JP4618530B2 - Method and apparatus for continuous evaluation of volatile components - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method and apparatus for evaluating the influence of components separated by gas chromatography on aroma.
[0002]
[Prior art]
Conventionally, smell-smell gas chromatography (GC-O: GC-O) has been used as a method for retrieving trace aromatic components from animal and plant raw materials. That is, by searching for a trace component that is not detected by GC-MS by smelling the component separated and discharged at the column outlet of the gas chromatograph, this method is generally performed.
[0003]
In addition, as a screening method for characteristic aroma components using GC-O, an AEDA method, a Charm Analysis method, and the like are also performed. Such a perfume analysis technique is introduced, for example, in “Utilization of Gas Chromatography and Mass Spectrometer in Perfume Analysis” (Nishimura Fragrance Journal, 1997-6, 12, 1997).
[0004]
[Problems to be solved by the invention]
Among the screening methods for characteristic aroma components using the above-mentioned GC-O, the AEDA method is a method for examining the odor characteristics of each component by diluting the aromatic liquid of animal and plant raw materials and examining the threshold value of each component. Can do. However, since such GC-O only expresses each characteristic of the odor component in the gas phase through the nose, evaluation of the fragrance component in which the fragrance components such as masking and enhancement interact with each other. There are limits. Therefore, when evaluating the interaction between such fragrance components, a method is employed in which the concentration of the fragrance components is changed one by one and mixed with the original animal and plant raw materials, and then the change in the fragrance is evaluated.
[0005]
Although this method is useful for observing the interaction between fragrance components, the added fragrance component is limited to the identified components, and it is very labor intensive to see the change in fragrance one by one. The problem is that it takes time and experience.
[0006]
The inventors of the present invention have conducted intensive research for the purpose of overcoming the drawbacks and limitations of the conventional GC-O analysis method and aroma component evaluation method as described above, and faithfully reproducing the aroma of animal and plant raw materials and developing functionality. As a result of superimposing, the present invention was completed by developing a new method for collecting aromas that has not been described in the previous literature, where volatile components separated by gas chromatography and gas samples of animal and plant raw materials (samples) are continuously mixed and evaluated. did.
[0007]
The object of the present invention is to enable the faithful reproduction of the aroma of animal and plant raw materials and the development of functionality by a method for evaluating the influence of components separated by gas chromatography on aroma, preferably a novel aroma collection method. Another object of the present invention is to provide a method for evaluating volatile components.
[0008]
Another object of the present invention is to provide an apparatus used for the above-described method for evaluating volatile components.
[0009]
[Means for Solving the Problems]
This onset Ming, the volatile components separated by gas chromatography, a method of evaluating the volatile components, characterized by mixing the gas sample continuously, the mixing is provided outside of the path of the gas chromatograph the sample container, by introducing a carry yer gas discharged gas phase portion of the sample container as a discharge gas, it can be achieved by for combining the effluent gas from the gas chromatograph. In addition, malodorous substances and animal and plant materials are used as samples in the present invention.
[0010]
In the volatile component evaluation method of the present invention, a column for separating volatile components, a sample container provided with a carrier gas introduction path and an exhaust flow path, a flow path for exhaust gas from the sample container, and a column A gas chromatograph (apparatus) having a flow path that joins the flow path of the outflow gas from the gas can be used.
[0011]
In the gas chromatograph, means for separating volatile components can be provided on the flow path of the outflow gas from the column or the flow path after the merge with the flow path of the exhaust gas from the sample container.
[0012]
DETAILED DESCRIPTION OF THE INVENTION
The continuous evaluation method for volatile components of the present invention comprises a means for separating essential oils, blended fragrances, etc. composed of multiple components into respective components, and continuously separating the separated volatile components and the exhaust gas from the sample for evaluation test. It consists of a means for mixing. In the present invention, the mixed gas of the separated volatile component and the exhaust gas from the sample container is sensorially evaluated. At the same time, each component can be easily associated with the evaluation by a chromatograph.
[0013]
In the present invention, a gas chromatograph is used as a method for separating a volatile component composed of multiple components. As the gas chromatograph, those conventionally used for analyzing volatile components can be used.
