CN107429195B - Fragrance composition - Google Patents

Abstract

The present invention discloses a perfume composition comprising components having synergistic odor profiles, the perfume composition being prepared by: selecting a first inactive component in the first mixture that most closely resembles the odor profile of the candidate active component; selecting a second inactive component in the first mixture that is least similar in odor character to the candidate active component; preparing a second mixture in which the first inactive component is replaced by an equivalent strength concentration of the candidate active component and the second inactive component is replaced by a known active from the same odor class as the second inactive component; the candidate active component is then selected for the preparation of the composition if the odor of the second mixture is significantly more intense than the odor of the first mixture, in which case the candidate active component is considered to exhibit elastic activity.

Description

Fragrance composition

Technical Field

The present invention relates to perfume compositions having enhanced organoleptic properties, compositions comprising such perfume compositions, and methods of making and using such compositions. The present invention includes perfumes created using materials capable of synergistic blending.

Background

Odor detection is achieved by olfactory receptors located in neurons of the olfactory epithelium of the nasal cavity. The signals from these neurons pass to the olfactory corpuscles in the olfactory bulb and on to the higher centers of the brain for further interpretation. Each receptor neuron expresses a class of olfactory receptors, and this single class of olfactory receptor neurons is distributed throughout the olfactory epithelium. The output fibers from these scattered neurons converge together on a single olfactory body in the olfactory bulb. Thus, signals from olfactory neurons encoding similar molecular properties/parts carrying the same scent information content will tend to converge on the same olfactory corpuscle in the olfactory bulb. A single odorant molecule will typically excite more than one class of olfactory neurons, and the excitation pattern will be reproducible and unique to that molecule.

In this process, the odorant molecules are first fragmented and characterized by odorant receptors. Then, similar features of different odorant molecules enhance each other at different odorant receptors and at the olfactory bulb level. The whole is then reintegrated to provide a perception of smell, which can be as simple as a single perception. In this way, many odorous molecules emanating from a flower can excite multiple neurons whose signals recombine to produce a single olfactory experience that a viewer can identify as being unique to a particular flower. Different flowers may emit many of the same substances, but differences in levels and composition will reintegrate to produce different sensory perceptions, which may be identified as being from different flowers.

Such a combination method has been proposed previously, but the detailed process involved is far from known. The complexity of the combinatorial mechanism has been a feature of the re-repetition of olfactory studies. Early studies of odor mixtures attempted to map and classify the sensory phenomena when odors were mixed, and developed terms to describe the observed changes in overall intensity observed. Due to the complexity of the phenomena involved, these studies are limited to binary mixtures.

Progress at the biological level has proven to be equally troublesome. It has been observed that a single olfactory neuron integrates several chemical signals simultaneously. However, researchers emphasize that complex interactions between components occur and that responses of olfactory neurons cannot be easily inferred from responses of their components. They found that events occurring at the receptor neuron itself, which do not promote subsequent events at the olfactory bulb, can be associated with changes in perceived odor, for example, due to one odorant dominating or even masking the effect of another odorant. Natural odorants will induce multiple chemical integrations at olfactory receptor neurons, which may be equivalent to shifts in their odorant coding properties, so that they may play a major role in the perception process as a whole.

Thus, the problems underlying the challenges of researchers attempting to understand odors become more apparent, and the complexity and non-linearity of the observed phenomena make reliable classification even more difficult.

In nature, it is common for the scent experience to be caused by a complex mixture of scent molecules and this mixture is often perceived as a single perception. This condition can be observed in animals and insects where olfactory signals can drive critical behaviors. For example, moths can identify flowers that give off more than 60 substances, 9 of which are detected by the olfactory system. These have been shown to exhibit a single perception that can drive flower foraging behavior. Coding is organized by a cluster of olfactory-corpuscle coding units thought to combine different features of molecular stimuli into a single perception (by unknown mechanisms).

In human studies, the specific outcome of such odor mixing is variable and unpredictable, but some broadly classified responses are often observed.

The convergent nature of the processes taking place in the high centers of olfactory processing necessarily means that odor mixtures are not always a simple combination of their components. That is, a person may typically perceive a complex mixture of scents as a single whole, while also being able to break down the experience into sensory subunits. For example, when malodors and aromas are mixed, the experience can often be divided such that the relative distribution of each odor type with respect to the overall odor can be judged. Thus, there is one paradox: the mixture may be perceived as a single perceptual experience, and the experience may incorporate segmentation.

The outcome of introspection may not reflect the relative intensity of the component stimuli, or even their odor characteristics. However, this process can be completely reproducible, which can be used to design new products that deliver useful benefits, such as deodorant perfumes.

In such masking scenarios, it is common for one scent to reduce the perception of a second, less desirable scent. This is a common practice and approach that has been developed to optimize the process. Examples of synergistic interactions between odors are extremely rare in comparison.

In compiled studies based on results from 520 binary mixtures, the most likely result of odor mixing at levels above the threshold is that the total intensity of the mixture is lower than the sum of the intensities of the components and lower than would be expected by auto-addition according to Stevens' Law. The strength of a single material tends to increase as a logarithmic function of its concentration (stevens's law), so the first of these findings is not unexpected, however the second is even more surprising. It has also been found that one of the two components reduces the strength of the other component more than the opposite. They also found that the addition of a third, fourth or fifth equivalent strength component did not result in any increase in overall strength. This indicates a strong compressor mechanism in operation.

As indicated above, it was found that synergistic enhancement effects are less common. When found, they are considered to be associated with a "synthetic phenomenon" in which, when the two components are mixed, new and different odor qualities are produced. When subthreshold levels of odorants were mixed, some odor was perceived, but the observation could not be reasonably accounted for. It follows that any study of these effects will require both intensity and odour characteristics to be measured simultaneously.

Synergy has been described as a higher level of sensory impact than would be expected based on the impact of the unmixed components. One example is the addition of a subthreshold amount of one odorant, resulting in a small but measurable increase in the perceived intensity of the other (beverage) aroma or the perceived sweetness of the super-threshold sucrose. It is believed that the addition of a small amount of one substance can occasionally result in a significant increase in the intensity of the fragrance or aroma. However, these examples may not be considered as synergistic, deterministic examples unless the subthreshold stimulus itself has no odor. Due to the statistical nature of the threshold measurement (e.g., the level at which 50% of the subjects can detect their presence and thus 50% of the subjects cannot detect their presence), the added material will be supra-threshold for many subjects.

In view of such issues, the first clear unambiguous illustration of the synergy of odor detection in humans is shown. The material is maple lactone mixed with volatile carboxylic acid, acetic acid and butyric acid. Generally, at the detection threshold of a binary mixture, the threshold concentration of each component tends to be lower than the threshold for the component smelled alone, a phenomenon known as Agonism (aginism).

Researchers have extended their research to 3-component mixtures, but no general topic has emerged. They concluded that the rules for mixture interactions were such that each mixture had to be handled individually and empirically.

