CN102219669B - Method for extracting purslane linolenic acid with supercritical CO2 fluid - Google Patents
Method for extracting purslane linolenic acid with supercritical CO2 fluid Download PDFInfo
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- CN102219669B CN102219669B CN201010146072.9A CN201010146072A CN102219669B CN 102219669 B CN102219669 B CN 102219669B CN 201010146072 A CN201010146072 A CN 201010146072A CN 102219669 B CN102219669 B CN 102219669B
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- extraction
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- linolenic acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention relates to a method for extracting purslane linolenic acid with supercritical CO2 fluid. The method for extracting purslane linolenic acid with supercritical CO2 fluid comprises the following steps of: filling a proper amount of crushed purslane in an extraction column of a supercritical CO2 fluid extraction system and then sealing, heating up and boosting the extraction system respectively to reach an extraction condition, starting circular extraction and regulating CO2 flow rate, and keeping constant temperature/pressure extraction for a certain period of time. According to the method disclosed by the invention, alpha-linolenic acid is extracted from purslane by adopting the supercritical CO2 fluid extraction technique at the low temperature not more than 60 DEG C and under the high pressure about 40Mpa, thus oxidative deterioration of unsaturated fatty acid is effectively reduced so that CO2 infiltrates deeply into plant cells, and higher yield is obtained. Compared with traditional extraction methods, the method disclosed by the invention has high obtained yield and no residual solvent, and ensures that the product quality is remarkably improved and the extraction time is greatly shortened.
Description
Technical field
The present invention relates to a kind of employing supercritical CO
2the linolenic method of fluid extraction purslane.
Background technology
Alpha-linolenic acid (α-linolenic acid), as essential fatty acid, is the structured material of each tissue biological's film in body, is also the precursor of human body synthesis of prostaglandins.Recently study and show, alpha-linolenic acid has many pharmacological actions, if any reducing blood lipid, can reduce the content of Blood Cholesterol and triglyceride; Certain anticancer function is arranged, some tumours are had to obvious inhibition effect; Have hypotensive, suppress irritated, antithrombotic effect; Sight function and learning activities are had to promoter action etc.
Purslane (Portulaca oleracea L.) is Portulacaceae annual herb plant, has the effect of clearing heat and detoxicating, loose blood detumescence.Modern study finds, purslane is as the green wild plant of medicine-food two-purpose, except having reducing blood-fat, relaxed muscle, antibiotic, anti-inflammatory, analgesia and promoting, the effect such as wound healing, also has stronger anti-ageing and antioxygenation.Preliminary study shows in Herba portulacae extract to contain a large amount of unsaturated fatty acids compositions, and wherein alpha-linolenic acid can reach more than 10%.Purslane is widely distributed in China, aboundresources, but the deep processing utilization is also seldom.Research China purslane resource, and therefrom obtain linolenic acid, for the exploitation of China's wild plant resource and the research of natural product, all have very important significance.
Tradition is extracted alpha-linolenic acid and mostly is solvent extraction method and cold-press, but due to alpha-linolenic acid height nonsaturation, unstable in air, oxidizing reaction especially easily occurs under hot conditions, adopts that traditional extraction method ubiquity rate of recovery is low, the product yield is not high, the residual problem such as too much of objectionable impurities.
Summary of the invention
In order to address the above problem, the invention provides that a kind of flow process is simple, extraction time is short, solvent toxicity is little and can effectively prevent product rotten extract linolenic method from purslane.
To achieve the above object, the present invention has adopted following technical scheme: a kind of employing supercritical CO
2the linolenic method of fluid extraction purslane, comprise the following steps:
(1) get and be crushed in right amount 20～100 purpose purslanes, the supercritical CO of packing into
2after the column extractor of fluid extraction system, seal;
(2) extracting system is heated up respectively, boosted to extraction conditions, started cycling extraction, and regulated CO
2flow, keep constant temperature and pressure extraction certain hour.
Described supercritical CO
2the extracting pressure of fluid extraction process is 10～50M Pa;
Described supercritical CO
2the extraction temperature of fluid extraction process is 30～60 ℃;
Described supercritical CO
2the CO of fluid extraction process
2flow velocity is 1～5mL/min;
(3) extracting system separates and obtains the linolenic acid crude product after decrease temperature and pressure.
The present invention adopts supercritical CO
2the fluid extraction method is extracted linolenic acid from purslane, through supercritical CO once
2fluid extraction can extract the alpha-linolenic acid that obtains about 11.4mg～28.2mg from 100g purslane sample.
