Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
  • C11B9/00—Essential oils; Perfumes

Definitions

• This invention relates to perfume compositions with enhanced sensory
• compositions including such perfume compositions, and methods of making and using such compositions.
• the invention includes perfumes created using materials capable of synergistic blending.
• Odor detection is effected through olfactory receptors which are located in neurons in the olfactory epithelium in the nasal cavity. The signals from these neurons pass on to the glomeruli in the olfactory bulb and onto the higher center of the brain for further interpretation.
• Each receptor neuron expresses a single class of olfactory receptor, and olfactory receptor neurons of such a single type are distributed across the olfactory epithelium. The output fibers from these scattered neurons converge together on a single glomerulus in the olfactory bulb.
• the features of the odorant molecule are first fragmented and detected by the odor receptors. Then similar features of different odor molecules reinforce each other at the different odor receptors, and at the olfactory bulb level. The whole is then re-integrated to provide the odor perception, which can be as simple as a single percept.
• the many odorous molecules emanating from a single flower can excite multiple neurons, whose signals recombine to produce a single olfactory experience which the observer can recognise as typical of the particular flower.
• a different flower may emit many of the same materials but the differences in levels and composition will be re-integrated to yield a different sensory percept that can be recognised as coming from the different flower.
• olfactory signals can drive critical behaviours.
• a moth can identify a flower which emits more than 60 materials of which 9 are detected by the olfactory system. These have been shown to behave as a single percept capable of driving flower-foraging behaviour.
• the encoding is organised through a population of glomerular coding units which are thought to combine the different features of the molecular stimulants into the singular percept (via a mechanism as yet unknown).
• odor mixtures are not always simple combinations of their components. This being said it is often possible for humans to perceive a complex odor mixture as a single whole, while also being able to decompose the experience into sensory sub-units. For example, when a malodor and perfume are mixed it is often possible to compartmentalise the experience such that the relative contributions of each odor type to the overall odor can be judged. So there exists a paradox: that the mix may be perceived as a single perceptual experience, while that experience may be subdivided on introspection.
• introspection may not reflect the relative intensities of the component stimuli, or even their odor character. Nevertheless the process can be sufficiently reproducible that it can be used to design new products which deliver useful benefits, e.g. deodorant perfumes.
• Synergy has been described as a higher level of sensory impact than one would expect based on the impacts of the unmixed components.
• One example is adding a subthreshold amount of one odorant causing a small but measurable increase in the perceived intensity of another (beverage) odor or in the perceived sweetness of supra-threshold sucrose. It has been thought that the addition of small amounts of one material can occasionally lead to significant increases in the intensity of an aroma or flavour.
• the present invention seeks to address at least some of the issues described above. Specifically to identify groups of odor ingredients that can be used to create synergistic odor or perfume compositions and the resulting perfume compositions therefrom.
• the present invention relates to perfumes created using materials capable of synergistic blending in odor or flavor mixtures.
• the invention further includes products formed by incorporating such perfumes.
• Figure 1 is a graph showing a threshold value approximation.
• Figure 2 is a bar graph showing the standardized intensity scores of Examples 1-
• Figure 3 is a bar graph showing the average intensity scores of Examples A-F.
• Figure 4 is a bar graph showing the average intensity scores of Examples G-O.
• Figure 5 is a bar graph showing odd-numbered odour groups.
• Figure 6 is a bar graph showing even numbered odour groups.
• Figure 7 is a graph showing the average sample intensity of fragrances.
• the present invention has surprisingly found that specific combinations of ingredients can be used to create synergistic effects where the sensory impact of ingredients in the mix, or of the mix as a whole, is greater than one would expect based on the impacts of the unmixed components. Further, the present invention relates to compositions that include the synergistic effects, as well as methods of using such compositions to achieve desired responses in users, such as humans.
• 'resilient' materials Those ingredients which are more prominent in the mix than expected are referred to herein as 'resilient' materials and, not to be limited by theory, certain components of perfume compositions have been found to be more resilient than others.
• the present invention identifies these resilient odor components, including how to identify such resilient odor components and determine threshold levels, and further outlines how they can be combined beneficially with other perfume components.
