CN101906303B - Method for extracting natural antioxidant from star anises or star anise residues - Google Patents
Method for extracting natural antioxidant from star anises or star anise residues Download PDFInfo
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- CN101906303B CN101906303B CN 201010232709 CN201010232709A CN101906303B CN 101906303 B CN101906303 B CN 101906303B CN 201010232709 CN201010232709 CN 201010232709 CN 201010232709 A CN201010232709 A CN 201010232709A CN 101906303 B CN101906303 B CN 101906303B
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Abstract
The invention belongs to methods for extracting a natural antioxidant from star anises or star anise residues. The natural star anise antioxidant is obtained by extracting the star anises or the star anise residues by using water or an organic solvent or a mixed solvent of the water and the organic solvent. The natural star anise antioxidant extracted by using the method is a natural product and has no toxicity and good oxidation resistance, and compared with the vitamin C as a natural antioxidant, the natural star anise antioxidant has obviously advantages on the antioxidant activity. The invention not only sufficiently utilizes the star anises and the star anise residues remained after products such as essential oil, and the like are extracted, but also has lower raw material cost, simple extraction process and wide application prospect.
Description
Technical field
The present invention relates to the extraction of natural antioxidants, particularly from anistree or anistree residue, extract the method for natural antioxidants.
Background technology
Anistree, formal name used at school Illicium verum, another name star anise, Chinese anise (Guangxi), belong to the Magnoliaceae Illicium, originate in Southwestern Kwangsi, China, existing Guangxi, Guangdong, Guizhou, Yunnan and the south Fujian that mainly is distributed in China, there is a small amount of cultivation in Taiwan, also there is certain output in external Vietnam, is the precious economic tree of China's south subtropics distinctive " integration of drinking and medicinal herbs "; Octagonal fruit and star aniseed oil are the important source material of good seasonings, makeup and pharmaceuticals, are widely used in the industries such as food, light industry and medicine industry.At present both at home and abroad to the research of star anise, the separation that mainly concentrates on the chemical composition of anise tree volatile oil and shikimic acid with identify upper, existing a large amount of research papers and Patent Application Publication.In the product of anistree exploitation, the yield of extracting volatile oil from anise is about 7%～11% at present, and shikimic acid content is 4%～7%, and to other, the research of the extraction of the anise more than 80% residuum is few, utilizes still less.
Food, beverage, cosmetic industry all need to add antioxidant.There is larger problem in synthetized oxidation preventive agent aspect food safety, be the focus of food, beverage, the exploitation of cosmetic industry Recent study to the research of natural plant antioxidant both at home and abroad, but anistree antioxidant property research also has not been subject to enough attention.A.Padmashree, the people such as N.Roopa are once on " Food Chemistry " the 104th phase P59-66 in 2007, delivered " Star-anise (Illium verum) and blackcaraway (Carum nigrum) as natural antioxidants " literary composition, its result of study shows that the Fructus Anisi Stellati oil resin has oxidation-resistance.The people such as Wang Qin are in " China Condiment " the 3rd phase P38-49 in 2007, delivered the article of " Study on chemicalcomponent analyzed by GC-MS and antioxidation of star anise extracts ", report that it has carried out the anti-oxidant research of supercritical extract and organic solvent extraction thing, point out that anise tree volatile oil and oleo-resinous composition possess certain oxidation-resistance.Therefore carry out the research of from anistree and anistree residue, extracting natural antioxidants, to improving anistree comprehensive utilization, there is important economic worth and social benefit.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of extracting natural antioxidants from anistree or anistree residue.
The present invention solves the problems of the technologies described above with following technical scheme:
The step of extracting natural antioxidants from anise is:
(1) using water when extracting solvent:
Step 1: add to anistree dry powder the water that weightmeasurement ratio is 1: 5～40, carry out wet distillation, the distillation mode is water distillation, and distillation time is 2.5h;
Step 2: after collecting aniseed essential oil, by the anistree aqueous solution filtering separation after extracting, solution evaporation is concentrated, obtains the medicinal extract thing, and drying, make anistree natural antioxidants 1;
Step 3: by the anistree residue of step 2, then, according to step 1,2 operations, extract temperature from room temperature to the water boiling temperature, solids is dried and is made anistree natural antioxidants 2.
When needs are further purified anistree natural antioxidants 1 or anistree natural antioxidants 2, proceed following step:
Step 4: anistree natural antioxidants 1 or anistree natural antioxidants 2 are used water dissolution, then adopt solvent precipitation or ion exchange resin or macroporous adsorbent resin or silica gel chromatography or polymeric amide chromatogram or the separation methods such as gel chromatography or high performance liquid chromatography to carry out purifying, obtain anistree natural antioxidants 3.
