CN100390188C - Preparation method of black soybean seed capsule anthocyanin - Google Patents
Preparation method of black soybean seed capsule anthocyanin Download PDFInfo
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- CN100390188C CN100390188C CNB2005100364193A CN200510036419A CN100390188C CN 100390188 C CN100390188 C CN 100390188C CN B2005100364193 A CNB2005100364193 A CN B2005100364193A CN 200510036419 A CN200510036419 A CN 200510036419A CN 100390188 C CN100390188 C CN 100390188C
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Abstract
The present invention discloses a preparing method of anthocyanin of a black soybean seed hull, which comprise the following steps: 1 the black soyabean seed hull is peeled as raw material; 2 the black soyabean seed hull is crumbled into fine powder by a micronizer, and micro powder of the black soyabean seed hull is processed by a microwave machine; 3 the anthocyanin of the fine-crumbled black soyabean seed hull is leached by using 60 to 80% of ethanol as dissolvent; 4 anthocyanin leaching liquor of the black soyabean seed hull obtained from step 3 is concentrated in a vacuum way until the concentration of a solid object of the extracting solution reaches over 40%; 5 leaching concentrated solution obtained from step 4 is processed by adopting derosination, macroporous adsorbente resin adsorption and 65 to 75% of ethanol detachment, and the purified anthocyanin extracting solution of the black soyabean seed hull is obtained; 6 the extracting solution obtained from step 5 is concentrated in a vacuum way again until the concentration of the solid object reaches to more than 60%, and the anthocyanin of the black soyabean seed hull can be obtained by adopting freeze drying. The present invention has the advantages of simple manufacturing process and high stability of the anthocyanin.
Description
Technical field
The present invention relates to the preparation method of a kind of black soybean coat anthocyanogen.
Background technology
Semen sojae atricolor is one of agricultural resource of traditional dietotherapeutic, among the peoplely since ancient times enriches blood, invigorates blood circulation and the record of blacking hair and nourishing face with regard to useful Semen sojae atricolor, and this prompting Semen sojae atricolor has higher researching value and potentiality to be exploited.Modern nutriology research finds that further the natural anthocyanin class material in the black-food has the extremely strong active oxygen that prevents to endanger and antioxygenation, can eliminate the polyradical of crossing that produces in the organism metabolism process, has functions such as delaying senility, prevent various diseases.Black soybean coat is rich in the anthocyanin class compound, is the important source of natural pigment.Forefathers have carried out big quantity research to the chemical structure and the stability of black soybean coat pigment, see Xiao Xiang etc. the black-food pigment is removed active oxygen effect and anti-oxidant activity [J] medicine biotechnology, 2000,7 (2): 112-115., show that its main component is Root of Rocket Consolida-3-glucoside and Minor centaury-3-glucoside, but its less stable.
Existing preparation method about anthocyanogen mainly selects suitable solvent to extract according to the distribution position of anthocyanogen in the raw material.Its core technology mainly be solve that stability, the solvent of anthocyanogen in leaching process selected, purification process is with problems such as drying modes, purpose be to keep to greatest extent anthocyanogen stability, improve yield and the purity of anthocyanogen.
Summary of the invention
The object of the present invention is to provide that technology is simple, the preparation method of the black soybean coat anthocyanogen of anthocyanogen good stability.
For achieving the above object, may further comprise the steps:
1, strips with decorticator and account for Semen sojae atricolor to weigh 2%～4% black soybean coat be raw material;
2, adopt supper micron mill that black soybean coat is ground into 300～400 purpose fine powders; Handle black soybean coat micro mist, smudge cells with microwave machine.
3, make solvent with 60～80% ethanol fine black soybean coat anthocyanogen is carried out lixiviate;
4, the black soybean coat anthocyanogen vat liquor to gained in the step 3 carries out vacuum concentration, reaches more than 40% until the solid concentration of extracting solution;
5, take the alcohol desorption of degreasing, absorption with macroporous adsorbent resin and 65～75% to handle to the black soybean coat anthocyanogen lixiviate concentrated solution of gained in the step 4, the black soybean coat anthocyanogen extracting solution of purifying;
6, the black soybean coat anthocyanogen extracting solution to the purifying of gained in the step 5 carries out vacuum concentration once more, reaches 60% when above until solid concentration, adopts lyophilize to get the black soybean coat anthocyanogen again.
