CN111423933A - Supercritical extraction method of truffle oil - Google Patents
Supercritical extraction method of truffle oil Download PDFInfo
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- CN111423933A CN111423933A CN202010183441.5A CN202010183441A CN111423933A CN 111423933 A CN111423933 A CN 111423933A CN 202010183441 A CN202010183441 A CN 202010183441A CN 111423933 A CN111423933 A CN 111423933A
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- truffle
- supercritical extraction
- raw material
- extraction method
- oil
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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
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- 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
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/16—Refining fats or fatty oils by mechanical means
Abstract
The invention belongs to the technical field of truffle oil extraction, and discloses a supercritical extraction method of truffle oil. The extraction method of the truffle oil provided by the invention does not use organic solvents such as n-hexane, petroleum ether and the like, so that the problem of residue of the organic solvents can be solved, meanwhile, the truffle oil can be effectively extracted, the extraction temperature is always controlled below 60 ℃, the loss of heat-sensitive nutrient components in the truffle oil can be effectively reduced, and the obtained truffle oil has good quality and good stability.
Description
Technical Field
The invention belongs to the technical field of truffle oil extraction, and particularly relates to a supercritical extraction method of truffle oil.
Background
Currently, the closest prior art: aiming at the fact that the truffle oil is not extracted effectively at the present stage, the common methods of steam distillation and squeezing cannot extract effectively, and the truffle oil contains more impurities after being extracted by a solvent extraction method and is difficult to remove the residual organic solvent.
In summary, the problems of the prior art are as follows: the steam distillation and squeezing methods cannot effectively extract the truffle oil, the solvent extraction method has more impurities, and the residual organic solvent is difficult to remove.
The difficulty of solving the technical problems is as follows: steam distillation is carried out by introducing steam into organic substance which is insoluble or poorly soluble in water but has a certain volatility, and distilling the organic substance with steam at a temperature lower than 100 ℃. The heat-sensitive raw materials are easy to be heated and coked, the components of the heat-sensitive raw materials are changed due to oxidation, polymerization reaction and the like, and the aromatic odor of the obtained volatile oil can be changed; some water-miscible materials cannot be extracted efficiently; if the impurities in the reaction mixture are volatile, the purity of the extracted volatile oil cannot be ensured; the yield is low, the required time is long, and the use value of the volatile oil is reduced. Among the steam distillation equipment, because steam generator hardly guarantees the steam supply that lasts, the long-neck round bottom flask that uses in the distillation can produce certain influence to volatile oil extraction, and atmospheric pressure is big or the condensation effect is not good etc. can lead to oil-water separation not good, accepts that volatile oil can volatilize in the bottle and go bad in the receiving process, and this has all led to it can not effectively draw truffle oil. The solvent extraction method is simple and easy to implement, but chemical reagents such as dichloromethane and diethyl ether are mostly used, the types of the obtained compounds are few, for example, the extracted apricot mainly contains alkane compounds, the contribution rate of the alkane compounds to the aroma is small, the alkane is the main component forming the surface wax, the truffle oil obtained after extraction contains more wax, and the impurities are difficult to remove.
The significance of solving the technical problems is as follows: truffle oil belongs to heat-sensitive substances, and fragrant substances of truffle oil are easy to volatilize under the heating condition. There is an urgent need for an extraction method that prevents oxidation, pyrolysis and improves quality. The supercritical carbon dioxide extraction method has the advantages of low extraction temperature, no solvent residue, high extract quality and the like. Meanwhile, the truffle oil has inherent fragrance and taste of oil according to the sensory requirements of the national edible oil standard, is free from peculiar smell, clear and transparent, solves the technical problems, can fully extract truffle oil, improves the economic value of truffle oil, removes impurities and organic solvents, and obtains high-quality edible oil which has no solvent residue and meets the requirements of environmental protection.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a supercritical extraction method of truffle oil.
