CN102630943A - Spirulina gamma-linolenic acid extractive and preparation method thereof - Google Patents
Spirulina gamma-linolenic acid extractive and preparation method thereof Download PDFInfo
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- CN102630943A CN102630943A CN2012101421028A CN201210142102A CN102630943A CN 102630943 A CN102630943 A CN 102630943A CN 2012101421028 A CN2012101421028 A CN 2012101421028A CN 201210142102 A CN201210142102 A CN 201210142102A CN 102630943 A CN102630943 A CN 102630943A
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Abstract
The invention discloses a spirulina gamma-linolenic acid extractive and a preparation method of the spirulina gamma-linolenic acid extractive. The spirulina gamma-linolenic acid extractive has high antioxidation activity and antiplatelet activity. According to the spirulina gamma-linolenic acid extractive, spirulina powder is taken as a raw material; and by ultrasonic processing, organic solvent extraction, vacuum filtration, vacuum concentration, vacuum freezing drying and gas chromatograph-mass spectrometer measurement, the powdered spirulina gamma-linolenic acid extractive can be finally obtained. A DPPH (1.1-diphenyl-2-1picryhydrazyl radial) scavenging test, a lipid oxidation inhibition test and a platelet aggregation inhibition test show that the spirulina gamma-linolenic acid extractive has high antioxidation activity and antiplatelet activity, and finally prove that the mode of extracting gamma-linolenic acid from spirulina is an economic and effective mode. The method disclosed by the invention can be applied to the field of development of health-care food.
Description
Technical field
The present invention relates to a kind of spirulina gamma-Linolenic acid extract and preparation method thereof, belong to modern food processing and biological technical field with high anti-oxidation activity and platelet aggregation inhibitory activity.
Background technology
Gamma-Linolenic acid is described as the leading role of functional food " 21 century ", is indispensable a kind of polyunsaturated fatty acid in the human body.Gamma-Linolenic acid also is the precursor substance of human body synthesis of prostaglandins as the structural material of each tissue biological's film, has multiple important physical active functions such as the oxidation of lipotropism matter, antiatherosclerosis, reduction serum cholesterol concentration, raise immunity.
Discover recently; By FAO (Food and Agriculture Organization of the United Nation) recommend " optimal food of 21 century "---spirulina is unique biology that contains abundant gamma-Linolenic acid in the autotroph of finding so far; Content is up to 11970mg/kg algae powder; Account for the 20%-30% of frond fatty acid, its gamma-linolenic acid content can account for about the 8%-25% of its aliphatic acid.And in the evening primrose oil of the main extraction source of gamma-Linolenic acid, gamma-linolenic acid content is only at 7%-10%.This shows that spirulina is the very promising source of gamma-Linolenic acid, but is fully paid attention to, and also has only a small amount of research in the world.
At present domestic patent no record still for the preparation of spirulina gamma-Linolenic acid extract, the method for distilling that pertinent literature research is mentioned mainly concentrates on supercritical carbon dioxide extraction method, urea adduct method etc.But the former is high to equipment requirements, and recovery rate does not significantly improve; The latter has urea residual, be prone to form the suspect carcinogen urethanes, for directly being used for food and health products are not ideal.Therefore, it is organic extraction solvent that the present invention selects the volatile ethanol of safety for use, has invented a kind of safe and effective, economic easy-operating extracting mode; External activity through the research gamma-Linolenic acid simultaneously is for the research and development of the health products in spirulina source provide support.
Summary of the invention
It is easy to operate to the objective of the invention is to develop a kind of economy; Be fit to the technological process of the gamma-Linolenic acid of suitability for industrialized production; To remedy the blank for preparing for spirulina gamma-Linolenic acid extract in the market; Thereby the spirulina resource of deep development China's abundant is for the research and development of nutrient and healthcare products provide technical support.
