CN102630943B - 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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- CN102630943B CN102630943B CN201210142102.8A CN201210142102A CN102630943B CN 102630943 B CN102630943 B CN 102630943B CN 201210142102 A CN201210142102 A CN 201210142102A CN 102630943 B CN102630943 B CN 102630943B
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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 with high anti-oxidation activity and platelet aggregation inhibitory activity and preparation method thereof, belong to modern food processing and biological technical field.
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 human body.Gamma-Linolenic acid, as the structural material of each tissue biological's film, is also the precursor substance of human body synthesis of prostaglandins, has anti-lipid oxidation, antiatherosclerosis, reduction serum cholesterol concentration, strengthens the multiple important physiological active functionses such as immunologic function.
Research is recently found, united state food and agricultural organization 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 the 8%-25% left and right 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%.As can be seen here, spirulina is the very promising source of gamma-Linolenic acid, but is fully paid attention to, and also only has in the world a small amount of research.
The domestic patent of preparing for spirulina gamma-Linolenic acid extract there is no record at present, and the extracting method 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 requirement, and recovery rate does not significantly improve; The latter has urea residual, easily forms suspect carcinogen urethanes, for being directly used in food and health products are not ideal.Therefore, it is organic extraction solvent that the present invention selects the volatile ethanol of safety, has invented a kind of safe and effective, economic easy-operating extracting mode; Simultaneously by the external activity of research gamma-Linolenic acid, for the research and development of the health products in spirulina source provide support.
Summary of the invention
The object of the invention is to develop a kind of economy easy to operate, be applicable to the technological process of the gamma-Linolenic acid of suitability for industrialized production, to make up the blank of preparing for spirulina gamma-Linolenic acid extract in the market, thereby the spirulina resource of deep development China's abundant, for the research and development of nutrient and healthcare products provide technical support.
For achieving the above object, the present invention is comprised of following steps:
Step 1: algae powder and ethanol are mixed according to the ratio of 1: 12～18 (w/v), utilize ultrasonic wave to carry out clasmatosis in 0～40 ℃ of water, power is 400W, the broken time is 10～15min.If the time is longer, can adopt fragmentation stage by stage, each 5min, produces and destroys content in case local temperature is too high;
Step 2: the algae powder after fragmentation-alcohol suspension continues constant temperature oscillation and extracts, extracting temperature can regulate between 60～70 ℃, and extraction time is 90～150min, notes lucifuge;
Step 3: the first vacuum filtration of mixture after extraction, the clarified solution obtaining recycling Vacuum Concentration is removed unnecessary solvent;
Step 4: the concentrated extract obtaining, through vacuum freeze drying, can obtain pulverous spirulina gamma-Linolenic acid extract, is convenient to storage and recycling; After chromatography of gases quantitative analysis, obtain extraction efficiency (GLA/ dry weight) and can be greater than 8.1g/kg (wt%).
The spirulina gamma-Linolenic acid extract obtaining by the method, by external DPPH radicals scavenging experiment, lipid oxidation, suppress experiment and its biologically active of platelet aggregation inhibition experimental verification, confirmation has good antioxidation in vitro and platelet aggregation-against effect, can be applicable to health food development field.
Accompanying drawing explanation
Below accompanying drawing is briefly explained.
Fig. 1 is extraction process figure.
Fig. 2 is the gas chromatogram of gamma-Linolenic acid extract.Transverse axis represents retention time, and the longitudinal axis represents peak area.
Fig. 3 is the inhibition figure of gamma-Linolenic acid to the platelet aggregation of being induced by ADP, and transverse axis represents GLA concentration (g/L), and the longitudinal axis represents inhibiting rate (%).
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, but do not limit the scope of the invention.
Embodiment 1:
By the dry spirulina powder of 5g, fully mix with 60mL ethanol, first in ice-water bath, utilize ultrasonic wave to carry out clasmatosis, power is 400W, the broken time is 10min.Algae powder-alcohol suspension after fragmentation, continues lucifuge lixiviate in water bath with thermostatic control, keeps temperature 70 C, vibration 90min, rotating speed 150r/min.The gamma-Linolenic acid extract mixed solution that lixiviate obtains, first passes through vacuum filtration elimination residue, and clarified solution is transferred to Rotary Evaporators (175Mbar, 40 ℃) and carries out Vacuum Concentration, thereby removes unnecessary solvent.Through the concentrated extract obtaining, again by vacuum freeze drying, finally can obtain the spirulina gamma-Linolenic acid extract of white powder.
Get the pure concentrated sulfuric acid-methyl alcohol (1: 9 for extract of 10mL, v/v) esterification 10min in 70 ℃ of waters bath with thermostatic control, after cooling, add 1mL n-hexane and use distilled water constant volume, mix rear stratification, get supernatant liquid for gas chromatographic detection, and calculate corresponding content according to calibration curve, obtain extraction efficiency (GLA/ dry weight) and can be greater than 8.3g/kg (wt%).