(2) using organic solvent when extracting solvent:
Step 1: to anistree dry powder, add the organic solvent that weightmeasurement ratio is 1: 5～40, heating and refluxing extraction 2h;
Step 2: the anistree solution suction filtration after extracting, solution is concentrated, obtains the medicinal extract thing, and drying, make anistree natural antioxidants 4.
Step 3: after the anistree residue drying that step 2 is obtained, then, according to step 1,2 operations, extract temperature from room temperature to the solution boiling temperature.Make anistree residue natural antioxidants 5.
The organic solvent that the present invention uses comprises: methyl alcohol, ethanol, propyl alcohol, butanols, acetone, ether, sherwood oil, hexanaphthene etc.
(3) using organic solvent-water mixed solvent when extracting solvent:
Step 1: add the mixed solvent of organic solvent-water that weightmeasurement ratio is 1: 5～40 to anistree dry powder, it is 30～90% that the organic solvent in mixed solvent accounts for volume percent, heating and refluxing extraction 2h;
Step 2: the anistree solution suction filtration after extracting, the clear liquid concentrated by rotary evaporation, obtain the medicinal extract thing, and drying makes anistree natural antioxidants 4.
Step 3: after the anistree residue drying that step 2 is obtained, then, according to step 1,2 operations, extract temperature from room temperature to the solution boiling temperature.Make anistree residue natural antioxidants 5.
The organic solvent that the present invention uses comprises: methyl alcohol, ethanol, propyl alcohol, butanols, acetone, ether, sherwood oil, hexanaphthene.
The step of extracting natural antioxidants from anistree residue is:
(1) using water when extracting solvent:
Add to anistree residue the water that weightmeasurement ratio is 1: 5～40, carry out wet distillation, the distillation mode is water distillation, and distillation time is 2.5h; By the anistree aqueous solution filtering separation after extracting, solution evaporation is concentrated, obtains the medicinal extract thing, and drying, make anistree natural antioxidants 2.
When needs are further purified anistree natural antioxidants, anistree natural antioxidants 1 and/or 2 is used to water dissolution, then adopt solvent precipitation or ion exchange resin or macroporous adsorbent resin or silica gel chromatography or polymeric amide chromatogram or the separation methods such as gel chromatography or high performance liquid chromatography to carry out purifying, obtain anistree natural antioxidants 3.
(2) using organic solvent when extracting solvent:
By after anistree residue drying, add the organic solvent that weightmeasurement ratio is 1: 5～40, heating and refluxing extraction 2h; By the anistree solution suction filtration after extracting, solution is concentrated, obtains the medicinal extract thing, and drying, make anistree natural antioxidants 5.
The organic solvent used is methyl alcohol, ethanol, propyl alcohol, butanols, acetone, ether, sherwood oil, hexanaphthene.
(3) using organic solvent-water mixed solvent when extracting solvent:
By after anistree residue drying, add the mixed solvent of organic solvent-water that weightmeasurement ratio is 1: 5～40, it is 30～90% that the organic solvent in mixed solvent accounts for volume percent, heating and refluxing extraction 2h; By the anistree solution suction filtration after extracting, the clear liquid concentrated by rotary evaporation, obtain the medicinal extract thing, and drying makes anistree natural antioxidants 5.
The organic solvent used is methyl alcohol, ethanol, propyl alcohol, butanols, acetone, ether, sherwood oil, hexanaphthene.
Extract anistree natural antioxidants by method of the present invention, product is natural product, nontoxic, have good antioxidant property, anti-oxidant activity and natural antioxidants vitamins C (Vc) relatively, have clear superiority, not only take full advantage of the anistree residue of the anistree residuum with extracting the wet goods product that volatilizees, and raw materials cost is lower, extraction process is simple, has a extensive future.
Embodiment
In technology of the present invention, can using water as extracting solvent, also can using the mixed solvent of organic solvent or organic solvent-water as extracting solvent, extract anistree natural antioxidants from anistree or anistree residue.The antioxidant effect of the anistree natural antioxidants of gained will exceed several times than the natural antioxidants vitamins C.
Prepare the finished product of anistree natural antioxidants by method of the present invention after, with following method, measure its antioxidant effect:
Accurately pipette the star anise extract sample solution that 2mL 0.100mmol/L DPPH solution and 2mL concentration are 0.04mg/ml, shake up immediately, after lucifuge reaction 0.5h, do reference with dehydrated alcohol, with its light absorption value at the 517nm place of spectrophotometric determination (ABS), the following formula of the data obtained substitution is calculated to its inhibiting rate (SA):
Wherein: the absorbancy that Ai is DPPH solution while adding analyte sample fluid; Aj is the absorbancy of analyte sample fluid in ethanol; The absorbancy that Ao is DPPH ethanolic soln while not adding analyte sample fluid.