In another supra-threshold study, a binary mixture of fruity and woody scents using both pre-and post-nasal stimulation was examined. The fruity intensity may increase or decrease in the mixture depending on the level of the woody component. Synergy was reported based on electroencephalographic measurements, where amplified peak amplitudes of N1 were found in some of the mixtures. Other compounds smelled postnasally showed increased P2 amplitude during electroencephalography scans. These results may be evidence that sensory and cognitive processes are simultaneously functioning during scent perception.

The study of alkyl sulfides and mercaptans led to the conclusion that the mixing of such materials with similar chemical structures can be characterized by an average effect over all components.

The binary mixture of L-carvone (aniseed) and eugenol (clove) is present as a physical mixture at one nostril, separately at each nostril relative to each odorant (dichorism mix). Psychophysical and electroencephalographic responses were recorded. The second sniff mixture was perceived as stronger than the physical mixture. The perceived odor characteristics also differed between the two evaluation methods. The electroencephalographic response of the dichoristic mixture showed a difference between the P1 and N1 (more sensory) peaks. All results taken together show that significant left-right hemispheric interactions occur in the high-level center of the brain (or at least after sniffing the corpuscles) and that the periphery is also where significant interactions occur.

In a recent publication, it was shown that the quality (character) of the mixture is independent of any particular individual component, indicating that we are more or less synthetically perceiving the odor mixture as a single perception. In their research, the odor of a mixture and its pleasure are generally intermediate between each of the individual components.

WO2002049600, which is incorporated herein in its entirety by reference, discloses perfume compositions having specific components to promote a relaxed emotional state.

The present invention seeks to address at least some of the problems described above. In particular, to identify groups of odorous ingredients that can be used to produce synergistic odors or perfume compositions, and the perfume compositions derived therefrom.

Disclosure of Invention

The present invention relates to perfumes created using materials capable of synergistic blending in a scent or fragrance mixture. The invention also includes products formed by incorporating such perfumes.

In one aspect of the invention, there may be a method of preparing a perfume composition by including materials that, when substituted for components with similar odor characteristics in any of the multi-component embodiments described herein, provide an increase in intensity for these new mixtures relative to a similar use of the disclosed non-elastic ingredients.

Drawings

Fig. 1 is a diagram showing a threshold approximation.

FIG. 2 is a bar graph showing normalized intensity scores for examples 1-12.

FIG. 3 is a bar graph showing the average intensity scores for examples A-F.

FIG. 4 is a bar graph showing the average intensity scores for example G-O.

Fig. 5 is a bar graph showing odd-numbered odor groups.

Fig. 6 is a bar graph showing even numbered scent groups.

Fig. 7 is a graph showing the average sample intensity of perfume.

Detailed Description

The present invention surprisingly found that a specific combination of ingredients can be used to produce a synergistic effect, wherein the sensory impact of the ingredients in the mixture, or of the mixture as a whole, is greater than would be expected based on the impact of the unmixed components. Further, the present invention relates to compositions comprising synergistic effects, and methods of using such compositions to achieve a desired response in a user, such as a human.

Those ingredients in the mixture that stand out more than expected are referred to herein as "elastic" materials, and without being limited by theory, it has been found that certain components of the perfume composition are more elastic than others. The present invention identifies these resilient odour components, including how such resilient odour components are identified and threshold levels are determined, and further generalises how they can be advantageously combined with other perfume components. The elastomeric materials may also combine their odor with other ingredients present to create new and different odor characteristics in the mixture.

In a first aspect of the invention, the perfume composition comprises components from specific groups. The groups described below are referred to as group 1A, group 1B, and group 1C. The perfume composition of the present invention may comprise one or more components from one, two or all three of group 1A, group 1B and group 1C.

The first component (group 1A) is selected from the group consisting of: acetyl cedrene, synthetic camphor powder, cedar oil, cineole, cinnamaldehyde (10), labdane butter, citral dimethyl acetal, melodious musk, ligustral, beta-dihydrodamascone (10), delta-dihydrodamascone (10), ebony-l (10), ethyl vanillin (10), eugenol, Galbanone (10), gamma undecalactone, piperonal, hexyl cinnamaldehyde, ambergris ketone, alpha-isomethyl ionone, quincunol, methyl piperitol, methyl cinnamate, methyl 2 butyrate, silveranone, silverial, alpha-terpineol, allyl hexanoate, ramicinocin (10), anisic aldehyde (10), black pepper oil, santalol (10), Habanolide, dihydroeugenol, melonal, Violetyne (10), methyl benzoate, raspberry ketone, and mixtures thereof. Group 1A includes components that are active or elastomeric components in the perfume compositions of the present invention.

Throughout this specification, when an individual component includes "(10)", it means a 10% solution of the material in a solvent, preferably a non-odorous solvent, including, for example, dipropylene glycol.

The second component (group 1B) is selected from the group consisting of: alkyl alcohols, phenyl alkyl alcohols, terpene hydrocarbons or mixtures thereof. The components of group 1B may be added as part of the natural oils. The components of group 1B are described herein as "accelerators".

Specific examples of group 1B components include: linalool, aurantiterpene, phenylpropanol, phenylethanol, alpha-terpineol, marjoram alcohol, rose alcohol, citronellol, tetrahydrogeraniol, tetrahydrolinalool, geraniol, and mixtures thereof. It has been found that the components of group 1B further enhance the synergistic effect of the components of group 1A.

The third component (group 1C) may be selected from the group consisting of: aldehyde C12(10), anethole, Ambermax (10), isobornyl acetate, watermelon ketone 1951(10), coumarin, cuminaldehyde (10), ginger oil, synthetic oak moss, green leaf oil, methyl decenol, vetiver oil; and mixtures thereof. Materials from group 1C may also be added as part of the natural oils. Materials from group 1C are optional in the composition.

As indicated above, one or more components from one, two or three groups may be used in the present invention. One or more components from group 1A are present in the composition in the following amounts: from about 20% to about 80% by weight of the composition, or from about 30% to about 80% by weight of the composition, or from about 40% to about 80% by weight of the composition, or from about 50% to about 80% by weight of the composition, or from about 30% to about 60% or from about 50% to about 60% by weight of the composition. The number of individual components from group 1A may be one, two, three, four or more than four. When present, one or more components from group 1B are present in the composition in the following amounts: from about 5% to about 50% by weight of the composition, or from about 15% to about 50% by weight of the composition, or from about 25% to about 50% by weight of the composition, or from about 15% to about 25% or from about 10% to about 20% by weight of the composition. When included in the composition, the number of individual components from group 1B can be one, two, three, four, or more than four. When present, components from group 1C are present in the composition in the following amounts: up to about 35% of the composition or about 18% or less by weight of the composition. When included in the composition, the number of individual components from group 1C can be one, two, three, four, or more than four.

Accordingly, one aspect of the present invention includes a combination of the aforementioned group 1A, group 1B, and group 1C.

A second aspect of the invention includes materials, or materials excluded, whose use in compositions is limited. Two groups of these materials exist in the present invention. Group 2A and group 2B.

