvent be used to dissolve sesamin, stirs 4-7h down at 25-80 ℃;
(3) leave standstill 5-7h, treat layering after, get upper strata liquid and be rotated evaporation and remove organic solvent;
(4) add sherwood oil, 45-55 ℃ leaves standstill 0.5-2h, filters and obtains sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added the organic solvent that is used for dissolving sesamin, heating in water bath places 2-5 ℃ of refrigerator to carry out growing the grain 4-7h after promoting dissolving, filters then, obtains the sesamin purified crystals.
Preferably, the above-mentioned preparation technology who from sesame cake meal, obtains high purity sesamin, described organic solvent is anhydrous methanol, dehydrated alcohol or ethyl acetate.
Preferably, feed ratio is 1 among the above-mentioned preparation technology who obtains high purity sesamin from sesame cake meal, described step (2): 3.2-3.5, extracting temperature is 25-45 ℃.
Preferably, feed ratio is 1: 4.5 among the above-mentioned preparation technology who obtains high purity sesamin from sesame cake meal, described step (2).
Preferably, dwell temperature is 45-50 ℃ among the above-mentioned preparation technology who obtains high purity sesamin from sesame cake meal, described step (4).
Preferably, the above-mentioned preparation technology who from sesame cake meal, obtains high purity sesamin, the sesamin in the described step (5) after the dissolving places 4 ℃ of refrigerators to carry out growing the grain, obtains the sesamin purified crystals after repeating 2 times.
Beneficial effect of the present invention:
The above-mentioned preparation technology who from sesame cake meal, obtains high purity sesamin, employed raw material is the solid substance dead meal sesame cake meal after milling process is produced sesame oil, and the sesamin of separation and Extraction has higher extraction yield, has reached nearly 90%; Resulting sesamin purity height has reached 95.6% through the HPLC detection, for the further functional development and the application of sesamin are had laid a good foundation; Realize the comprehensive utilization of waste material, additional value of farm products is greatly increased, had considerable economic benefit, be fit to requirements of large-scale industrial production.
Description of drawings
Fig. 1 contains spirogram for HPLC Detection and Extraction sesamin crystalline.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is further described.
Embodiment 1
(1) be raw material with the solid substance sesame cake meal, sesame cake meal is pulverized with pulverizer, cross 120 mesh sieves, accurately take by weighing 500g, add the 2000ml normal hexane, 45 ℃ of water-bath 2h, middle constantly the stirring extracted;
(2) filter, filtrate is evaporated with Rotary Evaporators and is removed normal hexane and obtain oil-like extracts (sesame oil), and (oil-like extracts: anhydrous methanol g/ml) adds anhydrous methanol, at 40 ℃ of stirring 6h down at 1: 4.5 press solid-liquid ratio;
(3) leave standstill 7h, treat layering after, get upper strata liquid and be rotated evaporation and remove methyl alcohol;
(4) add sherwood oil 20ml, 45 ℃ leave standstill, and airtight mixing 0.5h filters and obtains sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added anhydrous methanol, heating in water bath places 4 ℃ of refrigerators to carry out growing the grain 7h after promoting dissolving, filters then, adds anhydrous methanol dissolving and 4 ℃ of refrigerator growing the grain 7h again, obtains the sesamin purified crystals after repeating 2 times.
Orthogonal test
Investigate different feed liquid ratio, extraction time and temperature to the influence of sesamin extraction effect, adopt single factor three levels to carry out L 9(3 4) orthogonal experimental design.Solid-liquid ratio is divided into 3 levels: 1: 1.5,1: 3,1: 4.5; Extraction time is divided into 3 levels: 2h, 4h, 6h; Temperature is divided into 3 levels: 40 ℃, 50 ℃, 60 ℃.Each each factor of test and level distribution see Table 1L 9(3 4) orthogonal test horizontal factor table, carry out 9 tests altogether.By analyzing orthogonal experiment data and result, see Table 2 orthogonal experiment data and result, its best of breed is solid-liquid ratio 1: 4.5 under selected level of factor, 40 ℃ of temperature, extraction time 6h.Carry out proof test by this optimal conditions, accurately take by weighing a certain amount of sesame cake meal, extract, add 4.5 times anhydrous methanol then, stir down 6h, behind the standing demix, get upper strata liquid and be rotated evaporation and remove methyl alcohol at 40 ℃ with normal hexane.Add sherwood oil 20ml, 45 ℃ of airtight mixing 0.5h obtain the sesamin crude product, and its extraction rate reached is to 88.3%.