• Resilient materials may also combine their odor with other ingredients present to create a new and different odor character in the mixture.
• the perfume composition comprises components from specific groups.
• the groups, described below, are referred to as Group 1 A, Group IB, and 1C.
• Perfume compositions of the present invention may include one or more components from one, two or all three of Groups 1A, IB and 1C.
• the first component (Group 1A) is selected from the group consisting of: acetyl cedrene, Camphor powder synthetic, Cedarwood oil, cineole, cinnamic aldehyde (10), cistus labdanum, citral dimethyl acetal, Cosmone, Cyclal C, beta damascone (10), delta damascone (10), Ebanol (10), ethyl vanillin (10), eugenol, Galbanone (10), gamma undecalactone, heliotropin, hexyl cinnamic aldehyde, iso E Super, alpha iso methyl ionone, Mayol, methyl chavicol, methyl cinnamate, methyl ethyl 2 butyrate, Silvanone, Silvial, alpha terpineol, allyl hexanoate, Labienoxime (10), anisic aldehyde(lO), Black Pepper Oil, Polysantol(
• an individual component includes “(10)” it signifies a 10% solution of the named material in a solvent, preferably an odourless solvent, including by way of example: dipropyleneglycol.
• the second component (Group IB) is selected from the group consisting of alkyl alcohols, phenyl alkylalcohols, terpene hydrocarbons or mixtures thereof.
• the components of Group IB can be added as part of natural oils. Components of Group IB are described herein as "promoters”.
• Group IB components include: linalol, orange terpenes, phenyl propyl alcohol, phenyl ethyl alcohol, alpha terpineol, Mayol, Mefrosol, citronellol, tetrahydrogeraniol, tetrahydrolinalol, geraniol; and mixtures thereof.
• the components of Group IB have been found to further enhance the synergistic effect of the components of Group 1A.
• the third component may be selected from the group consisting of aldehyde C12 (10), anethole, Ambermax (10), isobornyl acetate, Calone 1951 (10), coumarin, cuminic aldehyde (10), Ginger oil, Oakmoss synthetic, Patchouli oil, undecavertol, Vetiver oil; and mixtures thereof.
• the materials from Group 1C can also be added as part of natural oils. Materials from Group 1C are optional in the composition.
• one or more components of one, two or three Groups may be used in the present invention.
• One or more components from Group 1 A is present in the composition in 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 1 A can be one, two, three, four or more than four. When present, one or more components from
• Group IB is present in the composition in amount 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%> of the composition or from about 15 % to about 25%>, or from about 10%> to about 20%> by weight of the composition.
• the number of individual components from Group IB, when included in the composition can be one, two, three, four or more than four.
• a component from Group 1C, when present, is present in the composition in amounts up to about 35%> of the composition or from about 18%> or less by weight of the composition.
• the number of individual components from Group 1C, when included in the composition can be one, two, three, four or more than four.
• one aspect of the present invention includes a combination of the aforementioned Groups 1A, IB, and 1C.
• a second aspect of the present invention includes materials that are limited in their use in the composition, or materials that are excluded. There are two groups of these materials in the present invention: Group 2A and Group 2B.
• Group 2A includes allyl cyclohexyl propionate, Bangalol, Bourgeonal, Cassis bases, ethyl methyl phenyl glycidate, ethylene brassylate, Florosa, Herboxane, cis 3 hexenyl methyl carbonate, Jasmatone, Lemonile, Lilial, methyl anthranilate, Methyl Laitone, phenyl ethyl phenylacetate, Rose oxide, styrallyl acetate, Traseolide, Ultravanil, Ylang oil and mixtures thereof.
• Group 2B includes isononyl acetate, linalyl acetate, and mixtures thereof.
• the materials in Group 2A or Group 2B are independently present in the composition at no more than aboutl .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).
• the materials of Group 2A when used independently from being present in a natural oil, may be present in an amount of from zero percent to about 1.0% or up to about 0.6% by weight of the perfume composition.
• the materials of Group 2B when used independently from being present in a natural oil, may be present in an amount of from zero percent to about 1.0% or up to about 0.6% by weight of the perfume composition.
