JP2000053992A - New collection of fragrance and apparatus therefor, and fragrant liquid or fragrant composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To collect the fragrance of live flowers, fruits on the tree, cut flowers, fruits, or the like, by contacting humidified air or the like with animal/plant raw materials to include the fragrance of the raw materials followed by fractional extraction of the fragrance component. SOLUTION: The objective fragrance is collected by contacting humidified air or inert gas with animal/plant raw materials such as flowers being planted, fruits on the tree, vegetables being planted, herbs, cut flowers, fruits, vegetables, roasted coffee beans, teas or spice to include the fragrance of the raw materials in the above air or inert gas, followed by fractional extraction of the fragrance component.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to the fragrance of animal and plant raw materials such as planted flowers (hereinafter abbreviated as fresh flowers), fruits that become trees (hereinafter abbreviated as fresh fruits), cut flowers or freshly picked fruits. Fragrance collection method and device capable of collecting fragrance as it is, a fragrance liquid obtained by using the fragrance collection method and device, and component analysis of the fragrance liquid for reconstitution Perfume compositions.

[0002]

2. Description of the Related Art Conventionally, a steam distillation method, a solvent extraction method and the like have been industrially used as means for separating an aromatic component from animal and plant raw materials. In the field of fragrance analysis research, headspace gas analysis is often used as a means of trace analysis. After the fragrance of fresh flowers is directly collected by an adsorbent, the odor components are analyzed by gas chromatography or mass spectrometry. Component analysis is performed using the apparatus. Such a fragrance analysis technique is described in, for example, "Utilization of gas chromatography and mass spectrometer in fragrance analysis" (Nishimura
Fragrance Journal, 1997-6, 12, 19
97).

[0003]

Among the headspace gas analysis methods described above, a method referred to as a static headspace method is, for example, to collect gas (headspace gas) in the upper space of a closed container and extract it. Is directly analyzed by gas chromatography, and since the fragrance component before being injected into the analytical instrument is not modified at all, it can be said to be the original fragrance component. However, when sampling the atmosphere of a fresh flower that emits only a weak aroma and analyzing it by gas chromatography, the amount of air injected is limited, and it is difficult to detect trace components even if the detection sensitivity is increased. . Therefore, in such a case, the air is sent so as to continuously contact the fresh flowers, and the air containing the fragrance is brought into contact with an adsorbent such as silica gel or a porous polymer resin to adsorb and concentrate the fragrance component. A method (a method called a dynamic headspace method) is employed.

[0004] However, although the adsorbent is extremely useful for collecting fragrance components, its adsorption capacity is very selective, and the odor released from the adsorbent does not necessarily reproduce the original composition of the fragrance component. Not a thing.

[0005]

SUMMARY OF THE INVENTION The present inventors have overcome the drawbacks and limitations of the conventional headspace gas analysis method as described above, and faithfully reproduce the aroma of fresh flowers and fresh fruits, as well as aromatic liquids and flavors. As a result of intensive studies to develop commercial products as liquids, etc., we developed a new method for collecting fragrance, which is not described in the conventional literature, that uses humidified air or inert gas to collect fragrance components. Completed the invention.

The novel aroma collection method developed by the present inventors is based on a method named “Aquaspace” method by the present applicant, and is based on humidified air or inert gas (hereinafter abbreviated as humidified air). ) Is forcibly brought into contact with animal and plant raw materials such as fresh flowers and cut flowers to allow the humidified air to contain the fragrance component, and then the humidified air is cooled to collect the fragrance component together with the condensed water. It is a collection method. Unlike the conventional so-called headspace method, since the aromatic component is contained in the condensed water, for example, as it is, it can be commercialized as an aromatic liquid of flowers or extracted with an organic solvent as an aromatic liquid or a flavor liquid. is there.

The reason why the humidified air often includes the fragrance of fresh flowers and fresh fruits is that the humidified air stimulates the fresh flowers to make the flowers easily emit fragrance, or
It is guessed, but not certain, that water vapor repeatedly adheres and volatilizes at the site of fragrance emission of flowers, and as a result, it acts as a water vapor distillation at room temperature. Although such an inference can be made, the novel method and apparatus for collecting aroma components of the present invention are the result of many years of research efforts by the present inventors.