Table 1.L 9(3 4) orthogonal test horizontal factor table
Figure G2009102450115D00041
Table 2. orthogonal experiment data and result
Figure G2009102450115D00051
The sesamin Determination on content
(1) colorimetry
The drafting of typical curve: 5mg sesamin standard substance are dissolved in the 10ml anhydrous methanol, obtain 500 μ g/ml sesamin solution.Be diluted to 10,20,40,80,100 μ g/ml sesamin standardized solution with anhydrous methanol then.With methyl alcohol is blank, measure the absorbancy of each concentration standard liquid, calculate the regression equation of sesamin concentration and absorbancy then, Y=95.51X+2.9119 at the 290nm place, relation conefficient γ=0.9985, prompting sesamin concentration is good in 10-100 μ g/mL scope internal linear.
With sesamin crude product and sesamin purified crystals with the anhydrous methanol dissolving after, measure absorbancy at 290nm place, then according to the content of typical curve acquisition sesamin.After measured, the content of rough sesamin and sesamin purified crystals is respectively 70% and 95%.
(2) HPLC method
Sample pre-treatments: accurately take by weighing 5mg sesamin sample in the brown volumetric flask of 25mL, add the dissolve with methanol sample, at last with methanol constant volume to 25mL.With syringe draw samples from volumetric flask, after the filtration of 0.45 μ m strainer, be injected into into sample bottle, measure liquid as sample, analyze for HPLC.
The drafting of typical curve: 5mg sesamin standard specimen is dissolved in the 25mL volumetric flask with methyl alcohol, is mixed with the standardized solution of 200 μ g/mL, pipette standardized solution,, be prepared into the standardized solution of 5,20,40,80,100,200 μ g/mL with the methyl alcohol dilution.The standardized solution 20 μ L that get different concns with microsyringe successively inject liquid chromatograph, are ordinate zou with the peak area, and concentration is X-coordinate, the drawing standard curve.Y=26138X+22514, relation conefficient γ=0.9999.
The sesamin sample is injected liquid chromatograph with microsyringe, and measurement result is seen Fig. 1, and the purity that draws the sesamin purified crystals according to typical curve is 95.6%.
Embodiment 2
A kind of preparation technology who from sesame cake meal, obtains high purity sesamin, concrete steps are:
(1) be raw material with the solid substance sesame cake meal, sesame cake meal is pulverized with pulverizer, cross 80 mesh sieves, accurately take by weighing 500g, add the 3000ml normal hexane, 45 ℃ of water-bath 2h, middle constantly the stirring extracted;
(2) filter, filtrate is evaporated with Rotary Evaporators and is removed normal hexane and obtain oil-like extracts (sesame oil), and (oil-like extracts: anhydrous methanol g/ml) adds anhydrous methanol, at 43 ℃ of stirring 5h down at 1: 3.5 press solid-liquid ratio;
(3) leave standstill 7h, treat layering after, get upper strata liquid and be rotated evaporation and remove methyl alcohol;
(4) add sherwood oil 30ml, 50 ℃ leave standstill 2h, filter and obtain sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added in the dehydrated alcohol, heating in water bath places 4 ℃ of refrigerators to carry out growing the grain 6h after promoting dissolving, filters then, adds anhydrous alcohol solution and 4 ℃ of refrigerator growing the grain 6h again, obtains the sesamin purified crystals after repeating 2 times.
After testing, sesamin crude product extraction yield 88.0%; The purity of sesamin purified crystals detects through HPLC and reaches 95.1%.
Embodiment 3
A kind of preparation technology who from sesame cake meal, obtains high purity sesamin, concrete steps are:
(1) be raw material with the solid substance sesame cake meal, sesame cake meal is pulverized with pulverizer, cross 100 mesh sieves, accurately take by weighing 500g, add the 1800ml normal hexane, 40 ℃ of water-bath 3h, middle constantly the stirring extracted;
(2) filter, filtrate is evaporated with Rotary Evaporators and is removed normal hexane and obtain oil-like extracts (sesame oil), and (oil-like extracts: ethyl acetate g/ml) adds ethyl acetate, at 25 ℃ of stirring 7h down at 1: 3.2 press solid-liquid ratio;
(3) leave standstill 5h, treat layering after, get upper strata liquid and be rotated evaporation and remove ethyl acetate;
(4) add sherwood oil 30ml, 55 ℃ leave standstill 1h, filter and obtain sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added in the dehydrated alcohol, heating in water bath places 5 ℃ of refrigerators to carry out growing the grain 7h after promoting dissolving, filters then, adds anhydrous alcohol solution and 5 ℃ of refrigerator growing the grain 7h again, obtains the sesamin purified crystals after repeating 2 times.
After testing, sesamin crude product extraction yield 87.0%; The purity of sesamin purified crystals detects through HPLC and reaches 94.6%.