Adopt microwave frequency 2450MHz, microwave power 12～20kw, time 40～60s among the present invention in the step 2.
The detailed process of step 3 is among the present invention: with containing concentration is that 0.05～0.1% ascorbic 60～80% ethanol are made solvent, black soybean coat micro mist after pulverizing is pressed solid-liquid ratio 1: 4～6,50～70 ℃ of temperature, extraction time 1～2 hour, lixiviate number of times are 2～3 times;
In the step 5 sherwood oil is adopted in the skimming treatment of extracting solution among the present invention, the model that macroporous adsorbent resin is selected for use is NKA-II.
Among the present invention in step 3 and the step 5 vacuum tightness in the vacuum Concentrating Process be 0.09Mpa, temperature is 50～55 ℃.
Vacuum tightness 10～30Pa during lyophilize in the step 6 among the present invention, temperature is lower than-30 ℃, time of drying 20～24h.
The present invention compared with prior art has following advantage:
1, since the anthocyanogen more than 99% in the Semen sojae atricolor be distributed in and account for Semen sojae atricolor and weigh in 2%～4% the Testa sojae atricolor, choose and account for Semen sojae atricolor to weigh 2%～4% Testa sojae atricolor be the material extraction anthocyanogen, with be that material is compared with whole grain Semen sojae atricolor, can reduce the usage quantity of extracting solvent, save cost, raise the efficiency.
2, because black soybean coat is hard, directly use the yield of solvent extraction anthocyanogen low, extraction time is long, and is big to the loss of anthocyanogen, adopts supper micron mill that black soybean coat is ground into 300～400 purpose fine powders; Handle the Testa sojae atricolor micro mist with microwave machine, smudge cells can shorten extraction time, improves yield of getting anthocyanogen and the loss of anthocyanogen greatly.
Find through contrast experiment's (table 1), it is obviously different that the anthocyanogen crude product of variable grain fineness Testa sojae atricolor extracts yield, along with continuing to increase of fineness, the anthocyanogen crude product extracts yield and obviously improves, and when 40 orders were following, it was minimum to extract yield, it is medium to extract yield during 80～240 orders,, extract yield and significantly improve, but the difference between 320 orders and 400 orders is not obvious when above to 320 orders.So the present invention is selected black soybean coat is ground into 300～400 purpose fine powders.
Through the same discovery of contrast experiment's (table 2), the black soybean coat powder is after microwave treatment, and the anthocyanogen crude product extracts yield and obviously improves, and the difference between being untreated reaches conspicuous level (P＜0.05).Similarly, different extraction times, the look valency of anthocyanogen crude product there is considerable influence, in 1～2 hour, its look valency is higher, and more than 2 hours, the look valency obviously descends, and difference reaches conspicuous level (P＜0.05) (table 3).
The anthocyanogen crude product of table 1 variable grain fineness Testa sojae atricolor extracts yield
The extraction yield of anthocyanogen crude product in the table 2 different treatment Testa sojae atricolor
Table 3 different extraction times are to the influence (60 ℃) of Testa sojae atricolor anthocyanogen look valency
3, make solvent with containing 0.05～0.1% ascorbic 60～80% alcoholic acid, can increase the stripping of anthocyanogen in the raw material to greatest extent, improve the yield of anthocyanogen crude product; Because vitamins C can make extraction solution keep sour environment, help keeping the stability of anthocyanogen simultaneously.
Through experiment, be index with the anthocyanogen, primary extraction yield can reach 72.18%, secondaryly reaches 12.93%, and secondary adds up to more than 85%, shows that the extraction effect of conditions such as this ethanol and temperature is comparatively ideal.The results are shown in Table 4.