For realizing above-mentioned purpose, the present invention is made up of following steps:
Step 1: according to the mixed of 1: 12～18 (w/v), in 0～40 ℃ of water, utilize ultrasonic wave to carry out clasmatosis algae powder and ethanol, power is 400W, and the broken time is 10～15min.If the time is longer, can adopt fragmentation stage by stage, each 5min is in case too high content is produced of local temperature destroyed;
Step 2: the algae powder after the fragmentation-alcohol suspension continues constant-temperature shaking and extracts, and extracts temperature and can between 60～70 ℃, regulate, and extraction time is 90～150min, notes lucifuge;
Step 3: the mixture elder generation vacuum filtration after the solvent lixiviate, the clarified solution that obtains utilizes vacuum to concentrate again and removes unnecessary solvent;
Step 4: the concentrated extract that obtains can obtain pulverous spirulina gamma-Linolenic acid extract through vacuum freeze drying, is convenient to storage and utilizes; After the chromatography of gases quantitative analysis, obtaining extraction efficiency (GLA/ dry weight) can be greater than 8.1g/kg (wt%).
The spirulina gamma-Linolenic acid extract that obtains with the method; Suppress experiment and its biologically active of platelet aggregation inhibition experimental verification through external DPPH radicals scavenging experiment, lipid oxidation; Confirmation has good antioxidation in vitro and platelet aggregation-against effect, can be applicable to the health food development field.
Description of drawings
Briefly explain in the face of accompanying drawing down.
Fig. 1 is extraction process figure.
Fig. 2 is the gas chromatogram of gamma-Linolenic acid extract.Transverse axis is represented retention time, and the longitudinal axis is represented peak area.
Fig. 3 is a gamma-Linolenic acid to the inhibition design sketch of the platelet aggregation of being induced by ADP, and transverse axis is represented GLA concentration (g/L), and the longitudinal axis is represented inhibiting rate (%).
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is made further detailed description, but do not limit the scope of the invention.
Embodiment 1:
The spirulina powder that 5g is dry fully mixes with 60mL ethanol, in ice-water bath, utilizes ultrasonic wave to carry out clasmatosis earlier, and power is 400W, and the broken time is 10min.Algae powder-alcohol suspension after fragmentation continues lucifuge lixiviate in water bath with thermostatic control, keeps 70 ℃ of temperature, vibration 90min, rotating speed 150r/min.The gamma-Linolenic acid extract mixing solution that lixiviate obtains at first passes through vacuum filtration elimination residue, and clarified solution is transferred to Rotary Evaporators (175Mbar, 40 ℃) to carry out vacuum and concentrate, thereby removes unnecessary solvent.Pass through vacuum freeze drying again through concentrating the extract that obtains, finally can obtain the spirulina gamma-Linolenic acid extract of white powder.
Get the pure extract of 10mL with the concentrated sulfuric acid-methyl alcohol (1: 9; V/v) esterification 10min in 70 ℃ of waters bath with thermostatic control; The cooling back adds the 1mL n-hexane and uses the distilled water constant volume, and standing demix behind the mixing is got supernatant liquid and is used for gas chromatographic detection; And calculate corresponding content according to calibration curve, obtaining extraction efficiency (GLA/ dry weight) can be greater than 8.3g/kg (wt%).
Embodiment 2:
The spirulina powder that 20Kg is dry fully mixes with 250L ethanol, at first in 0～40 ℃ water-bath, utilizes ultrasonic wave to carry out clasmatosis, and power is 400W, and the broken time is 20min (dividing four-stage broken, each 5min).Algae powder-alcohol suspension after fragmentation continues the lixiviate of constant temperature lucifuge, keeps 70 ℃ of temperature, vibration 90min, rotating speed 150r/min.The gamma-Linolenic acid extract mixing solution that lixiviate obtains at first passes through vacuum filtration elimination residue, and clarified solution is transferred to and carries out vacuum in the economic benefits and social benefits cryogenic vacuum concentration tank and concentrate, thereby removes unnecessary solvent.Pass through vacuum freeze drying again through concentrating the extract that obtains, finally can obtain the spirulina gamma-Linolenic acid extract of white powder.
Get the pure extract of 10mL with the concentrated sulfuric acid-methyl alcohol (1: 9; V/v) esterification 10min in 70 ℃ of waters bath with thermostatic control; The cooling back adds the 1mL n-hexane and uses the distilled water constant volume, and standing demix behind the mixing is got supernatant liquid and is used for gas chromatographic detection; And calculate corresponding content according to calibration curve, obtaining extraction efficiency (GLA/ dry weight) can be greater than 8.7g/kg (wt%).
