KR20170000280A - The non-destructive extraction and analysis method for food sample - Google Patents
The non-destructive extraction and analysis method for food sample Download PDFInfo
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- KR20170000280A KR20170000280A KR1020150089314A KR20150089314A KR20170000280A KR 20170000280 A KR20170000280 A KR 20170000280A KR 1020150089314 A KR1020150089314 A KR 1020150089314A KR 20150089314 A KR20150089314 A KR 20150089314A KR 20170000280 A KR20170000280 A KR 20170000280A
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- Prior art keywords
- food
- food sample
- desiccator
- components
- apple
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Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7206—Mass spectrometers interfaced to gas chromatograph
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/02—Food
- G01N33/025—Fruits or vegetables
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
The present invention relates to a method for pretreatment for analyzing components of a food sample, and more particularly, to a non-destructive pretreatment / analysis method for identifying components of food without destroying or changing the original shape and state of the food sample.
As the basis of food research and development is to analyze the components of food samples, consumer interest in various preferences, health orientations, and safety has increased recently, and technologies to qualitatively and quantitatively analyze food ingredients have become more valuable, It is very important for food development.
Analysis of various components such as pesticides, alcohol, sugar, organic acids, volatile organic compounds, trans fatty acids, dioxins, environmental hormones, fats, flavors and fragrance components in pesticides, For the purpose of the experiment, it is necessary to process the sample so that it becomes the optimum measurement condition through the appropriate method before the instrumental measurement according to the purpose of the experiment. This is called sample preparation of the sample. The pretreatment of the sample is carried out in order to separate and concentrate the analyte, to remove and reduce the interference substances in the sample, to remove the sample matrix, and to improve the analysis. Sample preparation not only greatly influences the success of the analysis, It accounts for more than 60%. Among the pretreatment methods of the samples, the adsorption / absorption methods are widely used due to the simplicity and economy of the time and solvent usage.
For example, solid-phase extraction (SPE), solid-phase microextraction (SPME), and stir-bar sorptive extraction (SBSE) techniques are applied to the adsorption / . However, all of these techniques are premised on the pulverization of food samples.
However, there is a need for nondestructive analysis to identify the constituents of food without destroying or changing the original shape and condition of the food sample. However, until now, the composition of the sample is non-destructive There was no way to analyze it.
A problem to be solved by the present invention is to provide a method capable of improving, correcting and supplementing ingredients in a food by examining a result of the nondestructive analysis of a food sample to ensure stability through identification of the ingredients.
Another problem to be solved by the present invention is to provide a method which can reduce the time and effort required for the destruction of a food sample and that does not cause a change in the components during the destruction process.
In addition, a problem to be solved by the present invention is to nondestructively analyze a food sample, to analyze the state of preservation of the value of the food as a commodity, and to provide a method capable of immediately distributing or selling after analysis.
In order to solve the above problems, in one aspect, the present invention relates to (S1) a desiccator in which a food sample can be hermetically sealed, a hollow-formed desiccator and a valve coupled to the hollow of the desiccator Injecting a non-destructive food sample into a target material extraction apparatus including the apparatus;
(S2) saturating a food sample in a substance extraction apparatus; And
(S3) a step of introducing the adsorption / extraction device through the valve of the desiccator into the desiccator, thereby providing a method of non-destructively adsorbing and extracting the components of the food sample.
Object substance extraction device
The object substance extraction device is a device newly designed by the present inventors for non-destructively adsorbing and extracting a substance in a sample. In order to understand the present device, a patent application No. 10-2015-0089251 can be taken into consideration. 10-2015-0089251 are incorporated in the present invention as a whole, but the present invention is not limited thereto.
The object substance extraction device according to the present invention includes a valve coupled to the hollow of the desiccator for opening and closing the seal of the desiccator and the desiccator which can receive the food sample in a hermetically sealed state. Hereinafter, the object substance extracting apparatus according to the present invention will be described in more detail.
In the object substance extracting apparatus according to the present invention, the desiccator includes: a body in which a target object is accommodated; And a cover which can be hermetically coupled to the body and formed with a hollow.
The valve includes: a valve body having a through-hole through which the adsorption / extraction device can pass and communicating with the hollow, and a slide hole formed in the wall across the through-hole and being in contact with the hollow; And a slide member formed with a communication hole which can be selectively communicated with the through hole by sliding movement and inserted into the sliding hole to be slidable. The valve may further include a valve cap for coupling the valve body to the hollow. Further, the slide member may further include a pair of knobs provided at both ends thereof.