[0014]
Next, FIG. 1 shows an example of an apparatus (chromatograph) used in the continuous evaluation method of the present invention, but the apparatus of the present invention is not limited by this drawing. In FIG. 1, a gas chromatograph 1 includes a column 2 for separating volatile components, a sample container 5 provided with an introduction path 4 for a carrier gas 3 and an exhaust flow path (not shown) for the carrier gas 3, and the sample container. 5 is a gas chromatograph having a flow path 9 where a flow path 6 of exhaust gas from 5 and a flow path 8 of outflow gas 7 from the column 2 merge.
[0015]
A multicomponent essential oil or the like is injected from the injection port 10, and the volatile component separated by the column 2 is woven into the flow path 8 as the outflow gas 7 through the detector 11. On the other hand, the gas sample emitted from the animal and plant material sample introduced into the sample container 5 is mixed and mixed with the effluent gas 7 by the carrier gas 3 via the exhaust gas flow path 6 and the merged flow path 9. .
[0016]
In the present invention, a sample for evaluation testing was introduced in the sample container, components volatilized in the sample container (gaseous sample) is continuously discharged as a discharge gas in the carry Ya Gasu introduced into the sample container.
[0017]
The sample for the evaluation test may be in any form such as solid or liquid. When the sample is a liquid, it is preferable to stir in the sample container, and a known method can be used as the method. When the sample is a gas, the sample can be continuously introduced into the sample container with a pump or the like.
[0018]
In the present invention, the sample container can be heated or cooled as required depending on the sample or the purpose of evaluation. As a method for adjusting the temperature in the sample container, a known method such as a method in which a heater is installed outside the container or a method in which a jacket is attached to the container and a temperature adjusting fluid is passed can be used. Further, a temperature measuring instrument can be installed inside or on the outer surface of the sample container, and means for adjusting the temperature by the output of the measuring instrument can be applied. The material of the sample container is preferably one that does not release volatile components such as odor itself, and a glass container or the like is usually used. Discharge port for discharging the volatile components from the sample container is placed on top of the container, inlet carry Ya Gasu is preferably installed below from the discharge port.
[0019]
The carrier Ya Gasu, although inert gases such as typically nitrogen is used, may be used a gas containing oxygen in accordance with the application.
[0020]
The exhaust gas from the sample container merges with the volatile components separated by the column of the gas chromatograph, but a gas retention container can be installed on the flow path until the gas is merged. In addition, heat retention or warming means can be provided by a known method in the flow path up to the merge and the gas retention container.
[0021]
In the present invention, the volatile component separated by the gas chromatograph is divided into a combined flow path of the flow path to the detector and the gas from the sample container, or is guided to the combined flow path after passing through the detector. When the detector of the gas chromatograph may cause a change in volatile components due to heating or the like, it is preferable to divide the flow path to the detector after column separation.
[0022]
In the present invention, a means for adjusting the lag time generated between the output of the chromatogram and the sensory evaluation is provided particularly when the flow path to the detector is divided. Examples of the lag time adjusting means in the present invention include a method by adjusting the distribution amount of each flow path and a method of performing a delay process on the output of the chromatogram.
[0023]
In the present invention, a means for collecting a volatile component separated by a gas chromatograph, or a volatile component contained in a mixed gas of the separated component and an exhaust gas from the sample container can be provided. A switching means for the flow path is installed on the flow path of the separated component by gas chromatograph or the flow path after merging with the exhaust gas from the sample container, and this switching means guides each arbitrary component to the collection container. Can do. The collection of separated components or mixed gases can be collected for each component, or any component can be collected and combined sequentially, and moreover, multiple collection containers can be installed in parallel. It is also possible to switch the flow path. As the channel switching means, a channel switching cock may be provided and switched manually, or a method of mechanically operating the switching valve with reference to the chromatogram output may be used.
[0024]
As a specific collection method, known methods such as resin adsorption, condensation by cooling, and absorption in a solvent can be used, but generally the amount of components to be collected is often a very small amount. preferable. Further, for example, a volatile component collected by an adsorbent can be desorbed with an organic solvent or the like, and a component analysis can be performed after the solvent is recovered.