• the total concentration of non-essential oil additions of materials from Groups 2A and 2B comprises less than 2% by weight of the total perfume composition, and more desirably less than about 1% by weight of the total perfume composition.
• the perfume compositions of the present invention are free of any materials from group 2A, and in some embodiments, the perfume compositions of the present invention are free of any materials from group 2B.
• the present invention has surprisingly found that specific combinations of ingredients can be used to create synergistic odor or perfume compositions. Not to be limited by theory, certain components of the perfume composition have been found to be more resilient than others.
• a resilient odor component is one that provides a character to the entire composition greater than would be expected to otherwise provide based on the odor properties of the single material.
• the present invention identifies resilient odor components which are more easily identified in mixes and their odor character becomes a clear component of the odor character of the mixture as a whole.
• Another benefit of the present invention is that the presence of resilient materials leads can lead to a new and different odor character being created in the mixture.
• the present invention is quite useful in that it achieves providing a stronger, or more complex, or unique perfume while avoiding the need for adding more ingredients in the composition. For example, a resilient component may give a higher perceived intensity while using less of that resilient component in the perfume composition.
• odor character contribution of a second group of materials is reduced on mixing with more resilient materials.
• these non-resilient materials may be masked altogether. Therefore the amounts of the non-resilient materials, such as those listed in Groups 2A and 2B, in the compositions should be limited in the levels described above, if used at all.
• Resilient components, such as those in Group 1 A should be present in a significantly higher amount than components in Group 2 A and/or in Group 2B.
• the aforementioned aspect of the invention includes perfume compositions including one or more component selected from at least one of Groups 1A, IB and 1C in combination with a component from one or more of Groups 2 A and 2B.
• a third group of materials tend to be present when resilient materials and/or mixes containing them are enhanced, but do not generally demonstrate such a prominent olfactory contribution themselves.
• These are the Group IB promoters. Many of the Group IB promoters are alcohols, which are general blending materials. This invention has surprisingly found that the Group IB materials promote the contribution of the resilient material in the perfume composition.
• the Group IB promoters increase the intensity of the resilient component(s).
• Group IB promoters will increase the intensity of the Group 1 A material(s) without the odor of the Group IB promoter coming through prominently.
• the Group IB promoters are optionally included in the perfumes of the present invention.
• a threshold concentration of an odor component is the minimum concentration at which the odor is perceived.
• Threshold concentration can be considered as a standard level for creating iso-intense concentrations, which can be identified relatively unambiguously for all materials. If no interactions were to take place between the iso-intense components of a mixture, then each material would be perceived equally. If some materials became more olfactorily prominent, and/or intense, then it is judged that their odor has been enhanced by the presence of the other materials. Thus forming mixtures with iso-intense materials gives a useful approach to identify when and how enhancement may take place within a mixture or for the mixture as a whole. At threshold levels of perception of the odor component such enhancement is more easily identified.
• a useful solvent for making liquid phase samples at threshold concentration is dipropylene glycol (dpg).
• concentration of perfumery material is generally so small in such compositions that physical effects between materials at threshold will be very small, and the main effects will be sensory.
• the present invention includes perfume compositions that include components that are consistently perceived at intensities above threshold in mixtures, while their concentration remains at threshold concentration level. Thus, the intensity of the odor of one or more components is increased through the present invention, even though the actual amount of the one or more components is at the threshold concentration level.
• Trivial additions include adding materials of the same odor facet to achieve a greater odor. For example, it is possible to combine materials at or below threshold concentration such that in combination they produce an odor above threshold perception level. This can be achieved by combining only materials which each act partially or totally at the same receptor(s). Such groups of materials will usually be identifiable in that they have similar odors or shared odor facets. For example, combining sub-threshold amounts of different rose-smelling materials may produce a suprathreshold mixture with a rose odor. However, this alone is not the mechanism of the present invention.
• the resilient odor components in the compositions of the present invention produce enhanced effects and odor intensity benefits. This can be achieved without the simultaneous presence of other materials with shared odor characteristics. Of course, the present invention does not exclude their use with such materials.
• the approach of blending materials only having similar odor characteristics is described above by way of example to differentiate the alternative approach to 'apparent enhancement', which is based on trivial additive effects.