Group 2A includes allyl cyclohexyl propionate, pteritol (Bangalol), p-tert-butylbenzene propanal (Bourgel), blackcurrant base, ethyl Methyl phenyl glycidate, vinyl tridecanoate, lilac pyran, lavender dioxane (Herboxane), cis 3 hexenyl Methyl carbonate, Jasmatone, citral, lilial, Methyl anthranilate, Methyl lactone (Methyl Laitone), phenyl ethyl acetate, Rose oxide (Rose oxide), styryl acetate, musk teson, vanillin, Ylang oil (Ylang oil), and mixtures thereof.

Group 2B includes isononyl acetate, linalyl acetate, and mixtures thereof.

When present, the materials in group 2A or group 2B are independently present in the composition at no more than about 1.0% by weight of the composition, and more preferably no more than about 0.6% by weight of the composition (other than as a component of a natural oil). Thus, the materials of group 2A, when used independently of the presence in natural oils, may be present in an amount of from 0% to about 1.0% or up to about 0.6% by weight of the perfume composition. Similarly, the materials of group 2B, when used independently of the presence in natural oils, may be present in an amount of from 0% to about 1.0% or up to about 0.6% by weight of the perfume composition.

The total concentration of non-essential oil additions from the materials of groups 2A and 2B comprises less than 2% by weight of the total perfume composition, and more advantageously comprises less than about 1% by weight of the total perfume composition. In some embodiments, the perfume composition of the present invention does not contain any material from group 2A, and in some embodiments, the perfume composition of the present invention does not contain any material from group 2B.

All percentages are based on the total weight of materials in the perfume composition (except for materials added as part of natural essential oils), the total percentage of essential oils or the like (where they are the specified ingredients), and are 10 times the actual concentration of the pure material, where it is labeled as followed by (10), such as aldehyde C12 (10). In the case where the material is present in two or more groups, its distribution should be considered as being divided between the groups (e.g., creosol, alpha-terpineol); for example 50:50 between the two groups.

The present invention has surprisingly found that a specific combination of ingredients can be used to produce a synergistic odor or fragrance composition. Without being limited by theory, it has been found that certain components of the perfume composition are more elastic than others. The resilient scent component is a scent component that provides greater characteristics to the overall composition than would otherwise be expected based on the scent characteristics of a single material. The present invention identifies elastic odor components that are more easily identified in the mixture and whose odor characteristics become clear components of the odor characteristics of the mixture as a whole. Another benefit of the present invention is that the presence of the elastomeric material can result in new and different odor profiles being generated in the mixture. The present invention is quite useful because it enables the provision of more intense, or more complex, or unique fragrances, while avoiding the need to add more ingredients to the composition. For example, where less elastomeric component is used in the perfume composition, the elastomeric component may impart a higher perceived intensity.

When a mixture of scents is produced from equal proportions of equal strength components, mixtures containing a significant proportion of "elastomeric materials" are typically associated with higher perceived strength than mixtures in which they are not present.

The odor character contribution of the second group of materials, "non-elastic materials", is reduced when mixed with more elastic materials. In some compositions, these non-elastic materials may be completely masked. Thus, the amount of non-elastic materials in the composition, such as those listed in group 2A and group 2B, should be limited to the levels described above, if used. The elastomeric components, such as those in group 1A, should be present in a significantly higher amount than the components in group 2A and/or group 2B.

Thus, the aforementioned aspects of the invention include perfume compositions comprising one or more components selected from at least one of groups 1A, 1B and 1C in combination with components from one or more of groups 2A and 2B.

When the elastic material and/or the mixture comprising said elastic material is reinforced, the third group of materials tends to be present, but they do not generally show this prominent olfactive contribution by themselves. These are group 1B accelerators. Many of the group 1B accelerators are alcohols, which are common blending materials. The present invention surprisingly found that the group 1B material contributes to the contribution of the elastomeric material in the perfume composition. Group 1B accelerators increase the strength of the elastomeric component. The group 1B promoter will increase the strength of the group 1A material, while the odor of the group 1B promoter is not emitted significantly. Group 1B promoters are optionally included in the perfumes of the present invention.

The threshold concentration of the scent component is the minimum concentration at which a scent is perceived. These behaviors can be manifested in mixtures in which all components are present in equal parts at threshold concentrations as equal strength stimuli. The threshold concentration, which can be identified relatively clearly for all materials, can be considered as a standard level for producing equivalent intensity concentrations. Each material will be equally perceived if no interaction occurs between equally strong components of the mixture. If some materials become more olfactory and/or intense, it is judged that their odor has been enhanced by the presence of other materials. Thus, forming a mixture with materials of equal strength gives a useful method to identify when and how enhancements may occur within the mixture or to the mixture as a whole. Such enhancements are more easily identifiable at threshold levels of perception of the odor component.

A useful solvent for preparing a liquid phase sample of threshold concentration is dipropylene glycol (dpg). The concentration of perfume materials is typically small in such compositions, so that at a threshold the physical effect between the materials will be very small, and the main effect will be organoleptic.

The present invention includes perfume compositions comprising components that are consistently perceived in a mixture at an intensity above a threshold value while their concentration remains at a threshold concentration level. Thus, the intensity of the odor of one or more components is increased by the present invention even if the actual amount of one or more components is at the threshold concentration level.

Note that the intensity of a particular note of the scent profile can be increased by using a small addition (trivisual addition), but the present invention goes beyond using only the small additions described herein. The small additions include adding materials with the same odor notes to achieve a greater odor. For example, the materials may be combined at or below a threshold concentration such that, when combined, they produce an odor above a threshold perceived level. This can be achieved by combining only materials that each act partly or wholly on the same receptor. Such groups of materials will generally be identifiable in that they have similar odors or shared odor notes. For example, combining subthreshold amounts of different rose-scented materials may produce a supra-threshold mixture with a rose scent. However, this alone is not the mechanism of the present invention. The elastomeric odor component of the present compositions produces enhanced effects and odor intensity benefits. This can be achieved without the simultaneous presence of other materials having a common odor profile. Of course, the present invention does not exclude their use in combination with such materials. The method of blending only materials with similar odor characteristics is described above by way of example to distinguish this alternative from "sharp enhancement" based on small amounts of additive effects.

In addition to the elastomeric odor component used in the present invention, a second component may be added. The added second component material may not itself play this prominent olfactive role in the overall odor profile of the mixture. When among the most intense components, they may not be perceived, however, they are not so strongly diluted and do not detract from the strength properties of the mixture comprising the elastomeric material. It has been surprisingly found that the combination of the elastic odor component with the second component results in a mixture having useful, enhanced properties (e.g., higher perceived intensity of the mixture with the elastic odor component).

The perfume or fragrance composition according to the present invention can be used in a variety of products. As used herein, the term "product" shall refer to products that include the perfume compositions described above, and includes consumer products, medical products, and the like. Such products can be in a variety of forms including powders, bars, sticks, tablets, creams, mousses, gels, lotions, liquids, sprays, and sheets. The amount of perfume composition in such products may range from 0.05% (as for example in low odour skin creams) to 30% (as for example in fine fragrances) by weight thereof. The incorporation of perfume compositions into these types of products is known and the prior art can be used to incorporate perfumes for use in the present invention. In various methods of incorporating the perfume composition into a product include mixing the perfume composition directly into or onto the product, but another possibility is to adsorb the perfume composition onto a carrier material and then incorporate the perfume-plus-carrier mixture into the product.

