JP4623586B2 - New preparation method in fragrance preparation - Google Patents

Description

  The present invention relates to a method for blending fragrances.

In general, when a fragrance is prepared, a substance having a target fragrance is subjected to instrumental analysis using a gas chromatograph or the like, and is prepared based on the obtained data. However, when a preparation prepared based on the data obtained by this gas chromatography is added to a base material such as a beverage containing fruit juice and tasted, there are many cases where the object is first felt different from the scent smelled by the nose. . This is due to the fact that the environment in which the fragrance is expressed in the oral cavity is not taken into consideration when collecting the fragrance of the target substance in the first stage. In recent years, therefore, studies have been conducted to investigate the expression of aroma in the oral cavity assuming the oral cavity.
Robert, D.D. D. , Acree, E .; T.A. , J. et al. Agric. Food Chem. , 43, 2179-2186, (1995)

  Although it was known that there was a difference between the scent of smelling the fragrance composition with the nose as described above and the fragrance felt when the fragrance composition was added to the base and tasting, this difference was corrected. As a method of doing this, the fragrance composition was actually added to the base material, sensory evaluation was performed, and fine adjustment was repeated. An object of the present invention is to provide a method for easily correcting the composition of a fragrance based on data obtained by instrumental analysis in order to prepare a fragrance that reproduces the scent smelled by the nose in the oral environment. There is.

  The present invention introduces a fragrance composition into an intraoral model environment mixed with artificial saliva and a non-oral environment without using artificial saliva, and collects and analyzes the components of the volatile components to be vaporized. This is a fragrance blending method for calculating a correction value and correcting the composition ratio of the fragrance composition.

  If the method of this invention is utilized, the fragrance felt in an oral cavity can be easily matched with the fragrance which sniffed the fragrance | flavor composition before correction | amendment with the nose. Thereby, compared with the conventional method of repeating sensory evaluation and fine adjustment of a fragrance | flavor composition ratio, working efficiency can be improved markedly.

  The present invention is a method for optimizing the aroma image in the oral cavity by correcting the aroma balance that changes depending on the environment in the oral cavity. The correction method of the present invention collects aroma components that volatilize in the artificial saliva and the intraoral model environment that contains it, and the non-oral environment that does not use artificial saliva, and compares the results of component analysis to obtain a correction value. Is a method for correcting the composition ratio of the fragrance composition.

The intraoral model environment solution of the present invention is a solution for measuring the influence of saliva on the fragrance in the oral cavity and containing artificial saliva that reproduces saliva in the base. As the artificial saliva used in the present invention, an aqueous solution containing amylase, inorganic salt and mucin is used. The amylase used in the artificial saliva of the present invention is α-amylase, the salt is NaHCO ₃ , K ₂ HPO ₄ , NaCl, KCl, CaCl ₂ .2H ₂ O, and the mucin is derived from the porcine stomach. be able to. More specifically, for example, 1000 ml of distilled water, 5.208 g of NaHCO ₃ , 1.369 g of K ₂ HPO ₄ , 0.877 g of NaCl, 0.477 g of KCl, 0 of CaCl ₂ · 2H ₂ O As an example, 441 g, 2.160 g of porcine stomach mucin, and 125,000 units of α-amylase were added and dissolved.

  Moreover, the non-oral environment solution of the present invention refers to a solution consisting only of a base that does not contain artificial saliva.

  The base as used in the present invention refers to a medium into which a fragrance composition is introduced or a fragrance component is allowed to pass. Specifically, water or a solution mainly composed of water, which has been adjusted to a viscosity by adding water to fruit juice, beverage, puree, a solution containing an extract such as coffee, tea or tea, or a solution containing carbonic acid , Ice cream consisting of sugar, starch syrup, dairy products and stabilizers, jelly pudding using gelling agents, pudding baked and hardened using eggs, yogurt, fruit preparation used for adding yogurt, A perfumed object can be used according to the use of milk, a beverage containing milk, and other perfumes. These bases should be adjusted to such a degree that they can be easily stirred by adding water when using foods and beverages with high viscosity, or to the extent that bubbles can easily move when passing through a gaseous aroma component. Is preferred.

  In the present invention, the fragrance composition to be corrected is introduced into the intraoral model environment solution to collect the diffused fragrance component, or the component diffused from the fragrance composition to be corrected together with the carrier gas. The method of collecting the aroma components in the gas discharged by passing through the oral model environment solution is used.

  When the fragrance composition is introduced into the solution, the fragrance composition to be corrected is introduced into the artificial saliva in a closed container having a carrier gas inlet and an exhaust path, and the condition is 35 to 37 ° C, preferably 37 ° C. The aroma component that is stirred and diffused is introduced into the component collecting means outside the system together with the carrier gas and collected.