In the case of performing odor analysis using the present invention,
The fragrance component can be further concentrated by extracting the aromatic water as it is or by extracting it with an organic solvent, and then analyzed by combining gas chromatography and a mass spectrometer (abbreviated as GC-MS). The fragrance of fresh flowers obtained by this new method of collecting fragrance using humidified air is a fragrance that reproduces the literal `` freshness '' like the smell of flowers drifting in the morning fog. It is something that can never be obtained by the collection method. Based on the results of the fragrance analysis of the fragrance, it has become possible to obtain a fragrance composition reproducing the composition.

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail.

FIG. 1 shows an example of the method and apparatus for collecting fragrance of the present invention. The air blown by the blower 1 is humidified by the humidified air generator 2 and comes into contact with the fresh flowers 4 in the animal and plant raw material storage section (hereinafter referred to as aqua space) 3. 8, the ice cooling trap 5, the dry ice / ethanol trap 6,
While passing through the liquid nitrogen trap 7, the water is condensed and the aroma component is collected together with the moisture.

Although the above-mentioned components are essential components of the apparatus of the present invention, the aqua space may be a partially open container type as shown in FIG. 1 or a closed type container as shown in FIG. . For example, in the case of fresh flowers, a partially open container must be used, and in the case of cut flowers, a closed container is more advantageous. As a simple example, a glass apparatus as shown in FIG. 1 can be used. If it is necessary to increase the capacity, for example, a PEP, acrylic resin, or Teflon resin as shown in FIG. I just need.

Further, the cooling trap is not limited to ice-dry ice-acetone-liquid nitrogen, and is not particularly limited as long as it can effectively condense humidified air. After the cooling trap, an adsorption resin such as a porous polymer resin, for example, a resin adsorption cylinder made of 2,6-dimethyl-p-phenylene oxide polymer, an acrylic ester polymer or a styrene divinylbenzene polymer, or an adsorption cylinder made of activated carbon or the like is connected. This can be advantageous because it can capture the scent that escapes without being collected by the cooling trap.

The material of each part of the apparatus of the present invention is not particularly limited as long as it does not have a bad odor or does not generate a bad odor due to humidified air.
Examples thereof include plastics such as glass, stainless steel, PEP, and acrylic resin.

The blower used in the above apparatus depends on the purpose of collection and the size of the apparatus. For example, for the purpose of analyzing fresh flowers, about 5000 ml / min. Of air at 20 to 40 ° C, more preferably 20 to 40 ° C by a humidified air generator.
Humidified air at a temperature of の 30 ° C. and a humidity of 80% or more, more preferably 90% or more, is prepared and brought into contact with fresh flowers in the aqua space. On the other hand, about 450
0 ml / min. The humidified air containing the aroma is condensed by being pulled by the cold trap, and is condensed with the aroma and collected at the bottom of the vessel. The reason why the amount of air blow is set to be larger than the amount of exhaust air is to keep the inside of the apparatus in a pressurized state and to reduce the amount of foreign matter and unpleasant odor. Collect these condensed waters to make aromatic water, as it is, or
Extraction and concentration with a solvent such as ether to form an aromatic liquid, GC
-Can be measured by MS analysis. This aromatic liquid faithfully reproduces the fresh fragrance of fresh flowers, and is analyzed by GC-MS.
The reconstitution of the analysis results can also be evaluated as a fragrance composition that is close to that.

Further, industrially, for example, an apparatus as shown in FIG. 2 can be scaled up and used. The aqua space is a closed type, and the inside is multi-stage as shown in FIG. 3, and fresh cut flowers are placed on each stage so that a larger amount of aromatic water can be obtained.

As described above, the humidified air has a temperature of 2
Air or an inert gas having a temperature of 0 to 40 ° C and a humidity of 80% or more, more preferably a temperature of 20 to 30 ° C and a humidity of 90% or more. Helium, nitrogen and argon can be used as the inert gas, but nitrogen is the most economical and useful. In addition, whether to use air or inert gas depends on
It is necessary to select a suitable one according to the animal or plant raw material from which the aroma is to be collected. For example, in the case of a fresh flower, a fresh fruit, or a cut flower, it is preferable to use air because there is a risk of withering due to suffocation.