To provide a more concise description, some of the quantitative representations presented herein are not intended to be limited by the term "about". It is understood that each quantity given herein is intended to refer to the actual given value, regardless of whether the term "about" is explicitly used, and also to refer to the approximation to such given value that would reasonably be inferred by one of ordinary skill in the art, including approximations due to experimental and/or measurement conditions for such given value.

The present invention includes perfume compositions and products containing such perfume compositions, as well as methods of using such perfume compositions and products. The method of use comprises providing a perfume composition or product as described herein to a person and having the person smell the resulting smell to achieve the desired effect. The desired effect may include, for example, providing emotional benefits, cognitive benefits, and/or improved interaction with other perceptual patterns to a user (such as a human).

The present invention also provides a method of evaluating certain perfumes/odors and determining a threshold concentration of a perfume or fragrance that can be used to identify the benefits of the present invention. This evaluation can then be used to produce a perfume composition (or product containing a perfume composition) having a desired threshold amount of a desired fragrance. Thus, a method of determining a threshold amount of fragrance and using the results of the evaluation to prepare a perfume composition is provided. The method can further include forming a product having the perfume composition.

In the following examples and description, the process includes the use of a solvent. The solvent in the examples is dipropylene glycol, sometimes referred to herein as dpg, although other solvents with little or no odor may also be used.

In these examples, the threshold value of each ingredient at dpg was first determined, and then each ingredient was incorporated into the perfume at that level. Fragrances were also produced with all ingredients present at approximately 0.3 times the threshold, and another group with all ingredients present at 0.1 times the threshold concentration. For illustrative purposes, the following experiment was performed in a 125ml brown glass jar using a 10ml aliquot of the fragrance.

Threshold measurement

One suitable Method for ascertaining the detection and/or recognition threshold of each odor component from a liquid solution is derived from the limiting Method (Method of Limits) (described in ASTM 'Manual on Sensory Testing Methods', STP 434(1968), American Soc for Testing Materials, philiadelphia, pa.19103, USA, the entire contents of which are incorporated herein by reference). Initial experiments were performed to determine approximate threshold levels. Concentration series of samples were prepared and diluted until perfume odor was indistinguishable. The fragrance component in dipropylene glycol in the ascending concentration series starting below the threshold level is then presented to each evaluator, who then judges the presence or absence of the specified odor quality in each sample. This series continues until the judgment changes (from "absence" to "presence"). Data from more than 15 assessments were pooled and analyzed to extrapolate the concentration in the series at which the target odor would be detected (and/or identified) in 50% of the assessments.

Hypothesis detection Rate and log₁₀The relationship between concentrations is sigmoidal, so that for each component a 50% detection rate is predicted, and a fit line is obtained following the following function:

wherein y is percent detectable rate and x is log of concentration percent of the components in dipropylene glycol₁₀K is a constant that determines the gradient of the sigmoid function, and the threshold is the concentration value at the inflection point of the sigmoid curve (and, therefore, the concentration at the 50% detection rate).

The values of k and threshold are approximated and then fitted using the solveradd-in module of Microsoft XL 2007 such that the Root Mean Square Error (RMSE) between the observed and predicted points is minimized. The resulting RMSE for all fitted lines was below 10% and was considered acceptable. Figure 1 shows a threshold approximation for one sample fragrance ingredient.

Evaluation of odor intensity measurements

A team of male and female evaluators was used in the evaluation of sample strength. In this work, the assessor was between the ages of 25 and 65. They were selected for evaluation based on their ability to correctly rank the odor intensity of serial dilutions (at dpg) of perfume ingredients. The standard perfume ingredient used in the conference on odor assessment was benzyl acetate prepared in the series of dilutions listed in the table below. Each dilution is associated with an odor intensity score. Other materials may be used in a similar manner.

Standard dilutions as above are given during the evaluation and are provided as a reference to help the evaluator during the evaluation.

The examples tested were prepared as described herein. An example consists of a dilution of a mixture of materials at or above their respective threshold concentrations in dpg. Generally, approximately 10g of each solution was placed in a capped 125ml jar and allowed to equilibrate at room temperature for a minimum of 2 hours. The assessment was performed by an assessor removing the cap and sniffing the contents. Jars were evaluated in random order. The evaluator assigned a score of between 0 and 8 to each sample, where 0 corresponds to no odor and 8 represents a very strong odor. Thereafter, at least 15 evaluations were obtained for each sample.

Where the assessment of the samples is conducted over several meetings and/or with different subjects, comparison between the samples may be facilitated by normalizing the results for each sample between the meeting and the assessor. This may occur, for example, when too many samples are available to an evaluator to be reliably evaluated in a meeting. The data for examples 1 to 12 were analyzed in this manner, as described below.

The evaluator is presented with a segment of samples in a series of meetings to reduce the evaluation fatigue and inconsistencies associated with a large number of samples. The score for each assessor was normalized as follows: for each evaluator, the average of all individual scores within the meeting is calculated

And calculating the standard deviation(s) of the samples of the same score group_{(evaluator, conference)}). Using these statistics, each of the assessors' data points is converted to a normalized score, i.e., the ith score (x) for each assessor_i) Recalculated to (x)_std,i) The following are:

the data were further analyzed using analysis of variance. The average of all normalized scores for all evaluators was then calculated for each sample

The examples were prepared using a variety of fragrance ingredients listed in table a. All exemplary mixtures were prepared volumetrically based on the addition of a known small amount of each stock solution (in dpg) to a vial and dilution to the required amount with additional clean dpg. An ideal stock solution would be such that 20 μ Ι _ of each ingredient stock solution, when further diluted in a total of 20mL _ of solution, would deliver a solution of all ingredients at the estimated threshold concentration for each ingredient.

Stock solutions were prepared gravimetrically in serial dilution steps: for example, to prepare a 0.0005% solution of one ingredient, 0.50g was added to 9.50g dpg to give a total of 10.00g of a 5% solution; then 0.15g of this solution was diluted in 14.85g dpg to give a total of 15g of a 0.05% solution; this second solution was then diluted with the same dilution factor by adding 0.15g of the 0.05% solution to 14.85g dpg, resulting in 15g of the 0.0005% solution.

The mixture stock was stored in a refrigerator in a container with very little remaining headspace above the solution (to minimize volatile loss).

Each example was prepared by adding the target amount of each stock solution to a vial and making up to a total of 20.0 g. The mixtures were then stirred and allowed to equilibrate. Each mixture was used as is and further diluted by a factor of 3/10 and 1/10 to produce a subthreshold mixture. In this way, 3 concentrations of each mixture were prepared: (1) each component was at a threshold concentration, (2) each component was at a 0.3 threshold concentration, and (3) each component was at a 0.1 threshold concentration.

TABLE A

Example 1: 141.5 μ L of 0.10% solution of cis-3-hexenol dpg, 50.7 μ L of 5.00% solution of cedar oil dpg, 6.1 μ L of 9.93% solution of methyl danlifolier dpg, 44.6 μ L of 1.00% solution of ethyl crocetin dpg, and 18.4 μ L of 3.34% solution of citronellol dpg were added to 19.74mL of dpg and mixed.