Relatively, result is as shown in table 1 for its anti-oxidant activity and natural antioxidants vitamins C:
The resistance of oxidation of the above-mentioned five kinds of anistree natural antioxidantss of table 1
As seen from Table 1, the anti-oxidant activity of five kinds of anistree natural antioxidantss that obtain by method of the present invention is all strong than vitamins C anti-oxidant activity, can be applied to the fields such as food, beverage, makeup fully.
Embodiment 1
Take the anistree dry powder of 100g, add 500mL water, carry out wet distillation, the distillation mode is water distillation, 100 ℃ of distillation temperatures, and distillation time is 2.5h.After collecting aniseed essential oil, the anistree aqueous solution after extracting is centrifugal, and the clear liquid concentrated by rotary evaporation, obtain the medicinal extract thing, and drying makes anistree water extraction natural antioxidants 1, and quality is 33g, and yield is 33%.By after above-mentioned anistree slag drying, repeat above-mentioned steps and make anistree slag antioxidant 2.Take 5g natural antioxidants 1, with the 50mL water dissolution, adding 3 times of volumes is the dehydrated alcohol of 150mL, puts into refrigerator, standing over night, and after precipitation is complete, the filtering separation precipitation, the clear liquid concentrated by rotary evaporation, obtain the medicinal extract thing, and drying makes anistree natural antioxidants 3.
Utilize DPPH free radical analytical method to be measured the antioxidant property of natural antioxidants 1, natural antioxidants 2 and natural antioxidants 3, when being 0.02mg/mL, the concentration that mensuration obtains each extract to the inhibiting rate of DPPH free radical, and compares with the inhibiting rate of the natural antioxidants vitamins C (Vc) of same concentration.The antioxidant property that extracts respectively the natural antioxidants 1, natural antioxidants 2 and the natural antioxidants 3 that obtain from anistree and anistree residue is all strong than Vc, is respectively 2.3,3.8,3.2 times of Vc.
Embodiment 2
Take the anistree dry powder of 15g, add 80% ethanolic soln 450mL with the weightmeasurement ratio of 1: 30, backflow 2h, the anistree alcoholic solution after extracting is centrifugal, and the clear liquid concentrated by rotary evaporation, obtain the medicinal extract thing, and drying makes natural antioxidants 4, and quality is 4.6g, and yield is 30%.By after above-mentioned anistree slag drying, according to above-mentioned steps, make anistree natural antioxidants 5.
Utilize DPPH free radical analytical method to be measured the antioxidant property of natural antioxidants 4 and natural antioxidants 5, when being 0.02mg/mL, the concentration that mensuration obtains each extract to the inhibiting rate of DPPH free radical, and compares with the inhibiting rate of the natural antioxidants vitamins C (Vc) of same concentration.The antioxidant property that extracts respectively the natural antioxidants 4 that obtains and natural antioxidants 5 from anistree and anistree residue is all strong than Vc, is respectively 2.6,3.5 times of Vc.
Embodiment 3
Take the anistree dry powder of 15g, with the weightmeasurement ratio of 1: 20, add 95% edible ethanol, backflow 2h, filter the alcoholic solution after extracting, and the solution distillation and concentration, obtain the medicinal extract thing, and drying makes anistree natural antioxidants 4, and quality is 4.6g, and yield is 30%.Using above-mentioned anistree slag water as extracting solvent, according to above-mentioned steps, make anistree natural antioxidants 2.
Utilize DPPH free radical analytical method to be measured the antioxidant property of natural antioxidants 4 and natural antioxidants 2, when being 0.02mg/mL, the concentration that mensuration obtains each extract to the inhibiting rate of DPPH free radical, and compares with the inhibiting rate of the natural antioxidants vitamins C (Vc) of same concentration.The antioxidant property that extracts respectively the natural antioxidants 4 that obtains and natural antioxidants 2 from anistree and anistree residue is all strong than Vc, is respectively 2.6,3.8 times of Vc.
Embodiment 4
Take the anistree dry powder of 15g, with the weightmeasurement ratio of 1: 18, add acetone, backflow 2h, by the solution filter after extracting, the solution distillation and concentration, obtain the medicinal extract thing, and drying makes anistree natural antioxidants 4, and quality is 4.6g, and yield is 30%.Using above-mentioned anistree slag water as extracting solvent, according to above-mentioned steps, make anistree natural antioxidants 2.