Through supercritical CO
2the alpha-linolenic acid product of fluid extraction gained, after esterification is processed, takes reversed-phased high performace liquid chromatographic to carry out the linolenic acid detection by quantitative.
Described esterification method mainly comprises: get the 1mL sample liquid and dry up with nitrogen, add 2mL methyl alcohol-sodium methoxide solution, after 50 ℃ of reaction 10min, add the 2mL n-hexane extraction, collect the normal hexane phase.
Described reversed-phased high performace liquid chromatographic (RP-HPLC), key step is: according to many experiments relatively, select the Linolenic acid methylester chromatogram testing conditions of optimizing: moving phase: 0.05% phosphate aqueous solution: methyl alcohol=10: 90 (v/v); Flow velocity: 1.0mL/min; Detect wavelength: 210nm; Column temperature: 30 ℃; Sample size: 2 μ L.
The present invention uses supercritical CO
2fluid extraction technology extracts alpha-linolenic acid from purslane, and extraction process carries out being no more than under the low temperature of 60 ℃, has effectively reduced the deterioration by oxidation of unsaturated fatty acids; Extraction process carries out again under the high pressure up to the 40Mpa left and right, makes CO
2the deep vegetable cell inside of infiltrating, obtained higher output capacity.With traditional solvent-extraction process or cold-press, compare, target product yield of the present invention is high, and the noresidue solvent significantly improves quality product, and greatly shortened extraction time.Research method of the present invention and result provide reference for developing wild plant, for the deep development utilization of wild plant provides better method and platform.
Embodiment
Below by embodiment 1-5, concrete technical scheme of the present invention is described in further detail.
Embodiment 1: material particular diameter extracts the impact of yield on alpha-linolenic acid
A kind of employing supercritical CO
2the linolenic method of fluid extraction purslane, comprise the following steps: to get and be crushed in right amount 20～100 purpose purslane stems, the supercritical CO of packing into
2seal after the column extractor of fluid extraction system, extracting system is warming up to 30 ℃, boost to 40MPa, start cycling extraction, and regulate CO
2flow is 2mL/min, keeps constant temperature and pressure extraction 2h.Separate and obtain the linolenic acid crude product after decrease temperature and pressure.The results are shown in Table 1:
Table 1 material particular diameter extracts the impact of yield on alpha-linolenic acid
Embodiment 2: the impact of extracting pressure on the alpha-linolenic acid yield
A kind of employing supercritical CO
2the linolenic method of fluid extraction purslane, comprise the following steps: to get and be crushed in right amount 50 purpose purslanes, the supercritical CO of packing into
2seal after the column extractor of fluid extraction system, extracting system is warming up to 30 ℃, boost to 10～50MPa, start cycling extraction, and regulate CO
2flow is 2mL/min, keeps constant temperature and pressure extraction 2h.Separate and obtain the linolenic acid crude product after decrease temperature and pressure.The results are shown in Table 2:
The impact of table 2 extracting pressure on the alpha-linolenic acid yield
Embodiment 3: the impact of extraction temperature on the alpha-linolenic acid yield
A kind of employing supercritical CO
2the linolenic method of fluid extraction purslane, comprise the following steps: to get and be crushed in right amount 80 purpose purslanes, the supercritical CO of packing into
2seal after the column extractor of fluid extraction system, extracting system is warming up to 30～60 ℃, boost to 40MPa, start cycling extraction, and regulate CO
2flow is 2mL/min, keeps constant temperature and pressure extraction 2h.Separate and obtain the linolenic acid crude product after decrease temperature and pressure.The results are shown in Table 3:
The impact of table 3 extraction temperature on the alpha-linolenic acid yield
Embodiment 4:CO
2the impact of flow velocity on the alpha-linolenic acid yield
A kind of employing supercritical CO
2the linolenic method of fluid extraction purslane, comprise the following steps: to get and be crushed in right amount 80 purpose purslanes, the supercritical CO of packing into
2seal after the column extractor of fluid extraction system, extracting system is warming up to 40 ℃, boost to 40MPa, start cycling extraction, and regulate CO