[0025]
Examples of the adsorbent used for collecting the components in the present invention include activated carbon, silica gel, and resin.
[0026]
【Example】
Examples of the present invention are shown below.
[0027]
Example 1
The coffee aroma concentrate 0.2mg obtained by steam distillation and simultaneously introduced into the gas chromatograph, put hot water extract 60g of coffee sample container provided outside of the path of the gas chromatograph, each with air as carrier Ya gas partial 160ml The fragrance in the head space portion in the container was discharged at a flow rate of 1, and was combined with the effluent gas from the gas chromatograph, and the mixed gas was evaluated.
[0028]
The gas chromatograph used in the experiment was a non-polar column, and the carrier gas of the gas chromatograph was helium gas at a flow rate of 4.4 ml / min. The temperature was raised from 40 ° C. to 230 ° C. at a rate of 3 ° C./min. .
As a result of sensory evaluation under the above conditions, it was confirmed that the roasting odor was emphasized in the portions corresponding to the four peaks in the chromatogram. Confirmation Regarding the volatile compounds corresponding to the four peaks, the aroma was confirmed independently, and all of the aromas were completely different from the roasted odor.
[0029]
(Example 2)
Gas chromatography was performed under the same conditions as in Example 1, and portions corresponding to the four peaks confirmed in Example 1 were collected with a porous adsorption resin. The collected components were analyzed with a gas chromatograph, and a fragrance was prepared based on the data (prepared fragrance 1).
[0030]
Next, the head space of the hot water extract of coffee was collected, analyzed in the same manner as described above, and a fragrance was prepared based on the data (formulated fragrance 2).
[0031]
The sensory evaluation of the above-mentioned blended fragrances 1 and 2 was performed by 10 panelists extracted at random, and 9 persons evaluated that the blended fragrance 1 had a clearly stronger roasted fragrance and a fragrant and favorable fragrance.
[0032]
【The invention's effect】
Since the present invention can easily and functionally evaluate the mixed gas of the separated volatile component and the volatile component for evaluation, it is very difficult to evaluate the fragrance component in which the fragrance components such as masking and enhancement interact with each other. It is a powerful method.
[0033]
Specifically, according to the present invention, when a sample is a malodorous material such as an animal or plant material, the presence or absence of a deodorizing effect can be determined by evaluating the odor or the like of the volatile component. Moreover, according to this invention, a volatile component isolate | separated by the gas chromatograph can be continuously mixed with the gas sample from animals and plants raw materials etc., and aroma etc. can be evaluated. Moreover, a fragrance | flavor composition can be obtained by analyzing the volatile component finally fractionated and reconstituting a required component.
[Brief description of the drawings]
FIG. 1 is a conceptual diagram for illustrating and explaining an apparatus (chromatograph) used in a continuous evaluation method of the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Gas chromatograph 2 ... Column 3 ... Carrier gas 4 ... Introduction path 5 ... Sample container 6 ... Exhaust gas flow path 7 ... Exhaust gas 8 ... Flow path 9 ... Flowing path 10 ... Inlet 11 ... Detector

Claims (5)

A sample vessel provided outside of the path of the gas chromatograph, the volatile components by introducing a carry yer gas phase portion of the sample container is discharged as an exhaust gas is characterized in that it is merged with the effluent gas from the gas chromatograph Evaluation method. Sample introduced into the sample container, the evaluation method of the volatile components according to claim 1 Symbol mounting characterized in that it is a plant and animal material. Evaluation of volatile components according to claim 1 Symbol placement, wherein the sample to be introduced into the sample container is malodorous substances.   A column in which a volatile component is separated, a sample container provided with a carrier gas introduction channel and an exhaust channel, a flow of exhaust gas from the sample container, and a flow of gas flowing out from the column merge. A gas chromatograph having a channel. 5. The gas chromatograph according to claim 4, wherein means for separating volatile components is provided on the flow path of the outflow gas from the column or the flow path after the flow of the exhaust gas from the sample container. Graph.

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