Example 2: 18.4 μ L of a 3.50% linalool dpg solution, 15.1 μ L of a 0.98% ebony alcohol dpg solution, 18.9 μ L of a 7.32% methyl cinnamate dpg solution, 18.9 μ L of a 7.01% benzyl acetate dpg solution, and 18.4 μ L of a 3.34% citronellol dpg solution were added to 19.91mL of dpg and mixed.

Example 3: 189.3. mu.L of a 3.25% solution of citral dimethyl acetal dpg, 8.9. mu.L of a 5.00% solution of methyl piperonyl alcohol dpg, 20. mu.L of a 1.50% solution of nutmeg oil dpg, and 6.9. mu.L of a 0.01% solution of bifenthrin dpg were added to 19.77mL of dpg and mixed.

Example 4: 195.5 μ L of a 2.10% solution of α -terpineol dpg, 18.2 μ L of a 1.15% solution of dihydromyrcenol dpg, 19.5 μ L of a 1.00% solution of eugenol dpg, 6.9 μ L of a 0.05% solution of ethyl methyl-2-butyrate dpg, and 88.7 μ L of a 0.50% solution of phenylethyl alcohol dpg were added to 19.67mL of dpg and mixed.

Example 5: 18.4 μ L of a 3.50% solution of linalool in dpg, 8.9 μ L of a 0.04% solution of eucalyptol in dpg, 9.9 μ L of a 5.21% solution of kestone in dpg, and 9.2 μ L of a 0.55% solution of delta-dihydrodamascenone in dpg were added to 19.95mL of dpg and mixed.

Example 6: mu.L of dpg solution of 1.01% ligustral, 15.1. mu.L of dpg solution of 4.99% roseola red oil, 13.8. mu.L of dpg solution of 10.00% methyl cinnamate, 6.9. mu.L of dpg solution of 0.01% bifenthrin, and 126.2. mu.L of dpg solution of 0.05% geranium oil were added to 19.83mL of dpg and mixed.

Example 7: mu.L of a 0.02% solution of p-tolylmethyl ether in dpg, 19.2. mu.L of a 13.11% solution of isononyl acetate in dpg, 20. mu.L of a 0.0010% solution of methyl lactone in dpg, 18.2. mu.L of a 1.20% solution of ethylmethylphenylglycidate in dpg, and 66.3. mu.L of a 0.05% solution of indole in dpg were added to 19.87mL of dpg and mixed.

Example 8: mu.L of a 0.12% solution of cyclamen aldehyde dpg, 19.2. mu.L of a 13.11% solution of isononyl acetate dpg, 18.2. mu.L of a 0.42% solution of coumarin dpg, 18.3. mu.L of a 9.49% solution of allyl cyclohexyl propionate dpg, and 103. mu.L of a 1.00% solution of rose carbinol dpg were added to 19.82mL of dpg and mixed.

Example 9: 17.8 μ L of a 0.00012% solution of lilac pyran dpg, 141.5 μ L of a 0.00071% solution of cis-3-hexenylmethyl carbonate dpg, 19.4 μ L of a 0.00053% solution of green leaf oil dpg, and 186.9 μ L of a 0.0075% solution of phenylethyl phenylacetate dpg were added to 19.63mL of dpg and mixed.

Example 10: 17.1. mu.L of a 1.02% solution of Galbanone dpg, 17.1. mu.L of a 2.48% solution of vetiver oil dpg, 19.5. mu.L of a 1.00% solution of eugenol dpg, and 17.7. mu.L of a 1.21% solution of methyl anthranilate dpg were added to 19.93mL of dpg and mixed.

Example 11: 183.3. mu.L of a 0.011% solution of linalyl acetate dpg, 19.2. mu.L of a 0.013% solution of isononyl acetate dpg, 18.5. mu.L of a 0.0025% solution of ethyl vanillin dpg, 18.3. mu.L of a 0.0087% solution of allyl cyclohexyl propionate dpg, and 126.2. mu.L of a 0.00032% solution of geranium oil dpg were added to 19.63mL of dpg and mixed.

Example 12: 17.8. mu.L of a 0.14% solution of convallaria pyrane dpg, 22. mu.L of a 5.00% solution of isobornyl acetate dpg, 18.5. mu.L of a 2.68% solution of ethyl vanillin dpg, and 29.7. mu.L of a 5.04% solution of phenylethyl phenylacetate dpg were added to 19.91mL of dpg and mixed.

The range of odors obtainable according to the present invention is extremely wide and is not limited to any particular segment. The following odor descriptions of the perfume compositions in table 3 show non-limiting examples of the breadth of odor types that can be obtained according to the present invention. The strength results are shown in table 4.

TABLE 3

TABLE 4

Two-way variance (two-way ANOVA) analysis was performed on the data set: the two qualitative predictors chosen, referred to as "examples", correspond to the samples evaluated, and "concentrations", correspond to the three sample intensities; threshold, 0.3 × threshold, and 0.1 × threshold.

ANOVA determined a significant fit of the two-factor model to the data at 95% confidence level (F-23.440, d.f. -13, p)<0.05,R²0.706). The sum of squares analysis of type I exhibited the examples (F9.703, d.f. 11, p)<0.05) and concentration (F98.993, d.f. 2, p)<0.05) significant contributing effect of the factors on data variability, as such significant differences are exhibited between samples at concentrations near the threshold. Model fit statistics are shown in tables 5 and 6.

TABLE 5

TABLE 6

FIG. 2 shows the mean and 95% confidence intervals for the normalized scores of the examples; it should be noted that examples 1-6 are shown with confidence scores >0, whereas examples 7-12 have negative averages.

Post-hoc Duncan analysis (Post-hoc Duncan analysis) of the samples revealed significant differences between the examples according to the invention (examples 1-6) and the comparative examples 7-12. In table 7, there were no average differences between members of the groups with the same letters, while there were significant differences between the average values of samples of different groups (critical p ═ 0.05). No samples belonging to both groups a and B were found. Therefore, it can be said that examples 1 to 6 are significantly superior to comparative examples 7 to 12.

TABLE 7

Examples A to O

In a series of further examples a to O, the strength of each mixture was assessed by the subjects in separate experiments using a one-way rating scale (the rating scale and its use are described in ASTM 'Manual on Sensory Testing Methods', STP 434(1968), see in particular pages 19-22, American Soc for Testing Materials, philiadelphia, pa.19103, USA, which is incorporated herein by reference in its entirety). In this rating, "no intensity" is rated 0, and the other intensities are rated as previously described. Perfume compositions were prepared according to the general procedure described above for examples 1 to 12. The weight percent of each component in the composition is shown in tables 8-13. 10ml of each perfume solution was placed in a 125ml brown glass jar and allowed to equilibrate. The subjects evaluated the jar contents and rated the perceived odor intensity. The procedure was repeated via 3 meetings until 15 evaluations were performed.