The yield of table 4 Testa sojae atricolor anthocyanogen extract
4, for improving the purity of Semen sojae atricolor pattern glucoside extract, adopt degreasing and absorption with macroporous adsorbent resin to handle the technology that is further purified, have advantages such as operation is simple, cost is low, efficient is high, good stability extract.
Studies show that, because vat liquor is an ethanolic soln, contain some apolar substances in vat liquor, with the purification with macroreticular resin target compound time, they may produce some adverse influences to it, so need vat liquor is carried out skimming treatment.From the degreasing effect of sherwood oil, normal hexane and 3 kinds of organic solvents of toluene as can be known, minimum to anthocyanogen influence in the extract with petroleum ether degreasing, rate of loss is 8.1%, is 11.2% with the rate of loss of normal hexane, and the rate of loss of usefulness toluene is then bigger, is 22.7%.Learn check by statistics, difference was not remarkable between sherwood oil and normal hexane were handled, and and the difference between not skimming treatment and O for toluene reach conspicuous level (P＜0.05).Therefore, degreasing can be selected sherwood oil for use to Semen sojae atricolor pattern glucoside extract.
By macroporous adsorbent resin Static Adsorption test-results (table 5) as seen, the macroporous resin of different model is obviously different to the adsorption effect of Semen sojae atricolor pattern glucoside extract, and is in selected 8 kinds of resins, best with the effect of NKA-II.
The macroporous adsorbent resin separating effective ingredient mainly is a reversibility (promptly separating absorption) of utilizing its absorption.Because resin polarity difference, the power of adsorption also has difference, and the desorb difficulty or ease are also different, and therefore, having higher desorption efficiency also is the important step of resin screening.Desorption experiment result's (table 6) by Static Adsorption test as can be known, NKA-II has higher desorption efficiency, 70% ethanol is easy to from resin the anthocyanogen desorb be got off.
The different macroporous adsorbent resins of table 5 are to the adsorptive power of Semen sojae atricolor pattern glucoside extract
The different strippants of table 6 are to the desorption efficiency of Semen sojae atricolor pattern glucoside extract
Embodiment
Embodiment one
1, selects " Semen sojae atricolor is drawn No. 1 in Guangdong " kind 100Kg for use, strip and account for Semen sojae atricolor to weigh 3% black soybean coat be raw material;
2, adopt supper micron mill that black soybean coat is ground into 320 purpose fine powders; Handle black soybean coat micro mist, smudge cells with microwave machine.Microwave frequency 2450MHz, microwave power 20kw, time 40s;
3, make solvent with containing 0.1% ascorbic 70% ethanol, above-mentioned black soybean coat micro mist was pressed solid-liquid ratio 1: 5,55 ℃ of temperature, extraction time 2 hours, lixiviate number of times are 2 times;
4, the Semen sojae atricolor pattern glycosides vat liquor to gained in the step 3 carries out vacuum concentration, and vacuum tightness is 0.09Mpa, and temperature is 50 ℃, reaches more than 40% until the solid concentration of extracting solution;
5, the Semen sojae atricolor pattern glycosides lixiviate concentrated solution of gained in the step 4 is adopted petroleum ether degreasing, and be the absorption with macroporous adsorbent resin of NKA-II, the alcohol desorption with 65%, Semen sojae atricolor pattern glycosides extracting solution that must purifying with model;
6, the Semen sojae atricolor pattern glycosides extracting solution to the purifying of gained in the step 5 carries out vacuum concentration, vacuum tightness is 0.09Mpa, temperature is 55 ℃, solid concentration reaches 60% when above, adopt lyophilize to get Semen sojae atricolor pattern glucoside extract, vacuum tightness during lyophilize is 15Pa, and temperature is-25 ℃, time of drying 24h.