• a second component may be added.
• Added second component materials may not play such a prominent olfactory role themselves in the overall odor profile of the mixture. They may not be perceived as among the most intense components, however neither do they strongly dilute or detract from the intensity performance of mixtures containing resilient materials. It has been surprisingly found that the combination of resilient odor components with a second component produces mixtures with useful, enhanced performance (e.g., higher perceived intensity of the mix with the resilient odor component).
• the perfume or fragrance compositions according to the present invention can be used in a variety of products.
• the term "product” shall refer to products including perfume compositions described above, and includes consumer products, medicinal products, and the like. Such products can take 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 lie in a range from 0.05% (as for example in low odor skin creams) to 30% (as for example in fine fragrances) by weight thereof.
• the incorporation of perfume composition into products of these types is known, and existing techniques may be used for incorporating perfumes for this invention.
• various methods to incorporate perfume compositions into a product include mixing the perfume composition directly into or onto a product, but another possibility is to absorb the perfume composition on a carrier material and then admix the perfume-plus-carrier mixture into the product.
• the present invention includes perfume compositions and products including such perfume compositions, as well as methods of using such perfume compositions and products.
• the methods of use include providing a perfume composition or product as described herein to a human and allowing the human to smell the resulting odor to achieve a desired effect.
• the desired effect may include, for example, providing to a user (such as a human) emotional benefits, cognitive benefits, and/or improved interactions with perceptions in other modalities.
• the present invention also includes a method to evaluate certain perfumes/odors and determining the threshold concentration for a perfume or flavour that can be used to identify the benefits of the invention.
• the evaluation may then be used to produce a perfume composition (or product including the perfume composition) with the desired threshold amount of the fragrance desired.
• a method of determining a threshold amount of a fragrance, and preparing a perfume composition using the results of the evaluation may further include forming a product with the perfume composition.
• the method includes use of a solvent.
• the solvent in the examples is dipropylene glycol, sometimes referred to here as dpg, though other low odor or odourless solvents may be used.
• the threshold in dpg of each ingredient was first determined and then each ingredient was incorporated into the perfume at that level.
• Perfumes were also created with all the ingredients present at approximately 0.3 times threshold, and another set with all ingredients present at 0.1 times threshold concentration. For illustration the experiments below were carried out using a 10ml aliquot of perfume in 125ml brown glass jars.
• One suitable method for ascertaining the detection and/or recognition threshold of each odor ingredient from a liquid solution is derived from the Method of Limits (which is described in the ASTM "Manual on Sensory Testing Methods', STP 434 (1968),
• y is the percentage detection rate
• x is the logio of the percentage concentration of the ingredient in dipropylene glycol
• k is the constant determining the gradient of the sigmoid function
• threshold is the concentration value at the inflection point of the sigmoid curve (and also therefore, the concentration at the 50% detection rate).
• k and threshold were approximated, then fitted using the solver add-in module of Microsoft XL 2007 such that root mean squared error (RMSE) between the observed and predicted points was minimised.
• RMSE root mean squared error
• the resultant RMSEs for all fit lines were below 10% and deemed acceptable.
• Fig. 1 shows a threshold value approximate for one sample perfume ingredient.
• a team of male and female assessors are used in the evaluation of sample intensity.
• the assessors were between the age of 25 and 65 years old. They were selected for evaluations on the basis of their ability to correctly rank the odour intensities of a series of dilutions (in dpg) of perfume ingredients.
• the standard perfume ingredient used in odour assessment sessions was benzyl acetate, prepared in a series of dilutions listed in the table below. Each dilution was associated with an odour intensity score. Other materials could be used in a similar fashion.
• Standard dilutions as above were present during evaluations and provided for reference to assist assessors in the evaluations.
• the examples tested were prepared as described herein.
• the examples consisted of dilutions in dpg of mixtures of materials, at or above their individual threshold concentrations.
• approximately lOg of each solution was placed in a capped 125ml jar and allowed to equilibrate for a minimum of 2 hours at room temperature.