Examples a to O show the benefits of the invention: the mixture according to the invention, when present at a threshold concentration, will smell stronger than a similar mixture using a less active or inactive material according to the invention. In the examples, components with less or no activity are labeled "inactive". Components that are part of the present invention are labeled "elastic or active". In addition, the combination of the group 1a material and the group 1b material (or similar alkyl alcohol), both present at a threshold concentration, can deliver sensory stimulation at its intensity. The average or mean score for examples a-O is shown in fig. 3 and 4. Black bars indicate 95% confidence intervals.

TABLE 8

TABLE 9

Watch 10

TABLE 11

TABLE 12

Watch 13

Using the test methods described above, the perfumes produced according to the present invention exhibit higher odor intensity, and in some aspects, significantly higher odor intensity, than the comparative perfumes. For purposes of illustration, care should be taken that the perfume does not contain materials whose main odor characteristics are in common with other materials in the perfume. This effectively minimized (or excluded) additional effect caused by two similar odors at or around the threshold excites the same receptors and thus the above threshold activity levels are obtained at said receptors. Thus, the fragrances of the present invention are shown to have a higher intensity, which is caused by synergistic interactions between the ingredients. This phenomenon has traditionally been considered rare. The present invention allows for the formulation of fragrances with internal cooperativity in a reliable and reproducible manner. The present invention provides a method for formulating such perfumes, in addition, the perfumes themselves cover a broad odor spectrum and provide benefits. Perfumes are often one of the more expensive components of consumer products, and any such widely available strength increase is therefore valuable to the formulator.

Rapid test of elasticity

In another aspect of the present invention, there is a method for identifying whether a new material exhibits elasticity that is simple and relatively rapid to perform. In other approaches, multiple evaluations of many component mixtures are included in the equilibrium experimental design, however, if a test can be devised in which new material can be added to the standard mixture, there is a high likelihood that the elastic properties of the test material will become apparent, then the test is preferred. This is the purpose of this alternative rapid test method to determine elasticity. As used below, this method will be referred to as "rapid testing".

The approach taken is to form two mixtures in which all the components are inelastic and are present at a threshold concentration. There is also minimal odor character overlap between each ingredient. These components can then be replaced by the test material. Elastomeric materials are defined, in part, by the tendency to increase the strength of the mixture containing the elastomeric material. New components can be classified by measuring the change in perceived intensity that occurs when a known non-elastic material is replaced.

If the strength of the mixture is significantly increased by replacing the inactive components with new test materials, synergistic interactions will be introduced and the test materials exhibit "elastic" activity, as that term is used herein.

Composition of the test mixture

The same odor classes as described above were used to design the mixture of inactive substances. The odor spectrum is subdivided into ten broad odor categories. These categories are: floral, aldehydic, citrus/fresh, green/watery, herbal, woody/amber, powdery/musky, spicy, fruity-light, fruity-heavy. These descriptors are commonly used in the perfume art and are well known to those skilled in the art. They were distributed into two mixtures, such that one mixture contained the following odor groups: aldehyde, grass/water, woody/amber, spicy and fruity-rich; and another mixture contains citrus/fresh, herbal, powder/musk, fruity-bland and floral. The new test material should replace one of the inactive materials in the appropriate test mixture, preferably the inactive substance with the odor characteristics most similar to the test material.

The inventors have found that the rapid test is most effective when two active substances are present in the mixture. This method generally achieves a significant increase in strength compared to mixtures in which no active substance is present.

Overview of Rapid test protocol

Preferred rapid test protocols are outlined below.

It has proven preferable to use test materials in which one of the inactive materials has been replaced by an active substance. Thus, two "standard" active materials have been named for use with each of the mixtures of inactive materials. A standard active is a material that will be incorporated into a test mixture at a threshold concentration along with the test material. Both substituents should produce a mixture having a significantly higher strength than the original mixture in the absence of the active substance. The two "standard" actives have different odors and belong to different odor classes. They are listed in the experimental section below.

The invention includes a method for identifying and selecting new active substances whereby a candidate material delivers an enhanced intensity (greater than or equal to one unit on the standard scale described herein) when it replaces the inactive material in one of the two test materials described for that purpose, with or without the second inactive material being replaced by a known active material. Preferred active and inactive substances are described in the specification. The present invention includes the preparation of perfume compositions using substituted inactive materials or inactive materials.

The first stage of the test is to identify which class the test material belongs to and select the mixture with the most similar type of inactive substance to it. The unknowns would replace the non-elastic material from the same odor group. This mixture will serve as the basis for further exploration. Next, a non-elastic material that is judged to be the most different in odor from the unknown material should be selected. The non-elastic material will be replaced by elastic material from the same odor class. Examples of elastic materials for each odor class are given in the above text.

In view of the desired results in determining the effective benefit of substitution, and the ultimate goal of preparing compositions with suitable elastomeric components, the present invention includes a rapid test method. The method can be used to identify and select new active substances whereby candidate material delivers enhanced intensity (e.g., greater than or equal to one unit on the standard scale described herein) when it replaces the inactive material in one of the two test materials for this purpose. This may be done with or without the second inactive material being replaced by a known active material. Preferred active and inactive substances are described above.

The method may include the following processes. First, the user identifies and considers each of the inactive components in the two test mixtures. In step 1, an inactive component is selected which is most similar to the candidate material in terms of odor profile. This identified component is referred to as the "most similar" inactive material. This will identify which of the two test mixtures will be used in the following step. The next step (step 2) is to identify which inactive material selected from the test mixture of step 1 is the most different from the candidate material. Identification of the most different inactive materials is optional, however, it is preferred to identify the component in order to maximize the difference. The identified "most different" material will be replaced by a known active from the same odor class.

The third step is to reformulate the selected test mixture by replacing at least one of the two inactive substances identified in steps 1 and 2 above, and advantageously both (the most similar inactive substance and the least different inactive substance). For example, the most similar inactive substance (identified by step 1) may be removed and replaced with a candidate material of equivalent strength concentration, and the least similar substance may be removed and replaced with a known active substance of equivalent strength concentration from step 2. Examples of suitable concentrations of active substances are described above. The threshold concentration of the candidate material may be found using the methods described above.

In step four, the strength of the new mixture from step 3 can be evaluated using the preferred method described in the following paragraph. A candidate material is considered to have exhibited elastic activity if the new mixture is significantly stronger (e.g., one unit or more in strength) than the initial test mixture of inactive substances. This conclusion can be used to develop perfume compositions comprising candidate materials. Thus, it may be useful to develop a modified perfume composition using the method of the present invention, whereby at least one component has been substituted, e.g. an active component in place of an inactive component or vice versa.

Evaluation of "elastic Activity": the strength of a new mixture incorporating the new test material and the standard active should be evaluated relative to the strength of a related mixture of five inactive materials. The intensity scale used in the experimental section below is preferably used. This is a sensory scale in which sensory scores are shown by the standard concentration of benzyl acetate in dipropylene glycol. If the new mixture is significantly stronger than the blend of inactive materials (e.g., more than 1 unit using this scale), the new test material can be considered to exhibit "elastic" activity. A composition comprising the elastic material may then be prepared.

The formulations of the two test mixtures, as well as the two standard actives used with each, are given in the experimental section.