The invention is realized in such a way that the supercritical extraction method of truffle oil comprises the following steps:
(1) slicing fresh truffle, and then carrying out pretreatment, wherein the pretreatment is enzyme treatment or ultrasonic treatment to obtain a treated truffle raw material;
(2) drying the pretreated truffle raw material, crushing the dried truffle, and grading the obtained powder to obtain the raw material;
(3) transferring the truffle powder obtained by the treatment in the step (2) into a supercritical extraction kettle, and extracting and separating by using carbon dioxide as a supercritical fluid and ethanol as an entrainer;
(4) collecting the extract, and freezing in a freezing chamber;
(5) centrifuging the extract after freezing, collecting supernatant and removing precipitate;
(6) the extract is subjected to reduced pressure treatment to separate truffle oil.
Further, in the step (1), the types of enzymes used for the enzyme treatment of the truffle raw material are cellulase, pectinase, protease, amylase and the like, and include but are not limited to one or more of the above; the sonication conditions used were: the ultrasonic time is 5-30 min, the ultrasonic temperature is 20-60 ℃, and the ultrasonic frequency is 2 times.
Further, in the step (2), the method for drying the truffle raw material is microwave, baking, drying, vacuum freeze-drying and the like, and includes, but is not limited to, one or more of the above.
Further, in the step (2), the particle size of the ground truffle raw material is 10-80 meshes.
Further, in the step (3), the extraction temperature in the supercritical extraction kettle is 30-60 ℃, the extraction pressure is 10-35 MPa, and the amount of carbon dioxide/amount of truffle raw material is 1-30 (L/min)/1 g.
Further, in the step (3), the dosage of the ethanol entrainer/truffle raw material is 0.2-4g/1 g.
Further, in the step (4), the freezing temperature in the freezing treatment is between-17 ℃ and 15 ℃.
Further, the separation mode of the truffle oil in the step (6) adopts a film evaporation device, a molecular distillation device, a countercurrent separation device and the like, and comprises but is not limited to one or more of the above devices.
In summary, the advantages and positive effects of the invention are:
the extraction method of the truffle oil provided by the invention does not use organic solvents such as n-hexane, petroleum ether and the like, so that the problem of residue of the organic solvents can be solved, meanwhile, the truffle oil can be effectively extracted, the extraction temperature is always controlled below 60 ℃, the loss of heat-sensitive nutrient components in the truffle oil can be effectively reduced, and the obtained truffle oil has good quality and good stability.
Drawings
Fig. 1 is a flow chart of a supercritical extraction method of truffle oil according to an embodiment of the present invention.
Fig. 2 is a diagram of the effect of truffle oil provided by the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 1, the supercritical extraction method of truffle oil provided by the embodiment of the present invention includes:
s101: slicing the fresh truffle, and then carrying out pretreatment, wherein the pretreatment is enzyme treatment or ultrasonic treatment to obtain a treated truffle raw material.
S102: and drying the pretreated truffle raw material, crushing the dried truffle, and grading the obtained powder to obtain the raw material.
S103: transferring the truffle powder obtained by the treatment in the step into a supercritical extraction kettle, and extracting and separating by using carbon dioxide as a supercritical fluid and ethanol as an entrainer.
S104: collecting the extract, and freezing in a freezing chamber.
S105: after freezing, the extract was centrifuged, and the supernatant was collected and the precipitate was discarded.
S106: the extract is subjected to reduced pressure treatment to separate truffle oil.
In the step (1) in the embodiment of the present invention, the types of enzymes used in the enzyme treatment of the truffle raw material are cellulase, pectinase, protease, amylase, etc., including but not limited to one or more of the above; the sonication conditions used were: the ultrasonic time is 5-30 min, the ultrasonic temperature is 20-60 ℃, and the ultrasonic frequency is 2 times
In the step (2) in the embodiment of the present invention, the method for drying the truffle raw material is microwave, baking, drying, vacuum freeze-drying, etc., including but not limited to one or more of the above.
In the step (2) in the embodiment of the invention, the particle size of the ground truffle raw material is 10-80 meshes.
In the step (3) in the embodiment of the invention, the extraction temperature in the supercritical extraction kettle is 30-60 ℃, the extraction pressure is 10-35 MPa, and the dosage of carbon dioxide/the dosage of truffle raw material is 1-30/1.