• Assessments were made by assessors removing the cap and smelling the contents. Jars were assessed in random order. Assessors assigned a score between 0 and 8 to each sample, with 0 corresponding to no odour and 8 representing very intense odour. After that, at least 15 assessments were obtained for each sample.
• assessments for a sample are carried out over several sessions and/or with different subjects, it is possible to facilitate comparisons between samples by normalising the results for each sample across sessions and assessors. This may occur, for example, when too many samples are available for the assessor to be reliably assessed in one session.
• the data for Examples 1 to 12 was analysed in this fashion, as described below.
• Assessors were presented with a segment of the samples in a series of sessions, in order to reduce the fatigue and inconsistency of assessment associated with a large number of samples.
• Each assessor's scores were standardised as follows: for each assessor, the mean of all the individual's scores within the session was calculated
• each of the assessor' s data points was converted to a standardised score, that is, the i th score for each assessor (x t ) was recalculated into (x s td,i) as follows:
• Each Example was prepared by adding the target quantity of each stock solution to a vial and making up to a total of 20. Og. Each mixture was then agitated and left to equilibrate. Each was used as-is, and was further diluted by a factor of 3/10 and 1/10, to produce the sub-threshold mixes. In this way, each mixture was prepared at 3 concentrations: (1) with each component at threshold concentration, (2) with each component at 0.3 threshold concentration and, (3) with each component at 0.1 threshold concentration.
• METHYL DIHYDROJASMONATE cyclopentaneacetic acid, 3-oxo-2-pentyl-, Hedione methyl ester
• Geranium oil 0.0003% 0.0003%
• EXAMPLE 1 141.5 ⁇ . of a cis-3-hexenol solution at 0.10% in dpg, 50.7 ⁇ _ of a cedarwood oil solution at 5.00% in dpg, ⁇ . ⁇ ⁇ . of a Methyl Diantilis solution at 9.93% in dpg, 44.6 ⁇ of an Ethyl Safranate solution at 1.00% in dpg, and 18.4 ⁇ . of a citronellol solution at 3.34% in dpg, were added to 19.74mL of dpg and mixed.
• EXAMPLE 2 18.4 ⁇ . of a linalol solution at 3.50% in dpg, 15.1 ⁇ . of an Ebanol solution at 0.98% in dpg, 18.9 ⁇ . of a methyl cinnamate solution at 7.32% in dpg, 18.9 ⁇ . of a benzyl acetate solution at 7.01% in dpg, and 18.4 ⁇ . of a citronellol solution at 3.34% in dpg, were added to 19.91mL of dpg and mixed.
• EXAMPLE 3 189.3 ⁇ . of a citral dimethyl acetal solution at 3.25% in dpg, 8.9 ⁇ . of a methyl chavicol solution at 5.00%> in dpg, 20 ⁇ . of a nutmeg oil solution at 1.50% in dpg, and 6.9 ⁇ of a Manzanate solution at 0.01% in dpg, were added to 19.77mL of dpg and mixed.
• EXAMPLE 4 195.5 ⁇ . of a terpineol alpha solution at 2.10% in dpg, 18.2 ⁇ . of a dihydromyrcenol solution at 1.15% in dpg, 19.5 ⁇ . of a eugenol solution at 1.00% in dpg, 6.9 ⁇ of a ethyl methyl-2-butyrate solution at 0.05% in dpg, and 88.7 ⁇ . of a phenyl ethyl alcohol solution at 0.50% in dpg, were added to 19.67mL of dpg and mixed.
• EXAMPLE 5 18.4 ⁇ of a linalol solution at 3.50% in dpg, 8.9 ⁇ of a cineole solution at 0.04%) in dpg, 9.9 ⁇ . of a Cashmeran solution at 5.21% in dpg, and 9.2 ⁇ . of a damascone delta solution at 0.55% in dpg, were added to 19.95mL of dpg and mixed.
• EXAMPLE 6 5 ⁇ . of a Cyclal C solution at 1.01% in dpg, 15. of a cistus labdnaum oil solution at 4.99% in dpg, 13.8 ⁇ . of a methyl cinnamate solution at 10.00%) in dpg, 6.9 ⁇ of a Manzanate solution at 0.01% in dpg, and 126.2 ⁇ L of a geranium oil solution at 0.05% in dpg, were added to 19.83mL of dpg and mixed. Examples 7-12. Fragrances not conforming to the selection rules for the invention.