Experimental part 1: rapid testing of elastic Components

Sample preparation

All sample and reference solutions consisted of dilutions, in dpg units. 10g of each solution was placed in a capped 100ml jar and allowed to equilibrate at room temperature for a minimum of 2 hours. Evaluation was performed by removing the cap and sniffing the contents, and replacing the cap.

Segments of the samples are presented to the evaluator in a series of meetings in order to reduce evaluation fatigue and inconsistencies associated with a large number of samples. The samples are presented in order from the weakest intensity assumed to the strongest intensity assumed to minimize the residue of strong samples. The baseline mixture was presented first, after which all other test mixtures were randomized.

Evaluation protocol

In evaluating the strength of the samples, a cohort of male and female evaluators between the ages of 25 and 65 were used. They were selected for evaluation based on their ability to correctly rate the odor intensity of a series of dilutions of perfume ingredients (in dipropylene glycol, dpg).

The intensity measurements are based on standard concentrations of benzyl acetate. Prior to the evaluation conference, the panelists were presented with benzyl acetate, which was prepared as a series of dilutions (at dpg), as listed in the table below. Each dilution was associated with an odor intensity score.

i: standard dilution of benzyl acetate at dpg with corresponding fractions：

The standard dilutions as above are given during the evaluation and are provided for reference to help the evaluator during the evaluation.

Experimental sample：

Two sets of experimental mixtures were prepared and evaluated: group 1: 1a, 1b, 1c, 1d and 1 e; and group 2: 2a, 2b, 2c, 2d and 2 e.

In developing these samples, one inactive ingredient was selected for each of the odor groups: 1, aldehyde fragrance; 2, citrus scent/freshness; 3, green grass fragrance and water sample; 4, herbal fragrance; 5, radix aucklandiae and amber; 6, powder sample, musk; 7, spicy; 8, the fruit fragrance is strong; 9, light fruity; 10, floral. These materials were then used to prepare two 5-component mixtures, which formed the baseline samples in each group.

Group 1 samples were made from the odd odor group only; group 2 samples were made from the even numbered odor group only. This precaution ensures that all samples are made from ingredients selected from non-adjacent odor groups, thereby minimizing any overlap in odor characteristics between the inactive components in each mixture. All ingredients were incorporated at their estimated threshold concentrations (in dpg) using the method described above.

Each group consisted of 5 samples ：

(a) The baseline mixture was made of only 5 known inactive ingredients, each selected from a different non-adjacent odor group.

(b) A baseline mixture version made with one inactive ingredient replaced with a known active ingredient from the same odor group resulted in a mixture of 4 inactive ingredients and 1 active material (e.g., mixture 1b contained active material from groups 7, 7act in the table below).

(c) This second, "b" mixture forms the basis of a third mixture (c) in which the second inactive ingredient is replaced by a known active ingredient, resulting in a mixture of 3 inactive ingredients and 2 active ingredients (e.g., mixture 1c contains active materials from groups 7 and 9, 7act and 9act in the table below).

(d) And (e) preparing two subsequent mixtures (d) and (e), each mixture comprising 3 inactive ingredients and 2 active ingredients, using mixture "c" as its starting point. In these mixtures, one of the two active ingredients from "c" is replaced by an alternative known active ingredient from the same odor group.

The new active for the mixtures of (d) and (e) provides a virtual test material to demonstrate the usefulness (or uselessness) of the test method.

The 10 samples obtained are described in the table below.

ii: formulations for group 1 and group 2 samples

Sensory analysis

The perceived intensity of all the above mixtures was evaluated with reference to the benzyl acetate-fixed intensity scale. The mean intensity was recorded and compared to assess whether inclusion of the test material and known active resulted in a significant increase in perceived intensity compared to the corresponding 5-component mixture with no active.

Data analysis

Average intensity fraction, n 15:

iii average number table: group 1 (odd odor group)

iv: average number table: group 1 (odd odor group)

The intensity score for each sample group was entered as a dependent variable for two-way analysis of variance (ANOVA). Each analysis has the same two factors: 1) "Observation", having 15 grades, corresponding to each group of panelists rating, 2) "sample", having 5 grades, corresponding to samples a-c in the respective sample mixture groups.

Fig. 5 shows a graph of the mean values of the intensity of the mixtures in group 1. In this figure, the bars labeled with different letters (e.g., A, B, or AB versus C, but not a versus AB) are significantly different. The ANOVA model was found to significantly predict changes in the dataset (F13.4, df (model) 18, p < 0.01). Type I SS analysis revealed a significant major impact of observation and sample factors, revealing relevant but consistent differences between the scale of use of the samples and individual panelists.

v: type I Square sum analysis (group 1)

Multiple comparisons post hoc revealed significant differences between samples at three levels (samples in the far right column that do not share the same group are significantly different, p < 0.05):

vi post hoc Duncan analysis (group 1)

Conclusion ANOVA (group 1): the ramiflorin and eugenol are active, i.e. elastic, within the definitions indicated above.

ANOVA, group 2 (even group)：

Fig. 6 shows a graph of the mean values of the intensity of the mixtures in group 2. In this figure, the bars labeled with different letters (e.g., A, B, or AB versus C, but not a versus AB) are significantly different. The ANOVA model was found to significantly predict changes in the dataset (F13.4, df (model) 18, p < 0.01). Type I SS analysis (lower page) revealed a significant major impact of observation and sample factors, revealing relevant but consistent differences between the observer and sample.

vii: type I Square sum analysis (group 2)

Post hoc multiple comparisons (Duncan method) revealed significant differences between samples at four levels (samples in the far right column that do not share the same group are significantly different, p < 0.05):

viii: post hoc Duncan analysis (group 2)

Conclusion (ANOVA group 2): both raspberry ketone and bitter orange leaf oil are active, i.e. elastic, within the definitions shown above.

Based on the results of two ANOVA, the following principle was demonstrated: in the presence of both active ingredients, the resulting mixture was significantly stronger than the baseline mixture. Both active mixtures were consistently demonstrated to be significantly stronger than the baseline mixture.

By the present invention, the elastic properties of an unknown material can be tested by substituting the known active in the mixture with other non-elastic materials of different odor properties, all present at a threshold concentration. If the substitution results in a significant increase in odor intensity of greater than one unit (on a standard benzyl acetate scale) relative to a mixture of 5 inactive materials, the unknown material may be designated as an elastic material according to the definition shown above.

Perfume formulations

The above method can be used not only for testing ingredients but also for testing fragrances. By "perfume" is meant a balanced blend of materials that exhibit uniform (if multi-faceted) odor characteristics. There are various odor mixtures used as single ingredients, such as natural oils; these have a combined odor character theme, although consisting of individual ingredients covering a range of different odor characters. Commercial perfumes also often have a clear odor theme in the sense that they can be placed in a "perfume pedigree" and discussed with respect to their history and practice as they evolve therefrom. It is common to discuss fragrances in the following areas, such as: sweet direction and flower and fruit fragrance; or fresh, spicy, musk, etc. The odor is more complex and has multiple bodies, but the odor character also tends to build with a uniform scale. If a perfume has too many facets of odor of the same significance, it will lose the intuition of the consumer value of the perfume. The problem is therefore what happens if the perfume is treated as a perfume ingredient.