In the step (3) in the embodiment of the invention, the dosage of the ethanol entrainer/the dosage of the truffle raw material is 0.2-4/1.
In the step (4) in the examples of the present invention, the freezing temperature in the freezing treatment is between-17 ℃ and 15 ℃.
In the embodiment of the present invention, the separation mode of the truffle oil in step (6) adopts a thin film evaporation device, a molecular distillation device, a countercurrent separation device, and the like, including but not limited to one or more of the above.
The technical solution of the present invention is described in detail below with reference to examples.
Example 1:
(1) cleaning fresh truffle, cutting into slices of about 3mm, dissolving enzyme in water, mixing with slices, reacting at 40 deg.C for 2 hr, inactivating enzyme, and drying.
(2) Pulverizing the truffle raw material to obtain 60-mesh truffle powder.
(3) And transferring the pretreated truffle raw material into a supercritical extraction kettle, and extracting and separating by using carbon dioxide as a supercritical extraction fluid and anhydrous ethanol as an entrainer. The extraction temperature is 50 ℃, the extraction pressure is 30MPa, the entrainer proportion is 1:1, the entrainer is pumped into the extraction reaction kettle by an entrainer pump for four times, and the carbon dioxide consumption/raw material quantity in the whole extraction process is 10: 1.
(4) The extract after completion of the extraction was refrigerated at 4 ℃ for 24 hours.
(5) The cold storage liquid was put into a centrifuge and centrifuged at 5000 rpm. The residue was discarded and the supernatant collected.
(6) Concentrating the supernatant at 50 deg.C with rotary evaporator to obtain truffle oil.
Calculating the oil yield:
the oil yield is × 100% of the mass of truffle oil/truffle raw material obtained by concentration and extraction.
The oil yield of the truffle oil in the embodiment is 1.2 percent through detection.
Example 2:
(1) cleaning fresh truffle, cutting into slices of about 3mm, performing ultrasonic treatment at 35 deg.C for 2 times, each for 20min, and drying.
(2) Pulverizing the truffle raw material to obtain 60-mesh truffle powder.
(3) And transferring the pretreated truffle raw material into a supercritical extraction kettle, and extracting and separating by using carbon dioxide as a supercritical extraction fluid and anhydrous ethanol as an entrainer. The extraction temperature is 45 ℃, the extraction pressure is 35MPa, the entrainer proportion is 1:1, the entrainer is pumped into the extraction reaction kettle by an entrainer pump for four times, and the carbon dioxide consumption/raw material quantity in the whole extraction process is 12: 1.
(4) The extract after completion of the extraction was refrigerated at 4 ℃ for 24 hours.
(5) The cold storage liquid was put into a centrifuge and centrifuged at 5000 rpm. The residue was discarded and the supernatant collected.
(6) Concentrating the supernatant at 50 deg.C with rotary evaporator to obtain truffle oil.
Calculating the oil yield:
the oil yield is × 100% of the mass of truffle oil/truffle raw material obtained by concentration and extraction.
The oil yield of the truffle oil in the embodiment is 1.1 percent through detection.
As shown in fig. 2, an effect graph of truffle oil provided by the embodiment of the invention is shown, wherein a is truffle oil at 4 ℃; b is truffle oil at-17 deg.C; c is truffle oil finished product.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. The supercritical extraction method of truffle oil is characterized by comprising the following steps:
(1) slicing fresh truffle, and then carrying out pretreatment, wherein the pretreatment is enzyme treatment or ultrasonic treatment to obtain a treated truffle raw material;
(2) drying the pretreated truffle raw material, crushing the dried truffle, and grading the obtained powder to obtain the raw material;
(3) transferring the truffle powder obtained by the treatment in the step (2) into a supercritical extraction kettle, and extracting and separating by using carbon dioxide as a supercritical fluid and ethanol as an entrainer;
(4) collecting the extract, and freezing in a freezing chamber;
(5) centrifuging the extract after freezing, collecting supernatant and removing precipitate;
(6) the extract is subjected to reduced pressure treatment to separate truffle oil.