2flow is 1～5mL/min, keeps constant temperature and pressure extraction 2h.Separate and obtain the linolenic acid crude product after decrease temperature and pressure.The results are shown in Table 4:
Table 4CO
2the impact of flow velocity on the alpha-linolenic acid yield
Embodiment 5: the impact of extraction time on the alpha-linolenic acid yield
Get and be crushed in right amount 50 purpose purslanes, the supercritical CO of packing into
2seal after the column extractor of fluid extraction system, extracting system is warming up to 50 ℃, boost to 30MPa, start cycling extraction, and regulate CO
2flow is 2mL/min, keeps constant temperature and pressure extraction 1～3h.Separate and obtain the linolenic acid crude product after decrease temperature and pressure.The results are shown in Table 5:
The impact of table 5 extraction time on the alpha-linolenic acid yield
Claims (1)
1. one kind adopts supercritical CO
2the linolenic method of fluid extraction purslane, is characterized in that comprising the following steps:
(1) get 100g and be crushed to 50 purpose purslanes, the supercritical CO of packing into
2after the column extractor of fluid extraction system, seal;
(2) extracting system is heated up respectively, boosted to extraction conditions, started cycling extraction, and regulated CO
2flow, keep constant temperature and pressure extraction 2h;
Described supercritical CO
2the extracting pressure of fluid extraction process is 40MPa;
Described supercritical CO
2the extraction temperature of fluid extraction process is 30 ℃;
Described supercritical CO
2the CO of fluid extraction process
2flow velocity is 2ml/min;
(3) extracting system separates and obtains linolenic acid crude product 26.1mg after decrease temperature and pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010146072.9A CN102219669B (en) | 2010-04-13 | 2010-04-13 | Method for extracting purslane linolenic acid with supercritical CO2 fluid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010146072.9A CN102219669B (en) | 2010-04-13 | 2010-04-13 | Method for extracting purslane linolenic acid with supercritical CO2 fluid |
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| CN102219669A CN102219669A (en) | 2011-10-19 |
| CN102219669B true CN102219669B (en) | 2014-01-01 |
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| CN201010146072.9A Expired - Fee Related CN102219669B (en) | 2010-04-13 | 2010-04-13 | Method for extracting purslane linolenic acid with supercritical CO2 fluid |
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| CN105193876B (en) * | 2015-10-11 | 2017-02-01 | 广州市禾基生物科技有限公司 | Purslane extract and preparation method thereof |
| CN107513388A (en) * | 2017-07-25 | 2017-12-26 | 康泽波 | It is a kind of to be used to administer medicament of soil arsenic pollution and preparation method thereof |
| CN112300000B (en) * | 2020-11-26 | 2022-05-17 | 辽宁中医药大学 | Ester compound with anti-tumor and anti-cholinesterase activities in purslane as well as extraction and separation method and application thereof |
| CN113520954A (en) * | 2021-08-24 | 2021-10-22 | 苏州健雄职业技术学院 | Traditional Chinese medicine acne removing cream and production process thereof |
Citations (4)
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| CN1424389A (en) * | 2002-12-20 | 2003-06-18 | 吉首大学科技研究开发中心 | Method for extracting linolenic acid oil from yangtao |
| CN1502353A (en) * | 2002-11-20 | 2004-06-09 | 北京瑞康医药技术有限公司 | Compound chuanxiong and angelica total extract and preparation, use thereof |
| CN101550078A (en) * | 2009-05-15 | 2009-10-07 | 淮海工学院 | Method of supercritical extraction of unsaturated fatty acid of schizochytrium limacinum |
| CN101643403A (en) * | 2009-04-10 | 2010-02-10 | 陈海燕 | Method for extracting linolenic acid from purslane |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1502353A (en) * | 2002-11-20 | 2004-06-09 | 北京瑞康医药技术有限公司 | Compound chuanxiong and angelica total extract and preparation, use thereof |
| CN1424389A (en) * | 2002-12-20 | 2003-06-18 | 吉首大学科技研究开发中心 | Method for extracting linolenic acid oil from yangtao |
| CN101643403A (en) * | 2009-04-10 | 2010-02-10 | 陈海燕 | Method for extracting linolenic acid from purslane |
| CN101550078A (en) * | 2009-05-15 | 2009-10-07 | 淮海工学院 | Method of supercritical extraction of unsaturated fatty acid of schizochytrium limacinum |
Non-Patent Citations (4)
| Title |
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| 徐徳钦等.正交实验法优化马齿苋中α-亚麻酸的提取工艺参数研究.《食品工业科技》.2010,第30卷(第2期),215-217. |
| 正交实验法优化马齿苋中α-亚麻酸的提取工艺参数研究;徐徳钦等;《食品工业科技》;20100225;第30卷(第2期);215-217 * |
| 超临界CO2萃取工艺在紫苏子脂肪油;辉国钧等;《中国医药工业杂志》;19960221;第27卷(第2期);51-53 * |
| 辉国钧等.超临界CO2萃取工艺在紫苏子脂肪油.《中国医药工业杂志》.1996,第27卷(第2期),51-53. |
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