Embodiment two
1, selects " Semen sojae atricolor is drawn No. 1 in Guangdong " kind 100Kg for use, strip and account for Semen sojae atricolor to weigh 4% black soybean coat be raw material;
2, adopt supper micron mill that black soybean coat is ground into 400 purpose fine powders; Handle black soybean coat micro mist, smudge cells with microwave machine.Microwave frequency 2450MHz, microwave power 12kw, time 60s;
3, make solvent with containing 0.08% ascorbic 60% ethanol, above-mentioned black soybean coat micro mist was pressed solid-liquid ratio 1: 6,60 ℃ of temperature, extraction time 1.5 hours, lixiviate number of times are 3 times;
4, the Semen sojae atricolor pattern glycosides vat liquor to gained in the step 3 carries out vacuum concentration, and vacuum tightness is 0.09Mpa, and temperature is 55 ℃, reaches more than 40% until the solid concentration of extracting solution;
5, the Semen sojae atricolor pattern glycosides lixiviate concentrated solution of gained in the step 4 is adopted petroleum ether degreasing, and be the absorption with macroporous adsorbent resin of NKA-II, the alcohol desorption with 70%, Semen sojae atricolor pattern glycosides extracting solution that must purifying with model;
6, the Semen sojae atricolor pattern glycosides extracting solution to the purifying of gained in the step 5 carries out vacuum concentration, vacuum tightness is 0.09Mpa, temperature is 50 ℃, solid concentration reaches 60% when above, adopt lyophilize to get Semen sojae atricolor pattern glucoside extract, vacuum tightness during lyophilize is 25Pa, and temperature is-30 ℃, time of drying 20h.
Embodiment three
1, selects " Semen sojae atricolor is drawn No. 1 in Guangdong " kind 100Kg for use, strip and account for Semen sojae atricolor to weigh 2% black soybean coat be raw material;
2, adopt supper micron mill that black soybean coat is ground into 400 purpose fine powders; Handle black soybean coat micro mist, smudge cells with microwave machine.Microwave frequency 2450MHz, microwave power 15kw, time 50s;
3, make solvent with containing 0.05% ascorbic 80% ethanol, above-mentioned black soybean coat micro mist was pressed solid-liquid ratio 1: 4,70 ℃ of temperature, extraction time 1 hour, lixiviate number of times are 3 times;
4, the Semen sojae atricolor pattern glycosides vat liquor to gained in the step 3 carries out vacuum concentration, and vacuum tightness is 0.09Mpa, and temperature is 55 ℃, reaches more than 40% until the solid concentration of extracting solution;
5, the Semen sojae atricolor pattern glycosides lixiviate concentrated solution of gained in the step 4 is adopted petroleum ether degreasing, and be the absorption with macroporous adsorbent resin of NKA-II, the alcohol desorption with 75%, Semen sojae atricolor pattern glycosides extracting solution that must purifying with model;
6, the Semen sojae atricolor pattern glycosides extracting solution to the purifying of gained in the step 5 carries out vacuum concentration, vacuum tightness is 0.09Mpa, temperature is 50 ℃, solid concentration reaches 60% when above, adopt lyophilize to get Semen sojae atricolor pattern glucoside extract, vacuum tightness during lyophilize is 30Pa, and temperature is-28 ℃, time of drying 22h.
Claims (6)
1. the preparation method of a black soybean coat anthocyanogen is characterized in that may further comprise the steps:
(1) strips with decorticator and account for Semen sojae atricolor to weigh 2%～4% black soybean coat be raw material;
(2) black soybean coat is carried out the broken and cytoclasis processing of micro mist;
(3) be that 0.05～0.1% ascorbic 60～80% ethanol is made solvent fine black soybean coat anthocyanogen is carried out lixiviate with containing concentration;
(4) the black soybean coat anthocyanogen vat liquor to gained in the step (3) carries out vacuum concentration, reaches more than 40% until the solid concentration of extracting solution;
(5) take the alcohol desorption of degreasing, absorption with macroporous adsorbent resin and 65～75% to handle to the black soybean coat anthocyanogen lixiviate concentrated solution of gained in the step (4), the black soybean coat anthocyanogen extracting solution of purifying;
(6) the black soybean coat anthocyanogen extracting solution to the purifying of gained in the step (5) carries out vacuum concentration once more, reaches 60% when above until solid concentration, adopts lyophilize to get the black soybean coat anthocyanogen again.