• Methyl Laitone 2a 0.00003% 0.00003%
• total 2a count (% in fragrance oil) 2 (7.96%) 1 (32.28%) 3 (93.53%) total 2b: count (% in fragrance oil) 1 (90.01%) 1 (46.82%)
• Geranium oil 0.00032% 0.00032%
• Methyl Dihydrojasmonate 0.0020% 0.0020%
• Methyl Laitone 2a 0.00003% 0.00003%
• total lc count (% in fragrance oil) 1 (14.52%) total 2a: count (% in fragrance oil) 2 (67.51%) 1 (15.17%) 2 (20.05%) total 2b: count (% in fragrance oil) 2 (40.97%)
• EXAMPLE 7 ⁇ . of a para-cresyl methyl ether solution at 0.02% in dpg, 19.2 ⁇ . of an isononyl acetate solution at 13.1 1% in dpg, 20 ⁇ . of a Methyl Laitone solution at 0.0010% in dpg, 18.2 ⁇ . of an ethyl methyl phenyl glycidate solution at 1.20% in dpg, and 66.3 ⁇ . of an indole solution at 0.05% in dpg, were added to 19.87mL of dpg and mixed.
• EXAMPLE 8 17 ⁇ of a Cyclamen Aldehyde solution at 0.12% in dpg, 19.2 ⁇ . of an isononyl acetate solution at 13.1 1%) in dpg, 18.2 ⁇ . of a Coumarin solution at 0.42% in dpg, 18.3 ⁇ . of an allyl cyclohexyl propionate solution at 9.49% in dpg, and 103 ⁇ . of a Mefrosol solution at 1.00% in dpg, were added to 19.82mL of dpg and mixed.
• EXAMPLE 9 17.8 ⁇ . of a Florosa solution at 0.00012% in dpg, 141.5 ⁇ . of a cis-3- hexenyl methyl carbonate solution at 0.00071%) in dpg, 19.4 ⁇ . of a patchouli oil solution at 0.00053%) in dpg, and 186.9 ⁇ of a phenyl ethyl phenyl acetate solution at 0.0075%) in dpg, were added to 19.63mL of dpg and mixed.
• EXAMPLE 10 ⁇ . ⁇ ⁇ . of a Galbanone solution at 1.02%> in dpg, ⁇ . ⁇ ⁇ . of a vetyver oil solution at 2.48% in dpg, 19.5 ⁇ . of a eugenol solution at 1.00%> in dpg, and 17.7 ⁇ . of a Methyl Anthranilate solution at 1.21% in dpg, were added to 19.93mL of dpg and mixed.
• EXAMPLE 1 1 183.3 ⁇ . of a linalyl acetate solution at 0.01 1% in dpg, l9.2 ⁇ L ⁇ of an isononyl acetate solution at 0.013%) in dpg, 18.5 ⁇ . of an ethyl vanillin solution at 0.0025%) in dpg, 18.3 ⁇ . of an allyl cyclohexyl propionate solution at 0.0087%) in dpg, and 126.2 ⁇ . of a geranium oil solution at 0.00032%) in dpg, were added to 19.63mL of dpg and mixed.
• EXAMPLE 12 17.8 ⁇ . of a Florosa solution at 0.14% in dpg, 22 ⁇ , of an Isobornyl Acetate solution at 5.00% in dpg, 18.5 ⁇ . of an ethyl vanillin solution at 2.68% in dpg, 29.7 ⁇ . of a phenyl ethyl phenyl acetate solution at 5.04%> in dpg, were added to 19.91mL of dpg and mixed.
• Fig. 2 shows the means and 95% confidence intervals for the standardised scores of the examples; note that examples 1-6 are shown to confidently score >0 whereas examples 7-12 have negative means.
• the examples A to O illustrate the benefits of the present invention: that a mixture according to the present invention will smell stronger when presented at threshold concentration than a similar mixture using materials that are with less-active or not active according to the present invention.
• the components that are less active or not active are labelled "Inactive”.