Embodiment 4
A kind of preparation technology who from sesame cake meal, obtains high purity sesamin, concrete steps are:
(1) be raw material with the solid substance sesame cake meal, sesame cake meal is pulverized with pulverizer, cross 100 mesh sieves, accurately take by weighing 500g, add the 2100ml normal hexane, 55 ℃ of water-bath 2h, middle constantly the stirring extracted;
(2) filter, filtrate is evaporated with Rotary Evaporators and is removed normal hexane and obtain oil-like extracts (sesame oil), and (oil-like extracts: dehydrated alcohol g/ml) adds dehydrated alcohol, at 45 ℃ of stirring 5h down at 1: 3.5 press solid-liquid ratio;
(3) leave standstill 5-7h, treat layering after, get upper strata liquid and be rotated evaporation and remove ethanol;
(4) add sherwood oil 25ml, 50 ℃ leave standstill 1.5h, filter and obtain sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added in the dehydrated alcohol, heating in water bath places 2 ℃ of refrigerators to carry out growing the grain 4h after promoting dissolving, filters then, adds anhydrous alcohol solution and 2 ℃ of refrigerator growing the grain 4h again, obtains the sesamin purified crystals after repeating 2 times.
After testing, sesamin crude product extraction yield 87.8%; The purity of sesamin purified crystals detects through HPLC and reaches 95.0%.
Embodiment 5
A kind of preparation technology who from sesame cake meal, obtains high purity sesamin, concrete steps are:
(1) be raw material with the solid substance sesame cake meal, sesame cake meal is pulverized with pulverizer, cross 60 mesh sieves, accurately take by weighing 400g, add the 2000ml normal hexane, 50 ℃ of water-bath 2h, middle constantly the stirring extracted;
(2) filter, filtrate is evaporated with Rotary Evaporators and is removed normal hexane and obtain oil-like extracts (sesame oil), and (oil-like extracts: anhydrous methanol g/ml) adds anhydrous methanol, at 30 ℃ of stirring 5h down at 1: 3.3 press solid-liquid ratio;
(3) leave standstill 6h, treat layering after, get upper strata liquid and be rotated evaporation and remove methyl alcohol;
(4) add sherwood oil 25ml, 55 ℃ leave standstill 2h, filter and obtain sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added in the anhydrous methanol, heating in water bath places 3 ℃ of refrigerators to carry out growing the grain 5h after promoting dissolving, filters then, adds anhydrous methanol dissolving and 3 ℃ of refrigerator growing the grain 5h again, obtains the sesamin purified crystals after repeating 2 times.
After testing, sesamin crude product extraction yield 87.6%; The purity of sesamin purified crystals detects through HPLC and reaches 94.5%.
Embodiment 6
A kind of preparation technology who from sesame cake meal, obtains high purity sesamin, concrete steps are:
(1) be raw material with the solid substance sesame cake meal, sesame cake meal is pulverized with pulverizer, cross 120 mesh sieves, accurately take by weighing 500g, add the 2000ml normal hexane, 45 ℃ of water-bath 2h, middle constantly the stirring extracted;
(2) filter, filtrate is evaporated with Rotary Evaporators and is removed normal hexane and obtain oil-like extracts (sesame oil), and (oil-like extracts: anhydrous methanol g/ml) adds anhydrous methanol, at 80 ℃ of stirring 4h down at 1: 5.5 press solid-liquid ratio;
(3) leave standstill 5h, treat layering after, get upper strata liquid and be rotated evaporation and remove methyl alcohol;
(4) add sherwood oil 25ml, 48 ℃ leave standstill 2h, filter and obtain sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added in the dehydrated alcohol, heating in water bath places 4 ℃ of refrigerators to carry out growing the grain 5h after promoting dissolving, filters then, adds anhydrous alcohol solution and 4 ℃ of refrigerator growing the grain 5h again, obtains the sesamin purified crystals after repeating 2 times.
After testing, sesamin crude product extraction yield 88.2%; The purity of sesamin purified crystals detects through HPLC and reaches 94.8%.
Embodiment 7
A kind of preparation technology who from sesame cake meal, obtains high purity sesamin, concrete steps are:
(1) be raw material with the solid substance sesame cake meal, sesame cake meal is pulverized with pulverizer, cross 60 mesh sieves, accurately take by weighing 500g, add the 2500ml normal hexane, 47 ℃ of water-bath 2h, middle constantly the stirring extracted;
(2) filter, filtrate is evaporated with Rotary Evaporators and is removed normal hexane and obtain oil-like extracts (sesame oil), and (oil-like extracts: anhydrous methanol g/ml) adds anhydrous methanol, at 65 ℃ of stirring 4h down at 1: 1.5 press solid-liquid ratio;
(3) leave standstill 5h, treat layering after, get upper strata liquid and be rotated evaporation and remove methyl alcohol;
(4) add sherwood oil 30ml, 55 ℃ leave standstill 0.5h, filter and obtain sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added in the anhydrous methanol, heating in water bath places 3 ℃ of refrigerators to carry out growing the grain 5h after promoting dissolving, filters then, adds anhydrous methanol dissolving and 3 ℃ of refrigerator growing the grain 5h again, obtains the sesamin purified crystals after repeating 2 times.