  In the case where the fragrance volatile component is passed through the solution, the oral environment solution or the non-oral environment solution is introduced into a sealed container having a carrier gas introduction port and an exhaust port, and the condition is 35 to 37 ° C, preferably 37 ° C Stir under. Next, the fragrance composition is put into a sealed container having a carrier gas introduction port and an exhaust port, and the carrier gas is introduced. A carrier gas containing a volatile component discharged from the discharge port is introduced into the oral environment solution or the non-oral environment solution and bubbled while stirring. A carrier gas containing a volatile component that has passed through the oral environment solution or the non-oral environment solution is introduced into a component collecting means outside the system to collect the volatile component.

  In the present invention, the fragrance component collected by volatilization from the intra-oral model environment solution and the fragrance component collected by injecting the fragrance composition into the non-oral environment solution and collecting the fragrance component are compared. The method to be used is used. Alternatively, the fragrance composition is diffused, and the fragrance component collected by passing the intraoral model environment base solution together with the carrier gas and the fragrance component collected by passing the non-oral environment solution are used as a device. An analysis and comparison method is used.

  In the present invention, a known volatile component collection method can be applied to the collection method of the fragrance component. Usually, for example, a solid phase micro extraction (hereinafter referred to as SPME) method or Tenax resin adsorption is used. A method suitable for collecting trace components such as collection is selected.

  For the aroma component analysis in the present invention, a gas chromatograph or a gas chromatograph mass spectrometer can be used. For example, aroma is collected by the SPME method, a component-adsorbed collection medium is introduced from an injection port such as a gas chromatograph, thermal desorption is performed, and analysis is performed, and the obtained area area is used as an analysis value.

  First, the value of the non-oral environment solution not containing saliva is selected for the analysis value of each fragrance component obtained by gas chromatographic analysis. Next, the value of the oral model environmental solution is selected and divided by the previously selected value. The reciprocal of the value at that time is used as a correction value. A value obtained by multiplying the correction value by the amount of each fragrance component is taken as the amount of the fragrance composition with coefficient correction.

  The fragrance composition with the blending ratio corrected according to the present invention is used for all oral products such as food and drink, toothpaste and mouthwash. In particular, it is preferably used for foods and drinks in an ingested form in which the aroma after opening is difficult to diffuse into the atmosphere, such as beverages that are drunk using straws such as brick packs and chilled cups, and foods and drinks in tube-type containers such as jelly beverages.

  Moreover, the correction | amendment part of the fragrance | flavor composition of this invention, ie, the composition which corresponds to the difference of each fragrance | flavor component of the fragrance composition before correction | amendment, and the fragrance | flavor composition after correction | amendment can also be made into a different form separately. In the correction part of the fragrance composition, for example, a precursor of a fragrance component such as a glycoside can be replaced in terms of molar ratio, and the fragrance composition in the correction part is covered by a known method such as microcapsule before correction. It can also be added to the perfume composition. Thus, the method which makes a correction | amendment part a different form diverges in an intraoral environment at the time of eating and drinking, Therefore It is used especially preferably for the food which requires chewing in the oral cavity, such as chewing gum.

(Calculation of correction value)
The experimental conditions of the experimental apparatus used were: SPELCO: RED, Polydimethylsiloxane, film thickness of 100 μm for the SPME collection medium, 500 ml of the Muenke-type washing bottle for the collection container, N _{2 for} the carrier gas, and the gas flow rate of 20 ml / min The gas ventilation time is 5 minutes, the SPME collection location is the Muenke-type washing bottle outlet, the volume of the object is 100 ml, the amount of flavor added to the object is 0.02%, the temperature in the water bath is 37 ° C. The stirrer for stirring the inside of the collection container was tested at a rotation speed of 120 rpm.

The ingredients used in the experiment and the flavors with known concentrations (standard flavors) were used in the following formulation.

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Isoamyl acetate 50mg
Ethyl acetate 10mg
Butyl butyrate 10mg
Isoamyl butyrate 10mg
Isoamyl isovalate 5mg
Octanol 3mg
trans-2-Hexeral 3mg
2-Methylbutyric acid 3mg
Hexanoic acid 3mg
Butyric acid 3mg
Ethanol 900mg
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Artificial saliva was prepared by blending the following components and adjusting to 1000 ml with distilled water.

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NaHCO ₃ 5.208 g
K ₂ HPO ₄ 1.369 g
NaCl 0.877g
KCl 0.477g
CaCl ₂ · 2H ₂ O 0.441 g
Porcine stomach mucin 2.160g
α-Amylase 125,000 units
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  The materials used for the base material are purified water, 100% banana juice (prepared to make 100% fruit juice with concentrated water), 50% banana puree (100% puree prepared with purified water to 50%) 3 types are available. An artificial intraoral model environment solution was prepared by adding 1/5 amount of each of three types of artificial saliva.

  Gas chromatograph mass spectrometry was performed on the aroma collected based on the experimental conditions. The analysis conditions are HP 6890/5973 MSD for the analytical apparatus, TC-WAX for the column used, 30 m × 0.25 mm × 0.25 μm, and the column flow rate is 1.5 ml / min. , 34 cm / sec. , 17 psi (constant pressure mode), the column oven temperature was first 65 ° C. to 120 ° C. (3 ° C./min.), And then heated to 120 ° C. to 250 ° C. (5 ° C./min.). The detector was MSD, EI, 70 eV, and the inlet temperature was 250 ° C.

