CN104629899A - Method for extracting malania oleifera oil by virtue of supercritical CO2 fluid - Google Patents
Method for extracting malania oleifera oil by virtue of supercritical CO2 fluid Download PDFInfo
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- CN104629899A CN104629899A CN201410850588.XA CN201410850588A CN104629899A CN 104629899 A CN104629899 A CN 104629899A CN 201410850588 A CN201410850588 A CN 201410850588A CN 104629899 A CN104629899 A CN 104629899A
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- extraction
- malania oleifera
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method for extracting malania oleifera oil by virtue of supercritical CO2 fluid. The method comprises the following steps: (1) drying and pulverizing malania oleifera nuts, sieving with a 8-20-mesh sieve to obtain malania oleifera nut powder; (2) feeding malania oleifera nut powder into a hermetically sealed extraction kettle and circularly carrying out supercritical CO2 extraction fluid extraction for 2-4 hours under the conditions of the extraction pressure of 25-40MPa, the extraction temperature of 45-55 DEG C, the analytical pressure of 6-10MPa and the analytical temperature of 55-65 DEG C, collecting an extract, namely, malania oleifera oil. The method has the advantages of high extraction efficiency, no need of any organic solvent, high extraction speed and short time and is simple and convenient to operate, safe and reliable compared to the traditional method; carbon dioxide is non-toxic, free of residues and can be recycled; and the product is good in color and low in acid value and low peroxide value.
Description
Technical field
The invention belongs to extracted form natural plant product technical field, specifically, relate to a kind of extracting method of Malania Oleifera Oil.
Background technology
Malania oleifera Malania oleifera Chun et Lee, after having another name called mountain paulownia fruit, kalimeris (strong language), is the fruit of Olacaceae malania oleifera platymiscium head of garlic fruit tree.Head of garlic fruit tree is the distinctive autogenus plant of China, and seldom, only NATURAL DISTRIBUTION is in West Guangxi to the narrow zone of southeastern Yunnan for existing malania oleifera quantity qf population resources.Malania oleifera is rich in grease, and oil length, up to 64.5%, is the desirable feedstock of synthetic musk ketone, there are some researches show the Selacholeic acid containing more than 50% in its grease, is that current occurring in nature finds the plant that Selacholeic acid content is the highest.Selacholeic acid is a kind of long-chain unsaturated fatty acid, and remarkable to the cardiovascular and human autoimmune's property curative effect of disease for the treatment of, be also important perfume base, market demand is huge, but occurring in nature storage is rare, and it is difficult to synthesize.Therefore, realizing is that raw material industrialization production Selacholeic acid has very important significance with Malania Oleifera Oil.
Research report is extracted about Malania Oleifera Oil less in existing document, mostly be Petroleum ether extraction, as: Ding Junfeng, Cao Jianhua, woods is built superfine. the dynamic extraction process condition [J] of the preferred malania oleifera of orthogonal experiment method. and Jiangxi Normal University's journal (natural science edition), 2008,32 (3): 269-272 disclose the preferred process condition of Petroleum ether extraction Malania Oleifera Oil and yield is 55%; Cao Jianhua, Ding Junfeng, woods is built superfine. Malania Oleifera Oil microwave radiation exaraction and Analysis of Fatty Acids Composition [J]. and Chinese oil, 2008,33 (10): 17-20 disclose the condition of microwave-assisted Petroleum ether extraction Malania Oleifera Oil and yield is 57.5%; Ding Junfeng, Cao Jianhua, woods is built superfine. the technical study [J] of ultrasonic-assisted extraction malania oleifera fruit oil. and food science and technology, 2008,33 (11): 170-173 disclose the condition of ultrasonic-assisted extraction Malania Oleifera Oil and yield is 62.3%.These researchs have certain reference significance, but go back Shortcomings: the yield of Malania Oleifera Oil is low, containing dissolvent residual.
Supercritical CO
2fluid extraction law technology utilizes supercritical CO
2fluid is solvent, some active principle or monomer is extracted from solid or liquid, and carry out a kind of technology of being separated, can effectively enhance productivity, rate of extraction is fast, the time is short, extracted amount is many, and can exempt any poisonous and hazardous organic solvent completely in process of production, not to environment, extract containing organic solvent residual, does not remain the natural characteristic of extract.
By literature search, the open source literature report identical with the present invention is had no.
Summary of the invention
The object of the present invention is to provide a kind of efficient, no solvent residue, and easy and simple to handle, the method for the extraction Malania Oleifera Oil of suitability for industrialized production can be realized.
The present invention specifically comprises the following steps:
A kind of supercritical CO
2the method of fluid extraction Malania Oleifera Oil,
(1) by Malania oleifera drying and crushing, cross 8 ~ 20 mesh sieves, obtain Malania oleifera powder;
(2) Malania oleifera powder is loaded in airtight extraction kettle carry out supercritical CO
2fluid extraction, extraction conditions is extracting pressure 25 ~ 40MPa, extraction temperature 45 ~ 55 DEG C, parsing pressure 6 ~ 10MPa, resolution temperature 55 ~ 65 DEG C, and cycling extraction, after 2 ~ 4 hours, is collected extract, obtained Malania Oleifera Oil.