In addition, the object substance extracting apparatus according to the present invention may further include an adapter inserted into the hollow of the desiccator and having a through-hole through which a component of the food sample can pass. Further, a through opening may be formed on the side surface of the adapter to prevent the adsorption / extractor from directly contacting the target object. The adapter may have a hollow adapter body having one end rounded to be positioned inside the desiccator through the hollow and the other end protruding to the hollow outside of the desiccator. In addition, one end of the adapter may be clogged with the center portion, and the through-hole may be formed to be inclined to at least one of both sides of the central portion. And a female screw portion formed on the inner circumferential surface of the valve so as to be coupled to the male screw portion formed on the outer circumferential surface of the other end of the adapter.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. Like reference symbols in the drawings denote like elements.
The terms " one side " and " other side " used in this specification may mean a specified side, or do not mean a specified side, but any side of a plurality of sides may be referred to as one side, And the other side is referred to as the other side.
The term " bond " or " connection, " as used herein, is intended to encompass a case in which one member and another member are directly or indirectly connected, And the like.
As used herein, the term " subject matter " includes various objects that can be extracted for analysis, and the term " subject matter " The 'ingredient of the food sample' may include various components such as an agricultural chemical, an alcohol component in a drink or alcohol, a sugar, an organic acid, a volatile organic compound, a trans fatty acid, a dioxin, an environmental hormone, a fat, a volatile component, have.
2 is a schematic exploded perspective view of a substance extracting apparatus according to a first embodiment of the present invention. FIG. 3 is a perspective view of the substance extracting apparatus according to the first embodiment of the present invention. Is a schematic cross-sectional view of a substance extraction apparatus according to a first embodiment of the present invention.
1 to 3, the object
The
The
The
The
The
The
The
The
The
The
FIGS. 4 and 5 are side cross-sectional views respectively showing the process of opening and closing a through hole of a valve in the object substance extracting apparatus according to the first embodiment of the present invention. FIGS. 6 and 7 are cross- FIG. 5 is a top view of a process of opening and closing a through hole of a valve in a material extraction device; FIG.
First, the opening / closing process of the through
The
The
When the sealing of the
The
The
When the through
The
The
Hereinafter, the process of opening and closing the through-hole of the valve will be described with reference to FIGS.
The
When the
When the
The adsorption /
After the through
When the adsorption /
FIG. 8 is a schematic overall perspective view of a substance extraction apparatus according to a second embodiment of the present invention, FIG. 9 is a schematic exploded perspective view of a substance extraction apparatus according to a second embodiment of the present invention, Is a schematic cross-sectional view of a substance extraction apparatus according to a second embodiment of the present invention.
Hereinafter, an operation of extracting a food sample component from the object
A second embodiment of the present invention includes a
The
That is, when the
However, when the
The
The
When the
Since the suction /
The
In particular, the
One end of the adapter
9) may be formed on the outer circumferential surface of the other end of the
The
The
The
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention as defined by the appended claims. Accordingly, such modifications or variations are intended to fall within the scope of the appended claims.
A method of non-destructively adsorbing and extracting components of food samples
A method of non-destructively adsorbing and extracting the components of a food sample using the above-described substance extraction apparatus will be described in detail below.
More particularly, the present invention relates to a substance extracting apparatus (hereinafter, referred to as " substance extracting apparatus ") including a valve coupled to the hollow of a desiccator for opening and closing a seal of a desiccator and a desiccator, Injecting a non-destructive food sample into a target substance extracting apparatus;
(S2) saturating a food sample in a substance extraction apparatus; And
(S3) transferring the adsorption / extraction device into the object substance extraction device.
As used herein, 'non-destructive' means that the original shape of the sample is maintained and the state of the sample is not changed, for example, means that the distribution or sale is immediately possible after analysis. Examples of destruction include, but are not limited to, physical processes such as pulverization, crushing, cutting, and heating.
The term "food sample" in this specification includes, without limitation, natural food raw materials, raw materials for synthetic foods, and processed foods or cooked foods, and the natural food raw materials include, for example, fruits and vegetables, , Peaches, strawberries, and the like. For convenience of explanation, the case where the food sample is an apple is described, but the description limited to the apple does not limit the scope of the present invention.
In the present specification, the 'food sample component' includes various components such as pesticides, alcohol components in beverages or alcohol, sugars, organic acids, volatile organic compounds, trans fatty acids, dioxins, environmental hormones, fats, volatile components, But it is preferably a volatile component, more preferably a volatile perfume component. For example, components known as volatile flavor components of apples may be included (see Table 1).