As described above, when the apparatus as shown in FIG. 2 is used, air having a temperature of 20 to 30 ° C. and a humidity of 90% or more is a suitable condition for maintaining the freshness of cut flowers. It can withstand fragrance collection and never wither. In addition, the ventilation can be interrupted, the cut flowers can be exchanged for fresh ones, and the collection can be resumed. The fragrance can be collected continuously for many days. Methods and apparatus.

A feature of the present invention relates to a method and an apparatus for collecting the fragrance of a fresh flower or a fresh fruit without changing the fragrance by heating or the like, and retaining the fragrance as it is.
This is completely different from the conventional method of collecting aroma by steam distillation. That is, the humidified air generator used in the present invention is required to be able to supply humidified air at 20 to 40 ° C. in the aqua space. At a temperature higher than 40 ° C., there is a concern that fresh flowers will die, At temperatures, it may be difficult to provide humidified air having a humidity of 80% or more. As a simple method for generating such humidified air, for example, air or inert gas that has been completely deodorized by passing through an activated carbon packed tower in odorless and clean water at a temperature of about 20 to 40 ° C. Obtained by blowing. There are trace amounts of various volatile components in the air, and when trying to collect the faint aroma of fresh flowers as in the present invention, these volatile components are a major obstacle, so that air or inert gas to be blown is Cleaning is absolutely necessary.

The fresh flowers or fresh fruits used in the present invention are, as described above, living flowers and fruits that are pumping nutrients from the roots, such as potted lilies and gardenia, or apples and peaches in fields, and Anything that fits in the space can be applied. In addition, not only fresh flowers and fresh fruits, but also fresh cut flowers, freshly harvested fruits, vegetables, or animals and plants that are processed foods of herbs, roasted coffee beans, tea such as tea, spices, seafood, and meat meat. Even for raw materials, there is no inconvenience in using the collection method and apparatus of the present invention.

[0020]

Next, embodiments of the present invention will be described in more detail with reference to Examples and Comparative Examples.

Example 1 A fragrance component of a fresh gardenia was collected by the aquaspace method using the fragrance component collection device of the present invention illustrated in FIG. 1, and the fragrance component composition was identified by GC-MS analysis. .
The gardenia was potted, and an aqua space made of acrylic resin was created so that flowers could enter. Clean and odorless humidified air 5000 ml / min. Was contacted with the gardenia in the aqua space for 7 hours continuously, and the humidified air containing the aroma was supplied to an ice trap-dry ice ethanol cold trap at 4500 ml / min. Was passed while exhausting the amount of air. The condensed water collected in the cold trap was collected to obtain 40 g of fresh gardenia aromatic water. Furthermore, ether was added to 40 g of the aromatic water to extract a fragrance component, and 93 mg was obtained as a concentrate. The fragrance component was identified by GC-MS analysis of the fragrance component concentrate.

Comparative Example 1 Using the same gardenia flower used in Example 1, the fragrance component of the gardenia was analyzed by a conventional headspace gas method. The method of collecting the aroma components was to remove the humidified air generator of the aquaspace method apparatus of Example 1 and to mount a column of porous resin 2,6-dimethyl-p-phenylene oxide polymer instead of the cooling trap. And air was blown for 7 hours, and the fragrance component was adsorbed by the resin and collected. Aroma components were desorbed from the resin using ether, concentrated and subjected to GC-MS analysis in the same manner as in Example 1 to identify the components.
The results are also shown in Table 1.

Comparative Example 2 The same gardenia flower used in Example 1 and Comparative Example 1 was picked and immersed in ether for 7 hours, and then the ether was distilled off to concentrate fragrance components. The components were identified by performing GC-MS analysis in the same manner as in Example 1. The results are also shown in Table 1.