Embodiment 2:
By the dry spirulina powder of 20Kg, fully mix with 250L ethanol, first in the water-bath of 0～40 ℃, utilize ultrasonic wave to carry out clasmatosis, power is 400W, the broken time is 20min (minute four-stage is broken, each 5min).Algae powder-alcohol suspension after fragmentation, continues the lixiviate of constant temperature lucifuge, keeps temperature 70 C, vibration 90min, rotating speed 150r/min.The gamma-Linolenic acid extract mixed solution that lixiviate obtains, first passes through vacuum filtration elimination residue, and clarified solution is transferred in economic benefits and social benefits cryogenic vacuum concentration tank and carries out Vacuum Concentration, thereby removes unnecessary solvent.Through the concentrated extract obtaining, again by vacuum freeze drying, finally can obtain the spirulina gamma-Linolenic acid extract of white powder.
Get the pure concentrated sulfuric acid-methyl alcohol (1: 9 for extract of 10mL, v/v) esterification 10min in 70 ℃ of waters bath with thermostatic control, after cooling, add 1mL n-hexane and use distilled water constant volume, mix rear stratification, get supernatant liquid for gas chromatographic detection, and calculate corresponding content according to calibration curve, obtain extraction efficiency (GLA/ dry weight) and can be greater than 8.7g/kg (wt%).
Embodiment 3:
Extract in embodiment 1, carries out respectively DPPH radicals scavenging experiment, and lipid oxidation suppresses experiment and platelet aggregation suppresses experiment.
DPPH radicals scavenging experiment: 50 μ L variable concentrations samples are added to 5mL 0.004%DPPH (methyl alcohol dissolving), measure absorbance after room temperature 30min under 517nm, choose Vc as positive control.Obtain result 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 add in reaction environment with thiobarbituricacidα-at 535nm place, if show antioxidation activity, corresponding absorptance is linear change with concentration.Obtain result as table 2.
Platelet aggregation suppresses experiment: by centrifugal rear platelet rich plasma (PRP) and the platelet-poor plasma (PPP) produced respectively of fresh pig blood.With ADP, induce blood coagulation, add the gamma-Linolenic acid extract of 5 μ L variable concentrations, obtain the cohesion curve in different time points (60s, 180s, 300s) platelet aggregation situation and 3min.Obtain result as table or Fig. 3.
Result (table 1, table 2, accompanying drawing 3) shows that the gamma-Linolenic acid extract being undertaken by step 1 has good antioxidation activity in vitro, and more outstanding in lipid environment; Extract also shows the activity of obvious inhibition platelet aggregation simultaneously.
Table 1 gamma-Linolenic acid and the VC removing effect to DPPH free radical
Table 2 gamma-Linolenic acid and VC are to by Fe
2+the inhibition of the lipid oxidation reaction of induction
Claims (1)
1. contain the active and platelet aggregation inhibitory activity of high anti-oxidation the preparation method of spirulina gamma-Linolenic acid extract, it is characterized in that said method comprising the steps of:
Step 1: algae powder and ethanol are mixed according to the ratio of 1:12～18 (w/v), utilize ultrasonic wave to carry out clasmatosis in 0～40 ℃ of water, power is 400W, the broken time is 10～15min.If the time is longer, can adopt fragmentation stage by stage, each 5min, produces and destroys content in case local temperature is too high;
Step 2: the algae powder alcohol suspension after fragmentation continues constant temperature oscillation and extracts, extracting temperature can regulate between 60～70 ℃, and extraction time is 90～150min, notes lucifuge;
Step 3: the first vacuum filtration of mixture after extraction, the clarified solution obtaining recycling Vacuum Concentration is removed unnecessary solvent, keeps pressure 175Mbar, 40 ℃ of temperature;
Step 4: remove the extract of desolventizing through vacuum freeze drying, can obtain pulverous spirulina gamma-Linolenic acid extract, be convenient to storage and reprocessing; Through gas-chromatography, carry out quantitative assay, the GLA productive rate obtaining is 8.1g/kg (GLA/ dry weight).
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| 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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| CN1253426C (en) * | 2003-05-08 | 2006-04-26 | 南京大学 | Process for extracting, preparing and purifying gamma methyllinolenate from algae |
| DE102004062141A1 (en) * | 2004-12-23 | 2006-07-06 | Nutrinova Nutrition Specialties & Food Ingredients Gmbh | Process for the preparation of a crude oil from mixtures of microorganisms and plants, the oil thus produced and the specific uses of the thus prepared and optionally additionally refined oil |
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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 |