Compared with prior art, the present invention adopts following technical scheme:
(1) production efficiency is high, and not to environment, avoid using any poisonous and hazardous organic solvent, extract does not contain organic solvent residual, and easy and simple to handle, can realize suitability for industrialized production;
(2) rate of extraction is fast, the time is short, extracted amount is many, malania oleifera cast of oil is good, Selacholeic acid content is high, acid number and peroxide value low.
Embodiment:
Embodiment 1
Get Malania oleifera 8kg drying and crushing, cross 8 mesh sieves, obtain Malania oleifera powder, Malania oleifera powder is loaded in airtight extraction kettle and carries out supercritical CO
2fluid extraction, extraction conditions is extracting pressure 35MPa, extraction temperature 45 DEG C, parsing pressure 6MPa, resolution temperature 55 DEG C, CO
2flow 180L/ hour, cycling extraction is after 3 hours, and collect extract, obtain golden transparent Malania Oleifera Oil 5.32kg, yield is 66.5%.
Embodiment 2
Get Malania oleifera 8kg drying and crushing, cross 12 mesh sieves, obtain Malania oleifera powder, Malania oleifera powder is loaded in airtight extraction kettle and carries out supercritical CO
2fluid extraction, extraction conditions is extracting pressure 30MPa, extraction temperature 45 DEG C, parsing pressure 6MPa, resolution temperature 55 DEG C, CO
2flow 170L/ hour, cycling extraction is after 2 hours, and collect extract, obtain golden transparent Malania Oleifera Oil 5.33kg, yield is 66.6%.
Embodiment 3
Get Malania oleifera 8kg drying and crushing, cross 20 mesh sieves, obtain Malania oleifera powder, Malania oleifera powder is loaded in airtight extraction kettle and carries out supercritical CO
2fluid extraction, extraction conditions is extracting pressure 25MPa, extraction temperature 45 DEG C, parsing pressure 6MPa, resolution temperature 55 DEG C, CO
2flow 165L/ hour, cycling extraction is after 3 hours, and collect extract, obtain golden transparent Malania Oleifera Oil 5.28kg, yield is 66.0%.
Embodiment 4
Get Malania oleifera 8kg drying and crushing, cross 20 mesh sieves, obtain Malania oleifera powder, Malania oleifera powder is loaded in airtight extraction kettle and carries out supercritical CO
2fluid extraction, extraction conditions is extracting pressure 40MPa, extraction temperature 45 DEG C, parsing pressure 6MPa, resolution temperature 55 DEG C, CO
2flow 200L/ hour, cycling extraction is after 2 hours, and collect extract, obtain golden transparent Malania Oleifera Oil 5.37kg, yield is 67.1%.
Embodiment 5
Get Malania oleifera 8kg drying and crushing, cross 18 mesh sieves, obtain Malania oleifera powder, Malania oleifera powder is loaded in airtight extraction kettle and carries out supercritical CO
2fluid extraction, extraction conditions is extracting pressure 35MPa, extraction temperature 55 DEG C, parsing pressure 10MPa, resolution temperature 65 DEG C, CO
2flow 180L/ hour, cycling extraction is after 4 hours, and collect extract, obtain golden transparent Malania Oleifera Oil 5.31kg, yield is 66.4%.
Embodiment 6 is Malania oleifera grinding particle size preferably
Get Malania oleifera 4 parts, every part of 8kg, drying and crushing, sieves by table 1 granularity, obtains Malania oleifera powder, loaded in airtight extraction kettle by Malania oleifera powder and carry out supercritical CO respectively
2fluid extraction, extraction conditions is extracting pressure 35MPa, extraction temperature 50 DEG C, parsing pressure 8MPa, resolution temperature 60 DEG C, CO
2flow 180L/ hour, cycling extraction 2 hours, the results are shown in Table 1.
The preferred result of table 1 granularity
As known from Table 1: pulverized by Malania oleifera as granularity 8 ~ 20 object powder, the appearance luster of fruit oil is better, and oil pump capacity is more; When granularity is lower than 8 order, oil pump capacity is few; When granularity is higher than 20 order, the appearance luster of oil is influenced.
Embodiment 7: preferably extracting pressure
Get Malania oleifera 4 parts, every part of 8kg, respectively drying and crushing, cross 16 mesh sieves, obtain Malania oleifera powder, Malania oleifera powder is loaded in airtight extraction kettle and carries out supercritical CO
2fluid extraction, extraction conditions is for extracting pressure is by set by table 2, and extraction temperature 50 DEG C, resolves pressure 7MPa, resolution temperature 55 DEG C, CO
2flow 170L/ hour, cycling extraction 3 hours, the results are shown in Table 2.
The preferred result of table 2 extracting pressure
As known from Table 2: when extracting pressure is 25 ~ 40Mpa, oil pump capacity is many, the appearance luster of oil is good; When extracting pressure is 23Mpa, oil pump capacity is few; When extracting pressure is up to 42Mpa, the appearance luster of oil is influenced.
