CN106045845A - Method for extracting linolenic acid from macrotermes barneyi light - Google Patents
Method for extracting linolenic acid from macrotermes barneyi light Download PDFInfo
- Publication number
- CN106045845A CN106045845A CN201610385954.8A CN201610385954A CN106045845A CN 106045845 A CN106045845 A CN 106045845A CN 201610385954 A CN201610385954 A CN 201610385954A CN 106045845 A CN106045845 A CN 106045845A
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- Prior art keywords
- linolenic acid
- macrotermes barneyi
- barneyi light
- macrotermes
- vacuum
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to a solvent extraction process, in particular to a method for extracting linolenic acid from macrotermes barneyi light. The method comprises the steps that fresh macrotermes barneyi light is taken, subjected to vacuum freeze-drying and then smashed into 420-mesh powder, sodium bicarbonate is added to the macrotermes barneyi light powder according to the mass ratio of 2:100, the mixture is mixed and stirred to be uniform, then the macrotermes barneyi light powder is put in an extraction kettle, supercritical CO2 with the pressure of 7.2-7.5 Mpa and the temperature of 32-35 DEG C is injected after the extraction kettle is sealed, extraction is conducted for 22-25 minutes, the powder enters a vacuum rectifying tower after separation of CO2, and linolenic acid is obtained after rectification is conducted at the temperature of 20-22 DEG C and the pressure of 8 Mpa. The linolenic acid extraction process is simple, the linolenic acid extraction rate is obviously increased, and the linolenic acid purity is obviously improved.
Description
Technical field
The present invention relates to a kind of solvent extraction technology, be specifically related to one from Macrotermes barneyi Light, extract linolenic side
Method.
Background technology
Macrotermes barneyi Light, belongs to the one of Coptotermes formosanus Shtrari., internal containing abundant nutrition and bioactive substance, through modern section
Learning and confirm, termite body is contained within 18 kinds of aminoacid, and wherein 8 kinds of aminoacid necessary to human body, queen and ant ovum are containing aminoacid
Many, most amino acid whose content exceed egg powder, contrast with the amino acid content of egg powder, and Macrotermes barneyi Light is except lysine, bright
Outside propylhomoserin, phenylalanine, glutamic acid, arginine, remaining amino acid content is above egg powder, wherein possibly together with abundant insatiable hunger
And fatty acid, such as linolenic acid, yet there are no from Macrotermes barneyi Light, extract linolenic technique, and existing linolenic acid extracts
Method exists that step is complicated, requirement of experiment is higher more, the shortcoming that solvent easily remains, product purity is the highest.
Summary of the invention
It is an object of the invention to provide one from Macrotermes barneyi Light, extract linolenic method.
One extracts linolenic method from Macrotermes barneyi Light, and the method is:
Take fresh Macrotermes barneyi Light, put into the vacuum cold tank that vacuum is 30-35pa, keep 35-40 to divide at-2 ~-3 DEG C
Zhong Hou, cools the temperature to rapidly-30 ~-35 DEG C, keeps 1-1.2 hour；
Macrotermes barneyi Light is crushed to 420 mesh；
Press the mass ratio interpolation sodium bicarbonate mixing and stirring of 2:100 to Macrotermes barneyi Light powder after, Macrotermes barneyi Light powder is put
Entering in extraction kettle, after sealing, injection pressure is 7.2-7.5Map, and temperature is the supercritical CO 2 of 32-35 DEG C, extracts 22-25 minute,
After separating CO2, entering in vacuum rectifying tower, at 20-22 DEG C, under 8Mpa, rectification obtains linolenic acid.
Linolenic acid extraction process of the present invention is simple, by add sodium bicarbonate can significantly improve linolenic extraction ratio in
Pressure rectification can significantly improve linolenic purity, and linolenic acid extraction ratio is at 99.6%-99.8%, and purity, up to 99-99.2%, is produced
Product acid value at 0.162-0.168 mgKOH/g, peroxide value at 1.46-1.52 meq/kg, no solvent residue in product.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be described,
Embodiment 1, one extract linolenic method from Macrotermes barneyi Light, and the method is:
Take fresh Macrotermes barneyi Light, put into the vacuum cold tank that vacuum is 30pa ,-2 ~ DEG C at keep 35 minutes after, fast
Speed cools the temperature to-30 DEG C, keeps 1 hour；
Macrotermes barneyi Light is crushed to 420 mesh；
Press the mass ratio interpolation sodium bicarbonate mixing and stirring of 2:100 to Macrotermes barneyi Light powder after, Macrotermes barneyi Light powder is put
Entering in extraction kettle, after sealing, injection pressure is 7.2Map, and temperature is the supercritical CO 2 of 32 DEG C, extracts 22 minutes, separates CO2
After, enter in vacuum rectifying tower, at 20 DEG C, under 8Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 99.61%, and purity is up to 99%, and product acid value is in 0.1622 mgKOH/g, mistake
Oxidation number at 1.468 meq/kg, no solvent residue in product.