[0024]

[Table 1]

Analysis results and odor sensory comparison Example 1 (Aquaspace method of the present invention) shown in Table 1,
As can be seen from the gardenia aroma components and their contents obtained in Comparative Example 1 (headspace gas method) and Comparative Example 2 (solvent extraction method), the composition is a three-part result. This is because, in the case of the headspace gas method of Comparative Example 1, since the odor components have to be collected by the adsorption resin, for example, hydrocarbons are selectively adsorbed at a high concentration, or Comparative Example 2 However, when the flowers are immersed in ether to concentrate the fragrance components eluted, a large amount of high-boiling fragrance components that are relatively difficult to volatilize will also be extracted, and the fragrance of the original flowers will be displayed on the chart. The result is not reproduced. In this regard, the present invention provides the aromatic water as it is, or
It is only the aromatic water extracted with ether and concentrated,
It can be said that it reproduces the original scent well,
This is a feature of the present invention.

Further, Example 1 (the aquaspace method of the present invention), Comparative Example 1 (the headspace gas method) and Comparative Example 2
The fragrance sensory evaluation was carried out by five well-trained panelists on the fragrance component concentrates obtained by (solvent extraction method) and the reconstituted fragrance composition based on the analysis results. As a result, all the five aromas and the reconstituted aroma composition obtained in Example 1 in which the aroma was collected using the aquaspace method of the present invention reproduced the aroma of the gardenia flower very well. Evaluation was made, and it was determined that there was a marked difference from Comparative Example 1 (headspace gas method) and Comparative Example 2 (solvent extraction method).

Example 2 The fragrance of a cut flower of Japanese narcissus was collected using the fragrance collecting device shown in FIG. Using 202 cut flowers, air volume 5
000 ml / min. The humidified air is blown into the aqua space for about 8 hours a day for a total of 18 days (144 hours in total) to come into contact with the flowers, and the humidified air containing the aroma is sucked and discharged at a flow rate of 4500 ml / min. And the mixture was led to a cooling trap to collect fragrance components as condensed water. About 900 g of aromatic water could be obtained, and this was processed to obtain an aromatic composition for cosmetics.

[0028]

According to the present invention, it is possible to collect the aroma of planted flowers (fresh flowers), fruits that become trees, cut flowers, fruits, and other animal and plant raw materials, especially fresh flowers. Thus, it has become possible to provide a method and a device for collecting a fragrance component which are useful for fragrance component analysis research or industrially as a fragrance composition for cosmetics.

[Brief description of the drawings]

FIG. 1 is an explanatory diagram of an aroma collection device of the present invention.

FIG. 2 is an explanatory diagram of a fragrance collecting device of the present invention in which an aqua space is closed.

FIG. 3 is an explanatory view of the inside of an example of a closed aqua space.

[Explanation of symbols]

 REFERENCE SIGNS LIST 1 blower 2 humidified air generator 3 aqua space 4 fresh flower 5 ice cooling trap 6 dry ice / ethanol trap 7 liquid nitrogen trap 8 exhaust fan 9 activated carbon filling tower 10 internal flower stand

Claims (8)

[Claims] The present invention is characterized in that humidified air or inert gas is brought into contact with animal and plant raw materials, and the humidified air or inert gas contains the odor of the animal and plant raw materials, and then the odor component is fractionated. A method for collecting aromas of animal and plant raw materials. 2. The method for collecting aroma according to claim 1, wherein the plant and animal raw materials are planted flowers, tree-forming fruits, planted vegetables and herbs. 3. The method according to claim 1, wherein the animal and plant raw materials are cut flowers, fruits, vegetables, herbs, roasted coffee beans, teas, spices and other processed foods. 4. The odor collection device according to claim 1, comprising a humidified air or inert gas generation unit, a storage unit for storing animal and plant raw materials, and a collection unit for aroma components. . 5. The method according to claim 1, wherein the humidified air or inert gas is 20 to 20.
The odor collection device according to claim 4, which is air or an inert gas having a temperature of 40 ° C and a humidity of 80% or more. 6. The fragrance component collecting section is selected from ice, dry ice-acetone (or ethanol) and liquid nitrogen.
5. A cooling trap comprising a combination of species or more.
6. The odor collection device according to claim 5. 7. An aromatic liquid obtained by the collecting method and apparatus according to claim 1. 8. A fragrance composition whose composition has been reconstituted based on the results of component analysis of the fragrance liquid according to claim 7.