As a food sample component is injected into a substance extraction device according to the present invention, more specifically, a food sample component is put into the body of the substance extraction device.
In the present specification, "saturation" means that a component of a food sample is contained in the substance extraction apparatus (particularly, a vacuum desiccator) to such an extent that the component of the food sample can be adsorbed and extracted. Which can not be contained within a device (particularly a desiccator). It is preferable that the 'saturation' is carried out at room temperature in order to prevent the denaturation of the food sample component, and the time required may vary depending on the type of food sample, the components to be adsorbed and extracted, and the adsorption / extraction machine.
The adsorption / extraction of the components of the food sample can be performed after the food sample is saturated in the target substance extraction device, but the saturation process and the adsorption / extraction process may be performed at the same time. Therefore, steps (S2) and (S3) may be performed simultaneously or may be performed with a time difference.
In the present specification, the term 'adsorption / extraction device' refers to a device for adsorbing / extracting components of a food sample contained in the air of the object substance extraction device (particularly, desiccator). Various devices known in the art can be used and can be selectively used in consideration of the characteristics of components to be adsorbed and extracted. Examples thereof include a solid-phase extraction (SPE) device, a solid-phase microextraction , A SPME apparatus, a stir-bar sorptive extraction (SBSE) apparatus, and the like. According to a specific embodiment of the present invention, the SPME device is used. The SPME device includes a needle part and a fiber part. For convenience of explanation, the suction / extraction device is an SPME device. It is to be understood that the defined description is not intended to limit the scope of the invention.
In order to prevent denaturation of food sample components, 'adsorption / extraction' is preferably carried out at room temperature, and the time required may vary depending on the type of food sample, the components to be adsorbed / extracted, and the adsorption / extraction equipment. 'Adsorption' follows the principle of equilibrium partitioning between the food sample and the adsorbed material phase.
In another aspect, the present invention provides a method for nondestructively analyzing a component of a food sample, comprising the step of analyzing the adsorbed and extracted components as described above.
Analysis method of adsorbed and extracted components
Various methods for analyzing adsorbed and extracted components known in the art can be used, and for example, HPLC analysis, GC-MS analysis, GC-MSD analysis, and the like can be used. Through this step, adsorbed and extracted food sample components can be analyzed qualitatively or quantitatively.
According to the present invention, there is provided a non-destructive extraction method and analysis method capable of confirming a component (especially a volatile flavor component) of a food without destroying or changing the original shape and state of a food sample. It is possible to improve, correct and supplement the components in the food, to reduce the time and effort required for the destruction of the food sample, to prevent the components from being changed during the destruction process, and , The value of the product as a food product can be analyzed in a preserved state, and there is an advantage that the distribution or sale is possible immediately after analysis.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic overall perspective view of a substance extraction apparatus according to a first embodiment of the present invention; FIG.
FIG. 2 is a schematic overall exploded perspective view of a substance extraction apparatus according to a first embodiment of the present invention. FIG.
3 is a schematic cross-sectional view of a substance extraction apparatus according to a first embodiment of the present invention.
FIGS. 4 and 5 are side cross-sectional views, respectively, illustrating a process of opening and closing a through-hole of a valve in the object material extracting apparatus according to the first embodiment of the present invention.
FIG. 6 and FIG. 7 are views of a process of opening and closing a through hole of a valve in the object material extracting apparatus according to the first embodiment of the present invention, respectively.
FIG. 8 is a schematic overall perspective view of a substance extraction apparatus according to a second embodiment of the present invention. FIG.
9 is a schematic overall exploded perspective view of a substance extraction apparatus according to a second embodiment of the present invention.
10 is a schematic cross-sectional view of a substance extraction apparatus according to a second embodiment of the present invention.
Figure 11 shows a sample of the subject material extraction device of the present invention and Headspace (HS) -SPME extraction from a non-destructive apple using the device.
12 is a graph for confirming the optimal saturation time of a perfume component in extracting volatile fragrance components of apples using the subject material extracting apparatus of the present invention.
FIG. 13 shows the result of analyzing the volatile flavor components of apples extracted by using the substance extraction apparatus of the present invention. (a) targets fresh apples, and (b) targets apples stored for nine months.
FIG. 14 is a graph showing the results of analysis of changes in the alcohol group components among the volatile flavor components of apples during the storage period of apples by using the substance extraction apparatus of the present invention.