Embodiment 2, one extract linolenic method from Macrotermes barneyi Light, and the method is:
Take fresh Macrotermes barneyi Light, put into the vacuum cold tank that vacuum is 32pa, after keeping 36 minutes at-2.2 DEG C, fast
Speed cools the temperature to-31 DEG C, keeps 1.05 hours；
Macrotermes barneyi Light is crushed to 420 mesh；
Press the mass ratio interpolation sodium bicarbonate mixing and stirring of 2:100 to Macrotermes barneyi Light powder after, Macrotermes barneyi Light powder is put
Entering in extraction kettle, after sealing, injection pressure is 7.28Map, and temperature is the supercritical CO 2 of 33 DEG C, extracts 23 minutes, separates CO2
After, enter in vacuum rectifying tower, at 20.5 DEG C, under 8Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 99.69%, purity up to 99.04%, product acid value at 0.1653 mgKOH/g,
Peroxide value at 1.477 meq/kg, no solvent residue in product.
Embodiment 3, one extract linolenic method from Macrotermes barneyi Light, and the method is:
Take fresh Macrotermes barneyi Light, put into the vacuum cold tank that vacuum is 34pa, after keeping 37 minutes at-2.5 DEG C, fast
Speed cools the temperature to-33 DEG C, keeps 1.08 hours；
Macrotermes barneyi Light is crushed to 420 mesh；
Press the mass ratio interpolation sodium bicarbonate mixing and stirring of 2:100 to Macrotermes barneyi Light powder after, Macrotermes barneyi Light powder is put
Entering in extraction kettle, after sealing, injection pressure is 7.42Map, and temperature is the supercritical CO 2 of 34 DEG C, extracts 24 minutes, separates CO2
After, enter in vacuum rectifying tower, at 21 DEG C, under 8Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 99.74%, purity up to 99.15%, product acid value at 0.1662 mgKOH/g,
Peroxide value at 1.507 meq/kg, no solvent residue in product.
Embodiment 4, one extract linolenic method from Macrotermes barneyi Light, and the method is:
Take fresh Macrotermes barneyi Light, put into the vacuum cold tank that vacuum is 35pa, after keeping 40 minutes at-3 DEG C, rapidly
Cool the temperature to-35 DEG C, keep 1.2 hours；
Macrotermes barneyi Light is crushed to 420 mesh；
Press the mass ratio interpolation sodium bicarbonate mixing and stirring of 2:100 to Macrotermes barneyi Light powder after, Macrotermes barneyi Light powder is put
Entering in extraction kettle, after sealing, injection pressure is 7.5Map, and temperature is the supercritical CO 2 of 35 DEG C, extracts 25 minutes, separates CO2
After, enter in vacuum rectifying tower, at 22 DEG C, under 8Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 99.8%, and purity is up to 99.2%, and product acid value is at 0.168mgKOH/g, peroxide
Change value at 1.52 meq/kg, no solvent residue in product.
The present invention will be described to combine concrete contrast test further below:
Experimental group, takes fresh Macrotermes barneyi Light, puts into the vacuum cold tank that vacuum is 33pa, keeps 38 points at-2.8 DEG C
Zhong Hou, cools the temperature to rapidly-34 DEG C, keeps 1.16 hours；
Macrotermes barneyi Light is crushed to 420 mesh；
Press the mass ratio interpolation sodium bicarbonate mixing and stirring of 2:100 to Macrotermes barneyi Light powder after, Macrotermes barneyi Light powder is put
Entering in extraction kettle, after sealing, injection pressure is 7.46Map, and temperature is the supercritical CO 2 of 34.5 DEG C, extracts 24 minutes, separates
After CO2, entering in vacuum rectifying tower, at 21.6 DEG C, under 8Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 99.71%, and purity is up to 99.136%.
Matched group 1: take fresh Macrotermes barneyi Light, puts into the vacuum cold tank that vacuum is 33pa, protects at-2.8 DEG C
After holding 38 minutes, cool the temperature to rapidly-34 DEG C, keep 1.16 hours；
Macrotermes barneyi Light is crushed to 420 mesh；
Inserting in extraction kettle by Macrotermes barneyi Light powder, after sealing, injection pressure is 7.46Map, and temperature is the supercritical of 34.5 DEG C
CO2, extracts 24 minutes, after separating CO2, enters in vacuum rectifying tower, and at 21.6 DEG C, under 8Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 90.93%, and purity is up to 99.128%.
Matched group 2: take fresh Macrotermes barneyi Light, puts into the vacuum cold tank that vacuum is 33pa, protects at-2.8 DEG C
After holding 38 minutes, cool the temperature to rapidly-34 DEG C, keep 1.16 hours；
Macrotermes barneyi Light is crushed to 420 mesh；
Inserting in extraction kettle by Macrotermes barneyi Light powder, after sealing, injection pressure is 7.46Map, and temperature is the supercritical of 34.5 DEG C
CO2, extracts 24 minutes, after separating CO2, enters in vacuum rectifying tower, and at 21.6 DEG C, under 7Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 90.93%, and purity is up to 81.14%.