2. The supercritical extraction method of truffle oil according to claim 1, wherein in step (1), the types of enzymes used for the enzyme treatment of truffle raw material are cellulase, pectinase, protease and amylase, including but not limited to one or more of the above; the sonication conditions used were: the ultrasonic time is 5-30 min, the ultrasonic temperature is 20-60 ℃, and the ultrasonic frequency is 2 times.
3. The supercritical extraction method of truffle oil according to claim 1, wherein in step (2), the truffle raw material is dried by one of microwave, oven drying and vacuum freeze drying.
4. The supercritical extraction method of truffle oil according to claim 1, wherein in step (2), the grain size of the truffle raw material is 10-80 mesh.
5. The supercritical extraction method of truffle oil according to claim 1, wherein in step (3), the extraction temperature in the supercritical extraction kettle is 30-60 ℃, the extraction pressure is 10-35 MPa, and the amount of carbon dioxide per truffle raw material is 1-30/1.
6. The supercritical extraction process of truffle oil according to claim 1, wherein in step (3), the amount of ethanol entrainer/truffle feedstock is 0.2-4/1.
7. The supercritical extraction method of truffle oil according to claim 1, wherein the freezing temperature in the freezing process in step (4) is-17 ℃ to 15 ℃.
8. The supercritical extraction method of truffle oil according to claim 1, wherein the truffle oil is separated in step (6) by one of a thin film evaporation device, a molecular distillation device and a counter current separation device.
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| CN202010183441.5A CN111423933A (en) | 2020-03-16 | 2020-03-16 | Supercritical extraction method of truffle oil |
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| CN202010183441.5A CN111423933A (en) | 2020-03-16 | 2020-03-16 | Supercritical extraction method of truffle oil |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2764778A1 (en) * | 1997-06-24 | 1998-12-24 | Truffes Du Terroir | PROCESS AND PLANT FOR TRANSFERRING FLAVORED TRUFFLE AROMAS WITH A SUPER CRITICAL CARBON DIOXIDE |
| CN101077989A (en) * | 2007-06-19 | 2007-11-28 | 西北农林科技大学 | Supercritical extraction method for India truffle oil |
| CN101933540A (en) * | 2010-09-17 | 2011-01-05 | 香格里拉县圣宝食品进出口有限责任公司 | Edible wild fungus oil |
| EP3772287A1 (en) * | 2019-08-07 | 2021-02-10 | Fortunati Alfonso Di Fortunati Danilo - Tartufi Freschi e Conservati | Production process of a food product with truffle aromas |
-
2020
- 2020-03-16 CN CN202010183441.5A patent/CN111423933A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2764778A1 (en) * | 1997-06-24 | 1998-12-24 | Truffes Du Terroir | PROCESS AND PLANT FOR TRANSFERRING FLAVORED TRUFFLE AROMAS WITH A SUPER CRITICAL CARBON DIOXIDE |
| WO1998058553A2 (en) * | 1997-06-24 | 1998-12-30 | Truffes Du Terroir (S.A.R.L.) | Method and installation for transferring truffle aromas to a liquid base using supercritical carbon dioxide |
| CN101077989A (en) * | 2007-06-19 | 2007-11-28 | 西北农林科技大学 | Supercritical extraction method for India truffle oil |
| CN101933540A (en) * | 2010-09-17 | 2011-01-05 | 香格里拉县圣宝食品进出口有限责任公司 | Edible wild fungus oil |
| EP3772287A1 (en) * | 2019-08-07 | 2021-02-10 | Fortunati Alfonso Di Fortunati Danilo - Tartufi Freschi e Conservati | Production process of a food product with truffle aromas |
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Effective date of registration: 20210421 Address after: Wuhua District of Yunnan city in Kunming Province, 650221 Yun Road No. 9 Applicant after: INSTITUTE OF AGRO-PRODUCTS PROCESSING YAAS Address before: 650224 Yunnan Province, Panlong District of Kunming City Bailong Temple No. 300 Applicant before: SOUTHWEST FORESTRY University |