Embodiment 3:
Extract among the embodiment 1 carries out DPPH radicals scavenging experiment respectively, and lipid oxidation suppresses experiment and platelet aggregation suppresses experiment.
DPPH radicals scavenging experiment: 50 μ L variable concentrations samples are added 5mL 0.004%DPPH (methyl alcohol dissolving), under 517nm, measure absorbance behind the room temperature 30min, choose Vc as positive control.Obtain result such as table 1.
Lipid oxidation suppresses experiment: lecithin is used to Fe
2+The oxidation reaction of mediation provides lipid system, measures absorbance GLA extract at the 535nm place with thiobarbituricacid and adds in the reaction environment, if show antioxidation activity, corresponding absorptance is linear change with concentration.Obtain result such as table 2.
Platelet aggregation suppresses experiment: fresh pig blood is produced platelet rich plasma (PRP) and platelet-poor plasma (PPP) respectively after centrifugal.Induce blood coagulation with ADP, add the gamma-Linolenic acid extract of 5 μ L variable concentrations, promptly obtain the cohesion curve in different time points (60s, 180s, 300s) platelet aggregation situation and the 3min.Obtain the result like table or Fig. 3.
Result's (table 1, table 2, accompanying drawing 3) shows that the gamma-Linolenic acid extract that is undertaken by step 1 has good antioxidation activity in vitro, and more outstanding in the lipid environment; Extract also shows the activity of obvious suppression platelet aggregation simultaneously.
Table 1 gamma-Linolenic acid and VC are to the removing effect of DPPH free radical
Table 2 gamma-Linolenic acid and VC are to by Fe
2+The inhibition effect of the lipid oxidation reaction of inducing
Claims (3)
1. spirulina gamma-Linolenic acid extract with the active and platelet aggregation inhibitory activity of high anti-oxidation and preparation method thereof.
2. one kind contains spirulina gamma-Linolenic acid preparation method of extract as claimed in claim 1, it is characterized in that said method comprising the steps of:
Step 1: according to the mixed of 1: 12～18 (w/v), in 0～40 ℃ of water, utilize ultrasonic wave to carry out clasmatosis algae powder and ethanol, power is 400W, and the broken time is 10～15min.If the time is longer, can adopt fragmentation stage by stage, each 5min is in case too high content is produced of local temperature destroyed;
Step 2: the algae powder alcohol suspension after the fragmentation continues constant-temperature shaking and extracts, and extracts temperature and can between 60～70 ℃, regulate, and extraction time is 90～150min, notes lucifuge;
Step 3: the mixture elder generation vacuum filtration after the solvent lixiviate, the clarified solution that obtains utilizes vacuum to concentrate again and removes unnecessary solvent, keeps pressure 175Mbar, 40 ℃ of temperature;
Step 4: remove the extract desolvate through vacuum freeze drying, can obtain pulverous spirulina gamma-Linolenic acid extract, be convenient to storage and reprocessing; Carry out quantitative assay through gas-chromatography, obtaining extraction efficiency (GLA/ dry weight) can be greater than 8.1g/kg (wt%).