Embodiment 8: the quality evalution of Malania Oleifera Oil
Get Malania oleifera 8kg drying and crushing, cross 12 mesh sieves, obtain Malania oleifera powder, Malania oleifera powder is loaded in airtight extraction kettle and carries out supercritical CO
2fluid extraction, extraction conditions is extracting pressure 35MPa, extraction temperature 45 DEG C, parsing pressure 6MPa, resolution temperature 55 DEG C, CO
2flow 180L/ hour, cycling extraction is after 3 hours, and collect extract, obtain golden transparent Malania Oleifera Oil 5.34kg, yield is 66.8%.
Separately get Malania oleifera 300g drying and crushing, cross 12 mesh sieves, obtain Malania oleifera powder, get Malania oleifera powder, according to " Ding Junfeng; Cao Jianhua; woods is built superfine. the technical study [J] of ultrasonic-assisted extraction malania oleifera fruit oil. food science and technology, 2008,33 (11): 170-173 " extract, obtain golden transparent colloidal solution 173.4g, yield 57.8%.
(1) supercritical CO is compared
2proterties, the proterties of the dregs of a decoction, the oil-collecting ratio of the Malania Oleifera Oil of extraction and Petroleum ether extraction, and adopt gas chromatograph (7890A, U.S. Agilent) to measure the content of peripheral nerve acid, the results are shown in Table 3.
The comparison of table 3 Different Extraction Method Malania Oleifera Oil proterties, yield and peripheral nerve acid content
Know from table 3 result: supercritical CO
2extract more than Petroleum ether extraction oil pump capacity, the appearance luster of oil is good, and peripheral nerve acid content is higher.
(2) adopt gas chromatograph-mass spectrometer (HP6890GC/5973MS, Hewlett-Packard of the U.S.) respectively to supercritical CO
2the Malania Oleifera Oil of extraction and Petroleum ether extraction has carried out lipid acid composition GC-MS and has analyzed, the Malania Oleifera Oil of two kinds of method gained is basically identical on lipid acid composition, primarily of 12 kinds of fatty acid component compositions such as oleic acid, 22 carbon monoenoic acids and cis-15-tetracosa carbon monoenoic acid, but supercritical CO
2the Selacholeic acid relative content of the Malania Oleifera Oil of extraction is higher, the results are shown in Table 4.
The GC-MS of table 4 two kinds of extracting method gained Malania Oleifera Oils analyzes
(3) by the fat in the Pharmacopoeia of the People's Republic of China 2010 editions annex VII A, a VII F, VII C, IX N and IX P and fatty oil assay method, respectively to supercritical CO
2the each physical and chemical index of Malania Oleifera Oil of extraction and Petroleum ether extraction measures, and the results are shown in Table 5.
The quality evaluation result of table 5 two kinds of extracting method gained Malania Oleifera Oils
As known from Table 5, supercritical CO
2acid number and the peroxide value of the Malania Oleifera Oil of extraction are lower, and quality is better than Petroleum ether extraction.
Claims (1)
1. a supercritical CO
2the method of fluid extraction Malania Oleifera Oil, is characterized in that comprising the following steps: (1), by Malania oleifera drying and crushing, is crossed 8 ~ 20 mesh sieves, obtained Malania oleifera powder; (2) Malania oleifera powder is loaded in airtight extraction kettle carry out supercritical CO
2fluid extraction, extraction conditions is extracting pressure 25 ~ 40MPa, extraction temperature 45 ~ 55 DEG C, parsing pressure 6 ~ 10MPa, resolution temperature 55 ~ 65 DEG C, and cycling extraction, after 2 ~ 4 hours, is collected extract, obtained Malania Oleifera Oil.
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Cited By (5)
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| CN105037133A (en) * | 2015-08-17 | 2015-11-11 | 浙江大学 | Method of extracting nervonic acid from malania oleifera |
| CN107267315A (en) * | 2017-06-02 | 2017-10-20 | 南阳师范学院 | A kind of cinnamomum camphora soap and preparation method thereof |
| CN107445826A (en) * | 2017-07-25 | 2017-12-08 | 天津泽达天健科技有限公司 | A kind of preparation method of neural acid esters |
| CN107822136A (en) * | 2017-10-30 | 2018-03-23 | 张文晋 | A kind of raw-food material and its extracting method containing high content nervonic acid |
| CN110331043A (en) * | 2019-07-31 | 2019-10-15 | 云南天宏香精有限公司 | A kind of mouth containing flavouring essence for tobacco and its preparation method and application |
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Cited By (6)
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| CN105037133A (en) * | 2015-08-17 | 2015-11-11 | 浙江大学 | Method of extracting nervonic acid from malania oleifera |
| CN107267315A (en) * | 2017-06-02 | 2017-10-20 | 南阳师范学院 | A kind of cinnamomum camphora soap and preparation method thereof |
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| CN110331043A (en) * | 2019-07-31 | 2019-10-15 | 云南天宏香精有限公司 | A kind of mouth containing flavouring essence for tobacco and its preparation method and application |
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Application publication date: 20150520 |