2. the preparation method of black soybean coat anthocyanogen according to claim 1 is characterized in that adopting in the step (2) supper micron mill that black soybean coat is ground into 300～400 purpose fine powders; Handle black soybean coat micro mist smudge cells, microwave frequency 2450MHz, microwave power 12～20kw, time 40～60s with microwave machine.
3. the preparation method of black soybean coat anthocyanogen according to claim 1, the detailed process that it is characterized in that step (3) is: the black soybean coat micro mist after will pulverizing is pressed solid-liquid ratio 1: 4～6,50～70 ℃ of temperature, extraction time 1～2 hour, lixiviate number of times are 2～3 times.
4. the preparation method of black soybean coat anthocyanogen according to claim 1 is characterized in that sherwood oil is adopted in the skimming treatment to extracting solution in the step (5), and the model that macroporous adsorbent resin is selected for use is NKA-II.
5. the preparation method of black soybean coat anthocyanogen according to claim 1 is characterized in that the vacuum tightness in the vacuum Concentrating Process is 0.09Mpa in step (4) and the step (6), and temperature is 50～55 ℃.
6. the preparation method of black soybean coat anthocyanogen according to claim 1, the vacuum tightness 10～30Pa when it is characterized in that lyophilize in the step (6), temperature is lower than-30 ℃, time of drying 20～24h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2008083513A1 (en) | 2006-12-13 | 2008-07-17 | Beijing Gingko-Group Biological Technology Co., Ltd. | Black soybean hull extract and process for preparation and use thereof |
| CN101161110B (en) * | 2007-11-19 | 2010-12-08 | 嘉应学院 | Method for extracting anthocyanin from lunar incense fructification |
| US8883230B2 (en) * | 2008-02-25 | 2014-11-11 | National Yang-Ming University | Use of black soybean for treating ophthalmic diseases |
| CN101250206B (en) * | 2008-03-26 | 2011-05-25 | 天津市尖峰天然产物研究开发有限公司 | Effective part containing cyaniding 3-O-glucoside as well as preparation method and use thereof |
| CN102258165B (en) * | 2010-09-08 | 2012-10-03 | 李德海 | Bog bilberry anthocyanin tablet and preparation method thereof |
| CN102993145B (en) * | 2011-09-19 | 2015-06-03 | 北大方正集团有限公司 | Lovastatin extraction and purification method |
| CN102631002B (en) * | 2012-05-15 | 2013-06-05 | 安徽燕之坊食品有限公司 | Functional beverage granule |
| CN102775454A (en) * | 2012-08-06 | 2012-11-14 | 宁波杰顺生物科技有限公司 | Extractive of blackcurrant fruit anthocyanin |
| CN104761596A (en) * | 2015-02-01 | 2015-07-08 | 云南农业大学 | Method for preparing anthocyanin standard substance |
| CN107988011B (en) * | 2017-12-27 | 2021-08-27 | 孝感麻糖米酒有限责任公司 | Black glutinous rice wine and preparation method thereof |
| CN110180216B (en) * | 2019-06-11 | 2021-05-25 | 南京农业大学 | Method and device for extracting and purifying anthocyanin by ultrasonic-enhanced fluidized bed type resin adsorption-desorption |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1040042A (en) * | 1988-08-05 | 1990-02-28 | 谢静波 | The extracting method of natural brown pigment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040042A (en) * | 1988-08-05 | 1990-02-28 | 谢静波 | The extracting method of natural brown pigment |
Non-Patent Citations (1)
| Title |
|---|
| 黑豆色素的提取工艺，理化性质和应用. 王海棠等.洛阳工学院学报，第19卷第2期. 1998 * |
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Effective date of registration: 20160303 Address after: 510610 Tianhe District, Guangzhou, Dongguan, Zhuang Zhuang Road, No. 1, No. 133, Patentee after: Sericulture & Agri-Food Research Institute, GAAS Address before: Five 510640 mountain road, Guangzhou, Guangdong, Tianhe District Patentee before: Research Institute of Agricultural Biological Technology of GAAS |