3. the application of spirulina gamma-Linolenic acid extract as claimed in claim 1 in correlation function food and nutritional health food is characterized in that said extract has the activity of tangible antioxidation activity and platelet aggregation-against.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103191579A (en) * | 2013-04-27 | 2013-07-10 | 云南蓝钻生物科技有限公司 | Method for extracting gamma-linolenic acid in spirulina through supercritical CO2 |
| CN105124200A (en) * | 2015-08-10 | 2015-12-09 | 浙江省海洋开发研究院 | Artificial formula feed for preventing and treating hemorrhagic disease of oplegnathidae |
| CN107874253A (en) * | 2016-09-30 | 2018-04-06 | 国家开发投资公司 | A kind of spirulina glycolipid preparation method rich in acid and gamma-linolenic |
| CN108358772A (en) * | 2017-12-20 | 2018-08-03 | 湖北工业大学 | A kind of preparation method and applications of spirulina gamma-Linolenic acid extract |
| TWI645847B (en) * | 2016-03-04 | 2019-01-01 | 蕭郁芸 | Orchid seed extract and product containing extract thereof |
| CN109349528A (en) * | 2018-11-26 | 2019-02-19 | 河南汇元特殊医学用途配方食品有限公司 | A kind of alimentary paste and preparation method thereof containing dietary fiber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0891773A1 (en) * | 1997-07-07 | 1999-01-20 | L'oreal | Use of gamma-linolenic acid for preventing oxydative stress |
| CN1448383A (en) * | 2003-05-08 | 2003-10-15 | 南京大学 | Process for extracting, preparing and purifying gamma methyllinolenate from algae |
| CN101133144A (en) * | 2004-12-23 | 2008-02-27 | 努特诺瓦营养产品及食品成分有限公司 | Method for producing a raw oil from mixtures of micro-organisms and plants, oil produced according to said method and specific uses of the thus produced oil and, optionally, additional refined oil |
-
2012
- 2012-05-08 CN CN201210142102.8A patent/CN102630943B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0891773A1 (en) * | 1997-07-07 | 1999-01-20 | L'oreal | Use of gamma-linolenic acid for preventing oxydative stress |
| CN1448383A (en) * | 2003-05-08 | 2003-10-15 | 南京大学 | Process for extracting, preparing and purifying gamma methyllinolenate from algae |
| CN101133144A (en) * | 2004-12-23 | 2008-02-27 | 努特诺瓦营养产品及食品成分有限公司 | Method for producing a raw oil from mixtures of micro-organisms and plants, oil produced according to said method and specific uses of the thus produced oil and, optionally, additional refined oil |
Non-Patent Citations (6)
| Title |
|---|
| 《卫生研究》 20030520 董杰明等 gamma-亚麻酸的保健作用 第299页右栏第3小节，第300页右栏第10小节 1,3 第32卷, 第3期 * |
| 《粮食与油脂》 20041010 慕鸿雁等 gamma-亚麻酸生理功能、资源及其分离纯化 第12-14页 1-3 , 第10期 * |
| 《郑州粮食学院学报》 19970330 曹健等 利用螺旋藻生产gamma-亚麻酸 第68-73页 1-3 第18卷, 第1期 * |
| 慕鸿雁等: "γ-亚麻酸生理功能、资源及其分离纯化", 《粮食与油脂》 * |
| 曹健等: "利用螺旋藻生产γ-亚麻酸", 《郑州粮食学院学报》 * |
| 董杰明等: "γ-亚麻酸的保健作用", 《卫生研究》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103191579A (en) * | 2013-04-27 | 2013-07-10 | 云南蓝钻生物科技有限公司 | Method for extracting gamma-linolenic acid in spirulina through supercritical CO2 |
| CN103191579B (en) * | 2013-04-27 | 2015-07-29 | 云南蓝钻生物科技有限公司 | A kind of supercritical CO 2the method of gamma-Linolenic acid in extraction spirulina |
| CN105124200A (en) * | 2015-08-10 | 2015-12-09 | 浙江省海洋开发研究院 | Artificial formula feed for preventing and treating hemorrhagic disease of oplegnathidae |
| TWI645847B (en) * | 2016-03-04 | 2019-01-01 | 蕭郁芸 | Orchid seed extract and product containing extract thereof |
| CN107874253A (en) * | 2016-09-30 | 2018-04-06 | 国家开发投资公司 | A kind of spirulina glycolipid preparation method rich in acid and gamma-linolenic |
| CN108358772A (en) * | 2017-12-20 | 2018-08-03 | 湖北工业大学 | A kind of preparation method and applications of spirulina gamma-Linolenic acid extract |
| CN109349528A (en) * | 2018-11-26 | 2019-02-19 | 河南汇元特殊医学用途配方食品有限公司 | A kind of alimentary paste and preparation method thereof containing dietary fiber |
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| CN102630943B (en) | 2014-03-19 |
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Effective date of registration: 20200323 Address after: 016100 the Inner Mongolia Autonomous Region city Etuokeqi Erdos Wulan Town Industrial Park of Spirulina Patentee after: ORDOS XINYULI SPIRULINA INDUSTRY GROUP Co.,Ltd. Address before: 100083 35 Qinghua East Road, Beijing, Haidian District, Beijing Forestry University Patentee before: BEIJING FORESTRY University |