FIG. 15 shows the results of analyzing the changes in the ether group among the volatile flavor components of apples during the storage period of apples, using the subject material extracting apparatus of the present invention.
16 is a graph showing the results of analysis of changes in the components of the 2-methylbutyl group among the volatile flavor components of apples during the storage period of apples by using the substance extraction apparatus of the present invention. 2mBuAc: 2-methylbutyl acetate; 2mBuHe: 2-methylbutyl hexanoate; 2mBuOc: 2-methylbutyl octanoate
17 shows the results of analysis of changes in hexyl acetate and hexylhexanoate among the hexyl ester groups in the volatile flavor components of apples during the storage period of apples using the subject material extraction apparatus of the present invention.
Hereinafter, production examples and examples will be described in detail to facilitate understanding of the present invention. However, the production examples and examples according to the present invention can be modified into various other forms, and the scope of the present invention should not be construed as being limited to the following production examples and examples. The production examples and embodiments of the present invention are provided to enable those skilled in the art to more fully understand the present invention.
Example 1. Analysis of apple aroma
1-1. Apple sample preparation
Apple samples were purchased from Fujisan apple (Andong area), which was commercially available, and stored in a refrigerator at 1 ° C. The apple samples were used without any pretreatment to prevent the change of the fragrance components.
1-2. Apple fragrance ingredient extraction
In order to inject SPME (Solid Phase Micro Extraction) directly into a vacuum desiccator, the lid of a commercially available vacuum desiccator (Duran, Hattenbergstraße, Mainz, Germany) is made into a specially made Teflon miniert ® valve cap A substance extraction apparatus was prepared.
1) Apple fragrant ingredient extraction
The apples were saturated in a vacuum desiccator for 20 hours in order to determine the optimum saturation time of the fragrance components for non-destructive analysis of the fragrance components of apples using a vacuum desiccator. One apple was placed in a material extraction apparatus and sealed, and after saturation at 25 ° C for 20 hours, the fragrance component of apple was extracted with a solid phase microextraction (SPME) apparatus (FIG. 11). A 50/30 μm divinylbenzene / carboxen / polydimethylsiloxane (DVB / CAR / PDMS) fiber (Supelco Inc., Bellefonte, PA, USA) was injected into the vacuum desiccator and exposed to the top of the apple for 30 minutes Respectively. The flavor components of apple adsorbed on SPME fiber were analyzed by gas chromatography / mass spectrometry (GC / MSD).
2) Quantitative and Qualitative Analysis of Flavor Components
Quantitative and qualitative analysis of the volatile flavor components isolated from the apples was carried out by mass selective detector (MSD, 5975, Hewlett-Packard Co., Palo Alto, USA) with GC (gas chromatography) (6890, Hewlett Packard Co., Palo Alto, USA) , USA) was used. The column was HP-5MS (30m × 0.25mm, 0.25μm, J & W Scientific, CA, USA) and the injector temperature was 240 ℃ and the oven temperature was 40 ℃ Kept for 3 minutes, then heated up to 200 ° C at 4 ° C per minute and held for 5 minutes. The moving phase was 1.0 mL of helium per minute and split mode (10: 1) was used. MS mass spectrometry was performed at 35 400 m / z, MS ionization voltage was 70 eV, ion source temperature was 150 ℃ and transfer line temperature was 280 ℃. The flavor components of apple were analyzed by MS fragmentation and Willy 275 MS spectra library (Agilent Technologies, Santa Clara, CA, USA).
Analysis results of 1-3 fractions of apple
1) Establish time to extract the fragrant components of apple
In order to confirm the optimum saturation time of the fragrance components, the apples were saturated in a vacuum desiccator for 20 hours and analyzed. As a result, it was confirmed that the optimum saturation time was 6 hours as shown in FIG.
2) Analysis of fragrance components of apple
The fragrance components of apples after 3, 6, 9 months of storage were analyzed nondestructively. In the vacuum desiccator, the fragrance component of the apple saturated for 6 hours was extracted with HS-SPME and qualified with GC-MSD. For the analysis of the fragrance components, the fragrance components and the content (%) of apples harvested in each region were analyzed, and the fragrance components and contents thereof are shown in Table 1.