After testing, sesamin crude product extraction yield 87.3%; The purity of sesamin purified crystals detects through HPLC and reaches 94.4%.
Embodiment 8
A kind of preparation technology who from sesame cake meal, obtains high purity sesamin, concrete steps are:
(1) be raw material with the solid substance sesame cake meal, sesame cake meal is pulverized with pulverizer, cross 100 mesh sieves, accurately take by weighing 500g, add the 2000ml normal hexane, 45 ℃ of water-bath 2h, middle constantly the stirring extracted;
(2) filter, filtrate is evaporated with Rotary Evaporators and is removed normal hexane and obtain oil-like extracts (sesame oil), and (oil-like extracts: anhydrous methanol g/ml) adds anhydrous methanol, at 70 ℃ of stirring 6h down at 1: 2 press solid-liquid ratio;
(3) leave standstill 7h, treat layering after, get upper strata liquid and be rotated evaporation and remove methyl alcohol;
(4) add sherwood oil 25ml, 53 ℃ leave standstill 1.5h, filter and obtain sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added in the dehydrated alcohol, heating in water bath places 4 ℃ of refrigerators to carry out growing the grain 7h after promoting dissolving, filters then, adds anhydrous alcohol solution and 4 ℃ of refrigerator growing the grain 7h again, obtains the sesamin purified crystals after repeating 2 times.
After testing, sesamin crude product extraction yield 87.9%; The purity of sesamin purified crystals detects through HPLC and reaches 95.2%.
Above-mentioned detailed description of this a kind of preparation technology who obtains high purity sesamin from sesame cake meal being carried out with reference to embodiment; be illustrative rather than determinate; can list several embodiment according to institute's limited range; therefore in the variation and the modification that do not break away under the general plotting of the present invention, should belong within protection scope of the present invention.

Claims (1)

1. preparation technology who from sesame cake meal, obtains high purity sesamin, it is characterized in that: concrete steps are:
(1) be raw material with the solid substance sesame cake meal, sesame cake meal is pulverized with pulverizer, cross 120 mesh sieves, accurately take by weighing 500g, add the 2000ml normal hexane, 45 ℃ of water-bath 2h, middle constantly the stirring extracted;
(2) filter, filtrate is evaporated with Rotary Evaporators and is removed normal hexane and obtain oil-like extracts sesame oil, and by the solid-liquid ratio oil-like extracts: anhydrous methanol is 1: 4.5g/ml adds anhydrous methanol, at 40 ℃ times stirring 6h;
(3) leave standstill 7h, treat layering after, get upper strata liquid and be rotated evaporation and remove methyl alcohol;
(4) add sherwood oil 20ml, 45 ℃ leave standstill, and airtight mixing 0.5h filters and obtains sedimentary sesamin crude product;
(5) sesamin crude product in the step (4) is added anhydrous methanol, heating in water bath places 4 ℃ of refrigerators to carry out growing the grain 7h after promoting dissolving, filters then, adds the anhydrous methanol dissolving again and in 4 ℃ of refrigerator growing the grain 7h, obtains the sesamin purified crystals after repeating 2 times.
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CN103896956B (en) * 2014-03-06 2016-03-30 河南省农业科学院芝麻研究中心 A kind of method extracting sesamin from sesame seed coat
CN104177370B (en) * 2014-09-04 2016-10-05 陕西源邦生物技术有限公司 A kind of method preparing high-load sesamin from sesame seed meal
CN104292238A (en) * 2014-10-15 2015-01-21 河南省农业科学院芝麻研究中心 Method for extracting sesamin from sesame cake meals
CN104817566A (en) * 2015-04-03 2015-08-05 安徽新桥工贸有限责任公司 Sesamin separation extraction method
CN112661767B (en) * 2020-12-04 2022-06-03 武汉轻工大学 Method for synchronously preparing sesame concentrated protein, sesame oil and sesamin from sesame cake meal
CN113480514B (en) * 2021-08-16 2022-07-22 内蒙古泓兴生物科技有限公司 Method for extracting sesamin
CN113717191B (en) * 2021-09-18 2024-06-11 安徽省凤阳县御膳油脂有限公司 Method for preparing sesamin by using sesame seed meal

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