Commercially relevant perfumes tend to show reasonable uniformity between odor profiles just above threshold and those at higher concentrations. Therefore, they can be treated as if they were a component such as essential oil, and observed whether it can be used as an elastic material.

Fragrances are not considered to be a complex combination of ten ingredients, but rather as a single scent having multiple faces. The brief exposure is sufficient to allow sufficient information about the scent characteristics to be received so that the subject can make a useful comparison between the fragrances at some time after the first perception. The initial exposure may be enhanced by deeper examination and introspection of the perceptual properties to break down the entire event into potential perceptual components. This process is similar to sensing purple and then evaluating the relative amounts of red and blue that make up it. The ability to resolve color analytically absolutely does not detract from the ability to perceive the blend in a single perceptual form.

Perfume behavior: measurement of fragrance elasticity

The elastic material can be identified using the procedure outlined above. This protocol is useful because it uses materials that are incorporated into the mixture at their threshold concentrations. The resulting perfume itself can be evaluated using its threshold concentration, as can be done for essential oil ingredients. Thus, a perfume may be incorporated into a test mixture at a threshold concentration.

Any problems associated with detecting the smallest component at a concentration below the concentration of the dominant olfactory note of the fragrance can be minimized by using a descending concentration series of measurement thresholds. For example, the test subject starts with a concentration above the threshold and evaluates successive dilutions until the perfume character is no longer detected. The last concentration at which the target odor property was perceived was recorded as the threshold for this evaluation. The subject should take care to avoid adaptation to the smell by using short sniffing, 2 seconds should be sufficient, and rest often. The subject may confirm the threshold by repeating the process for some samples approaching the threshold. A coincidence threshold is then calculated as the concentration at which 50% detection rate can be achieved. The perfume diluted to a consistent threshold is then used in the test for new actives as for other perfume ingredients.

The method is then similar to the method used above for testing new components.

Experimental section 2：

Evaluation protocol

The panel is identical to experimental part 1 and the concentration of the sample is assessed based on the same 8-point scale only and using a standard dilution of benzyl acetate as a reference.

Sample preparation

The sample consisted of 10mL of the mixture solution, placed in a 100mL amber powder jar, capped and equilibrated for 2+ hours, as described in experimental section 1.

Experimental sample

Four experimental samples were prepared: t, u, v and w, consisting of:

(t) the baseline mixture (t) was made of only 5 known inactive ingredients, each selected from a different non-adjacent odor group.

(u) form (u) of the base mixture was prepared in the case where one inactive ingredient was substituted with the known active ingredient from the same odor group (delta-damascone), resulting in a mixture of 4 inactive ingredients and 1 active.

(v) And (w) a mixture u is formed based on the third (v) and fourth (w), wherein the second inactive ingredient is substituted by one of two model perfumes: model 5, aesthetically pleasing consistent with the predominantly powdery sweet character, enhanced by the grass note, and model R1, developed by model 5 and adapted to fit the formulation rules of the synergistic odor as described above.

The 4 samples obtained are described in table ix below.

ix: formulation of mixtures t, u, v and w

Sensory results

One-way, intra-subject ANOVA was performed on the data. Fig. 7 shows a graph of the mean values of the intensities of the mixtures t, u, v and x, with error bars representing the 95% confidence intervals of the mean values. The significant major effects (F23.95, df 3, p <0.05) showed significant differences between the sample averages. Post hoc average comparisons of the Duncan method show that all sample intensity averages differ significantly from each other (p < 0.05). Mixture w (made from model R1) is the best performing sample and is significantly stronger than v (made from model 5, a variant of the same perfume).

x: post hoc Duncan analysis

Discussion and conclusions

This experiment shows that mixture w is significantly stronger than all other mixtures, and is stronger than mixture u by more than 1 unit, and stronger than mixture t by more than 2 units. This is true despite the fact that the concentration of model R1 fragrance incorporated into the mixture was significantly lower than the concentration of model 5 (in mixture v). Both model fragrances share similar odor and base ingredients; however, model R1 has been adjusted to conform to the rules of elastic fragrance described above. The sensory results are consistent with model R1, which appears as an elastic component. Thus, perfumes falling within the above description have been shown as elastic perfumes within the above definition.

As the perfume which is incorporated into the test as a single ingredient has shown varying degrees of elasticity, resulting in a significant increase in overall strength. If these fragrances are essential oils, they are identified as elastic and inelastic components. As perfumes, they can be considered to share similar characteristics as the elastic component, and based on their performance in this test, the presence of both elastic and non-elastic perfumes has been identified. This can be used to form a fragrance that is acceptable and suitable for the intended purpose.

While the invention has been described above with reference to specific embodiments thereof, it is apparent that many changes, modifications, and variations can be made without departing from the inventive concept disclosed herein. Accordingly, it is intended to embrace all such changes, modifications, and variations that fall within the spirit and broad scope of the appended claims.

Claims (4)

1. A process for preparing a perfume composition comprising a candidate active ingredient, the process comprising the steps of:

a. selecting a first inactive component in a first mixture that most closely resembles the odor profile of the candidate active component;

b. selecting a second inactive component in the first mixture that is least similar in odor character to the candidate active component;

c. preparing a second mixture, wherein the second mixture is the same as the first mixture except that the first inactive component is replaced by an equivalent strength concentration of the candidate active component and the second inactive component is replaced by a known active from the same odor class as the second inactive component, the odor class selected from the group consisting of: floral, aldehydic, citrus/fresh, green/water-like, herbal, woody/amber, powdery/musk, spicy, fruity-light, fruity-heavy;

d. evaluating the strength of the second mixture to determine whether the second mixture is significantly more intense than the first mixture, wherein if the second mixture is significantly more intense than the first mixture, the candidate active component is considered to have demonstrated elastic activity; and

e. Preparing a perfume composition comprising said candidate active ingredient.

2. The method of claim 1, wherein the second mixture has an intensity that is at least one intensity fraction unit greater than the first mixture.

3. A method of determining the level of elastic activity of a candidate active component, the method comprising the steps of:

a. selecting a first inactive component in the first mixture, the first inactive component having a most similar odor profile to the candidate active component;

b. selecting a second inactive component in the first mixture that is least similar in odor character to the candidate active component;

c. preparing a second mixture, wherein the second mixture is the same as the first mixture except that the first inactive component is replaced by an equivalent strength concentration of the candidate active component and the second inactive component is replaced by a known active from the same odor class as the second inactive component, the odor class selected from the group consisting of: floral, aldehydic, citrus/fresh, green/water-like, herbal, woody/amber, powdery/musk, spicy, fruity-light, fruity-heavy;

d. Evaluating the strength of the second mixture to determine whether the second mixture is significantly more intense than the first mixture, wherein if the second mixture is significantly more intense than the first mixture, the candidate active component is considered to have demonstrated elastic activity.

4. The method of claim 3, wherein the second mixture has an intensity that is at least one intensity fraction unit greater than the first mixture.

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