Utilize DPPH free radical analytical method to be measured the antioxidant property of natural antioxidants 4 and natural antioxidants 2, when being 0.02mg/mL, the concentration that mensuration obtains each extract to the inhibiting rate of DPPH free radical, and compares with the inhibiting rate of the natural antioxidants vitamins C (Vc) of same concentration.The antioxidant property that extracts respectively the natural antioxidants 4 that obtains and natural antioxidants 2 from anistree and anistree residue is all strong than Vc, is respectively 2.6,3.8 times of Vc.
Embodiment 5
Take and extracted the anistree residue powder of remaining drying 15g after volatile oil, add 500mL water, carry out wet distillation, the distillation mode is water distillation, 100 ℃ of distillation temperatures, and distillation time is 2.5h.The aqueous solution after extracting is centrifugal, and the clear liquid concentrated by rotary evaporation, obtain the medicinal extract thing, and drying makes anistree natural antioxidants 2.
Utilize DPPH free radical analytical method to be measured the antioxidant property of natural antioxidants 2, when being 0.02mg/mL, the concentration that mensuration obtains extract to the inhibiting rate of DPPH free radical, and compares with the inhibiting rate of the natural antioxidants vitamins C (Vc) of same concentration.The antioxidant property that extracts the natural antioxidants 2 obtained from anistree residue is stronger than Vc, is 3.8 times of Vc.
Embodiment 6
Take and extracted the anistree residue powder of remaining drying 15g after volatile oil,, add 80% ethanolic soln 450mL with the weightmeasurement ratio of 1: 30, backflow 2h, the anistree alcoholic solution after extracting is centrifugal, the clear liquid concentrated by rotary evaporation, obtain the medicinal extract thing, drying, make natural antioxidants 5.
Utilize DPPH free radical analytical method to be measured the antioxidant property of natural antioxidants 5, when being 0.02mg/mL, the concentration that mensuration obtains extract to the inhibiting rate of DPPH free radical, and compares with the inhibiting rate of the natural antioxidants vitamins C (Vc) of same concentration.The antioxidant property that extracts the natural antioxidants 5 obtained from anistree residue is stronger than Vc, is 3.5 times of Vc.
Claims (2)
1. a method of extracting natural antioxidants from anise, it is characterized in that take the processing step of organic solvent-water mixed solvent when extracting solvent as:
Step 1: add the mixed solvent of organic solvent-water that weightmeasurement ratio is 1:5～40 to anistree dry powder, it is 30～90% that the organic solvent in mixed solvent accounts for volume percent, heating and refluxing extraction 2h;
Step 2: the anistree solution suction filtration after extracting, the clear liquid concentrated by rotary evaporation, obtain the medicinal extract thing, and drying makes anistree natural antioxidants 4;
Step 3: after the anistree residue drying that step 2 is obtained, then, according to step 1,2 operations, extract temperature from room temperature to the solution boiling temperature, make anistree residue natural antioxidants 5.
2. the method for extracting natural antioxidants from anise as claimed in claim 1, is characterized in that the organic solvent used is methyl alcohol, ethanol, propyl alcohol, butanols, acetone, ether, sherwood oil or hexanaphthene.
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| CN102031196B (en) * | 2010-12-02 | 2012-07-18 | 北京航空航天大学 | Method for extracting effective ingredients in industrial residue of Chinese anise |
| CN102660290B (en) * | 2012-04-27 | 2014-03-12 | 东北林业大学 | Acorn shell pigment with antioxidant activity and preparation method and application thereof |
| CN105713732B (en) * | 2016-04-29 | 2020-03-17 | 山东农业大学 | Extraction method of star anise oil |
| CN113355156B (en) * | 2021-06-30 | 2022-12-02 | 四川省食品发酵工业研究设计院有限公司 | Antioxidant, preparation method thereof and application thereof in edible oil |
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| CN101411365A (en) * | 2008-11-14 | 2009-04-22 | 广东工业大学 | Recombinant aromatic condiment essential oil with oxidation resistance function and use method thereof |
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| CN101411365A (en) * | 2008-11-14 | 2009-04-22 | 广东工业大学 | Recombinant aromatic condiment essential oil with oxidation resistance function and use method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 3,5-二硝基水杨酸吸光光度法测定八角残渣中总糖、还原糖含量;舒馨等;《食品工业科技》;20100625;第31卷(第6期);341-343 * |
| 栗桂娇等.茴脑深加工制取茴香醛及茴香醛生物合成研究.《工业催化》.2007,第15卷37-40. |
| 舒馨等.3 5-二硝基水杨酸吸光光度法测定八角残渣中总糖、还原糖含量.《食品工业科技》.2010 |
| 茴脑深加工制取茴香醛及茴香醛生物合成研究;栗桂娇等;《工业催化》;20071231;第15卷;37-40 * |
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