Matched group 3: take fresh Macrotermes barneyi Light, puts into the vacuum cold tank that vacuum is 33pa, protects at-2.8 DEG C
After holding 38 minutes, cool the temperature to rapidly-34 DEG C, keep 1.16 hours；
Macrotermes barneyi Light is crushed to 420 mesh；
Inserting in extraction kettle by Macrotermes barneyi Light powder, after sealing, injection pressure is 7.46Map, and temperature is the supercritical of 34.5 DEG C
CO2, extracts 24 minutes, after separating CO2, enters in vacuum rectifying tower, and at 21.6 DEG C, under 6Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 90.93%, and purity is up to 83.08%.
Matched group 4: take fresh Macrotermes barneyi Light, puts into the vacuum cold tank that vacuum is 33pa, protects at-2.8 DEG C
After holding 38 minutes, cool the temperature to rapidly-34 DEG C, keep 1.16 hours；
Macrotermes barneyi Light is crushed to 420 mesh；
Inserting in extraction kettle by Macrotermes barneyi Light powder, after sealing, injection pressure is 7.46Map, and temperature is the supercritical of 34.5 DEG C
CO2, extracts 24 minutes, after separating CO2, enters in vacuum rectifying tower, and at 21.6 DEG C, under 5Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 90.93%, and purity is up to 82.17%.
Matched group 5: take fresh Macrotermes barneyi Light, puts into the vacuum cold tank that vacuum is 33pa, protects at-2.8 DEG C
After holding 38 minutes, cool the temperature to rapidly-34 DEG C, keep 1.16 hours；
Macrotermes barneyi Light is crushed to 420 mesh；
Inserting in extraction kettle by Macrotermes barneyi Light powder, after sealing, injection pressure is 7.46Map, and temperature is the supercritical of 34.5 DEG C
CO2, extracts 24 minutes, after separating CO2, enters in vacuum rectifying tower, and at 21.6 DEG C, under 9Mpa, rectification obtains linolenic acid.
Under the conditions of Gai, linolenic acid extraction ratio be 90.93%, and purity is up to 80.92%.
Claims (1)
1. one kind is extracted linolenic method from Macrotermes barneyi Light, it is characterised in that the method is:
Take fresh Macrotermes barneyi Light, put into the vacuum cold tank that vacuum is 30-35pa, keep 35-40 to divide at-2 ~-3 DEG C
Zhong Hou, cools the temperature to rapidly-30 ~-35 DEG C, keeps 1-1.2 hour；
Macrotermes barneyi Light is crushed to 420 mesh；
Press the mass ratio interpolation sodium bicarbonate mixing and stirring of 2:100 to Macrotermes barneyi Light powder after, Macrotermes barneyi Light powder is put
Entering in extraction kettle, after sealing, injection pressure is 7.2-7.5Map, and temperature is the supercritical CO 2 of 32-35 DEG C, extracts 22-25 minute,
After separating CO2, entering in vacuum rectifying tower, at 20-22 DEG C, under 8Mpa, rectification obtains linolenic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610385954.8A CN106045845A (en) | 2016-06-03 | 2016-06-03 | Method for extracting linolenic acid from macrotermes barneyi light |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610385954.8A CN106045845A (en) | 2016-06-03 | 2016-06-03 | Method for extracting linolenic acid from macrotermes barneyi light |
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| Publication Number | Publication Date |
|---|---|
| CN106045845A true CN106045845A (en) | 2016-10-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610385954.8A Pending CN106045845A (en) | 2016-06-03 | 2016-06-03 | Method for extracting linolenic acid from macrotermes barneyi light |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101121654A (en) * | 2007-07-24 | 2008-02-13 | 山东大学 | Supercritical CO2 extraction separation purification method for silkworm chrysalis alpha-linolenic acid |
| CN101519626A (en) * | 2008-02-25 | 2009-09-02 | 景凯 | Process for extracting Alpha-linolenic acid from silkworm pupa crude oil |
| CN103695182A (en) * | 2013-05-16 | 2014-04-02 | 黑龙江惠民兴生物科技有限公司 | Method for supercritical extraction of linolenic acid |
-
2016
- 2016-06-03 CN CN201610385954.8A patent/CN106045845A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101121654A (en) * | 2007-07-24 | 2008-02-13 | 山东大学 | Supercritical CO2 extraction separation purification method for silkworm chrysalis alpha-linolenic acid |
| CN101519626A (en) * | 2008-02-25 | 2009-09-02 | 景凯 | Process for extracting Alpha-linolenic acid from silkworm pupa crude oil |
| CN103695182A (en) * | 2013-05-16 | 2014-04-02 | 黑龙江惠民兴生物科技有限公司 | Method for supercritical extraction of linolenic acid |
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Application publication date: 20161026 |
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