  As a result of this gas chromatograph mass spectrometry, Avan has a non-oral environment that does not contain artificial saliva (assuming the scent smelled by the nose) and an oral model environment that contains artificial saliva (assuming the scent of the oral cavity). The value obtained by calculating the dance difference was defined as RN-Factor.

  RN-Factor was calculated for each component such as Isoamyl acetate, and RN-Factor of each component was calculated for each substrate. For example, when purified water was the base material, Isoamyl acetate was 0.81, Butyl butyrate was 1.08, Isoamyl butyrate was 1.29, Isoamyl isovalerate was 1.44, and RN-Factor such as Octanol 1.31 was obtained. When this is multiplied by the first formulation, the isoamyl acetate is 40.7, the butyl butyrate is 10.8, the isoamyl butyrate is 12.9, the isoamyl isovalerate is 7.2, and the Octanol 3.9. When the fragrance | flavor prepared based on this was added to the base material, the drink with the fragrance close | similar to a target object was able to be created.

(Confirmation test for correction products)
The volatilization amount of the volatile component measured in the non-oral environment and the intraoral model environment was compared with the amount of the volatile component measured in the intraoral model environment using the flavor calculated using the RN-Factor.

  When the standard flavor was added to the intraoral model environment, there was a decrease in each fragrance component compared to the case where the standard flavor was added in the non-oral environment. On the other hand, when the flavor calculated by RN-Factor was added to the sample to which saliva was added, the same numerical value as in the case of the non-oral environment was obtained on gas chromatography mass spectrometry. FIG. 1 shows the results of gas chromatograph mass spectrometry of the present invention when the base material is purified water.

(Confirmation of effect)
When a standard flavor was added to the non-oral environment and the intraoral model environment, a comparison of sensory tests of aroma was performed when the flavor calculated using the RN-Factor was added to the intraoral model environment.

  The panel elected eight members from the research department. There are five men and three women. Age structure is 5 people in their 20s and 3 people in their 30s. Samples were prepared by adding a standard flavor to the non-oral environment solution and the oral model environment solution for each of the three base materials (purified water, fruit juice, and puree) and the flavor calculated using the RN-Factor. Three types of samples added to the intraoral model environment solution were prepared, and random three-digit numbers were given as labels. The sample was subjected to evaluation at room temperature. The evaluation items were selected in advance by selecting words from the 40 evaluation terms, including blueness, sweetness, banana-like, fruity, and strength. The strength of each item was evaluated on a 9-level scale of 1-9.

  The panel smelled the samples presented in a random order and performed sensory evaluations on the above evaluation items. The evaluation results were analyzed by a one-way analysis of variance method and a multiple comparison method (Duncan method) using commercially available statistical analysis software SPSS13.0J.

  Tables of results are shown in Tables 1, 2, and 3. I, II, and III represent the test results in the non-oral environment, the test results in the oral model environment, and the test results in the oral model environment using the flavor calculated using the RN-Factor, respectively. Yes. We examined whether there was a difference between samples for each evaluation item using one-way analysis of variance and multiple comparison method (Duncan method). The numerical value of a result is represented by the average value of nine steps of 1-9, and the side alphabet shows the result of a significant difference. This shows that there is no difference between samples with the same letter.

  From the table, I and III have a similar fragrance because there are many items that are judged on the panel that there is no difference between I and III, and that only II is sensually different. Rated it different. Therefore, it turned out that the blending method by this RN-Factor is effective for perfume development.

  In the present invention, by simply collecting the aroma of the object by a new method, the existing analyzer can be used, and the blending of the fragrance can be made much faster using the existing fragrance components. Further, in the case of a beverage that uses a straw such as a brick pack in a commercially available product, that is, a beverage that does not smell from the nose, the odor closer to the target can be reproduced in the oral cavity.

Reproduction of aroma component aeration in the presence of artificial saliva in the absence of artificial saliva and in the presence of artificial saliva, and in the presence of artificial saliva in a sample prepared by the correction method of the present invention when the base material is purified water Gas chromatograph mass spectrometry result showing the property.

Claims (4)

Add the fragrance composition to the oral model environment solution containing artificial saliva in the base and the non-oral environment solution not containing artificial saliva, collect the aroma components that volatilize, analyze the components, and difference between the two A method for blending a fragrance, in which a correction value is calculated from the fragrance composition to correct the composition ratio of the fragrance composition. Aroma volatile from the fragrance composition is aerated with the carrier gas into the oral model environment solution containing artificial saliva in the base and non-oral environment solution not containing artificial saliva, and the discharged aroma components are collected respectively. Then, component analysis is performed, and a fragrance blending method is performed in which a correction value is calculated from the difference between the two to correct the composition ratio of the fragrance composition. Artificial saliva contains alpha-amylase, an inorganic salt, and animal mucin, The fragrance | flavor preparation method of Claim 1 or 2 characterized by the above-mentioned. The fragrance | flavor prepared according to the composition ratio correct | amended by the method of Claim 1 thru | or 3.

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