A total of 47 fragrance peaks were detected, and 38 fragrance components were quantified. More than 80% of the aroma components were consistent with the fragrance components of apples previously reported in other literature (A Review, New Zealand Journal of Crop and Horticultural Science, 2000, 28, 155-173; Review of apple flavor-state of The art, Critical reviews in Food Science and Nutrition, 1983, 18, 387-409, Causal effects of aroma compounds on Royal Gala apple flavors. Journal of the Science of Food and Agriculture, 1996, 71, 329-336). The main aroma components of the Fuji apple samples stored in the Andong area for 3 months were hexanol, butyl acetate, 2-methylbutyl acetate, butyl propanoate, butyl butanoate, hexyl acetate, hexyl hexanoate, butyl-2-methylbutanoate, pentyl- -2-methylbutanoate, 2-methylbutyl hexanoate, E, E-α-farnesene. The common flavor components of the apple samples stored for 6 months were 2-methyl-1-butanol, butyl acetate, 2-methylbutyl acetate, hexyl acetate, butyl-2-methylbutanoate, hexyl-2-methylbutanoate, -α-farnesene. The common aroma components of the apple samples stored for 9 months after harvest were 2-methyl-1-butanol, 2-methylbutyl acetate, hexyl-2-methylbutanoate, hexyl hexanoate, 2-methylbutyl hexanoate, -α-farnesene (Fig. 13).
34 fragrance components were detected in the 3 month old apple samples, and the fragrance peak numbers of the apple samples stored for 6 and 9 months were 17-19 and 11-12, respectively, compared with the apple samples stored for 3 months, And the fragrance component decreased as the storage period became longer. In addition, alcohol and ester groups were found to be major fragrance components in apple samples of various storage periods (3, 6, 9 months). However, the longer the storage period, the fewer alcohols such as butanol and hexanol were detected in the months, and the ester groups such as 2-methylbutylacetate, 2-methylbutyl hexanoate, 2-methylbutyloctanoate and hexyl hexanoate increased. It has been reported that the alcohol group is decreased and the ester group is increased during the fermentation period of fruit such as apple, strawberry, kiwi, melon and banana, and the alcohol acetyl transferases (AATs) Ester is produced. However, as shown in Fig. 14, 2-methyl butanol increased during the storage period.
Butyl ester group (butyl acetate, butyl butanoate, butyl-2-methylbutanoate) tended to decrease during the storage period (FIG. 15).
(2-methylbutyl acetate, 2-methylbutyl hexanoate, 2-methylbutyl octanoate) was found to increase during storage over the other ester groups. Among the components of the 2-methylbutyl group, 2-methylbutyl acetate (80% or more) (Fig. 16). 2-methylbutyl acetate has been reported to be the most important ester flavor component along with butyl acetate in various types of apples. The Hexyl ester group showed a decrease throughout the storage period in the Andong, Chungju, and Boeun regions. The content of hexyl acetate and hexyl octanoate in the group decreased during the storage period (Fig. 15).
During the storage period, hexyl acetate decreased and hexyl hexanoate increased (Fig. 17), which was similar to that reported for the other species, MacThoshi and Kortland apples (Odor-active volatiles in Mcintosh apples sotred in simulated low-etylene controlled atmosphere, Proc. Fourth National Res. Conf., 1985, 70-81).
The results of the present study indicate that the components of ethyl, butyl and hexyl esters decreased during the storage period of apple, and these fragrance components were considered to be short indices of fresh apple fragrance or short storage period. The contents of 2-methylbutyl ester increased, and 2-methylbutyl acetate and 2-methyl-butanol, the major components of the group, were thought to be the fragrant or off-flavor components of apples with long shelf life.
Claims (7)
(S2) saturating a food sample in a substance extraction apparatus; And
(S3) A method for non-destructively adsorbing and extracting a component of a food sample, comprising the step of transferring the adsorption / extraction device into a substance extraction device.
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KR20180124422A (en) | 2017-05-11 | 2018-11-21 | 한국식품연구원 | Methods for Extracting Aromatic Compounds of Aromatic plants |
KR20190056007A (en) | 2017-11-16 | 2019-05-24 | 고려대학교 산학협력단 | Sensor for coffee analysis and coffee analysis system containing the same |
CN112649539A (en) * | 2021-01-11 | 2021-04-13 | 湖南农业大学 | Detection method of in-vitro gas flower aroma substances |
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KR20180124422A (en) | 2017-05-11 | 2018-11-21 | 한국식품연구원 | Methods for Extracting Aromatic Compounds of Aromatic plants |
KR20190056007A (en) | 2017-11-16 | 2019-05-24 | 고려대학교 산학협력단 | Sensor for coffee analysis and coffee analysis system containing the same |
CN112649539A (en) * | 2021-01-11 | 2021-04-13 | 湖南农业大学 | Detection method of in-vitro gas flower aroma substances |
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