• the components that are part of the present invention are labelled "Resilient or Active”.
• the combination of group la materials and group lb materials (or similar alkyl alcohols), all present at threshold concentration can deliver a sensory boost in its intensity.
• the average or mean scores of Examples A-0 are shown in Figures 3 and 4. The black bars indicate a 95% confidence interval.
• Methyl Benzoate la ⁇ 0.006 07% 0.00597% 0.00599%
• Methyl Benzoate la ⁇ 0.006 07% 0.00605% 0.00594%
• Methyl Benzoate la ⁇ 0.006 07% 0.06071% 0.06055%
• Methyl Benzoate la ⁇ 0.006 07% 0.00607% 0.00607%
• fragrance oil ⁇ 1 (43.39%) 3 (60.22%) 3 (50.67°/ >) total lb: count (% in
• fragrance oil ⁇ 0 (1.47%) 1 (39.45%) 3 (49.05°/ >) total lc: count (% in
• fragrance oil ⁇ 3 (0.00%) 3 (78.21%) total lb: count (% in
• fragrance oil ⁇ 1 (23.08%) 1 (8.34%) total lc: count (% in
• fragrance oil ⁇ 2 (29.96%) 2 (2.26%) 2 (1.52%) total 2a: count (% in
• Perfumes created according to the present invention displayed higher odor intensities, and in some aspects significantly higher odor intensities, than comparative perfumes using the test method described above. For demonstration purposes, care was taken that the perfumes did not contain materials whose main odor character was shared with other materials in the perfume. This effectively minimised (or excluded) additive effects caused by two similar odors at or around threshold exciting the same receptors and thus resulting in an above -thresh old activity level at that receptor. Thus the perfumes of the invention are shown to have a higher intensity, which arises from a synergistic interplay between the ingredients. It has been traditionally understood that such phenomena are rare.
• the present invention allows for the formulation of perfumes with internal synergy in a reliable, repeatable fashion.
• the present invention provides a method for formulating such perfumes, and further, the perfumes themselves cover a wide odor range and offer benefits.
• Perfume is often one of the more expensive components of consumer products, so any such broadly-applicable increase in intensity is valuable to the formulator.
• the new test material should replace one of the non-active materials in the appropriate test mixture, preferably replacing the non-active most similar in odour character to the test material.
• the present inventors have found that the Quick Test works most effectively when two actives are present in the mixture. This approach regularly achieves a significant increase in intensity compared to the mix with no actives present.
• the standard active is a material which will be incorporated into the test mix along with the test material, both at threshold concentration. Together the two substitutions should result in a mixture with significantly higher intensity than the original mix with no actives present.
• the two 'standard' actives have different odours and fall into different odour classes. They are listed below in the Experimental Section.
• the present invention includes a method for identifying and selecting new actives whereby the candidate material delivers enhanced intensity (greater or equal to one unit on the standard scale described herein) when it is substituted for an inactive material in one of the two test mixtures described for this purpose, with or without a second inactive material being substituted with a known active.
• Preferred actives and inactives are described in the specification.
• the invention includes preparing a perfume composition using the substituted inactive material, or inactive materials. The first stage of the test is to identify into which class the test material falls and select the mix of inactives with a class most similar to this. The unknown will be substituted for the non-resilient material from the same odour group. This mixture will be used as the basis of the further investigation.
• non-resilient material judged to be most different in odour from the unknown should be selected.
• This non- resilient material will be substituted with a resilient from the same odour class. Examples of resilient materials for each odour class are given in the text above
• the invention includes the quick test method.
• the method may be used for identifying and selecting new actives whereby the candidate material delivers enhanced intensity (e.g., greater or equal to one unit on the standard scale described herein) when it is substituted for an inactive material in one of the two test mixtures described for this purpose. This may be performed with or without a second inactive material being substituted with a known active. Preferred actives and inactives are described above.
• a method may include the following process. First, the user identifies and considers each of the inactive components in two test mixtures. In step 1, an inactive component is selected which is most similar in odour character to the candidate material. This identified component is known as the "most similar" inactive. This is will identify which of the two test mixtures will be used in the following steps. The next step (step 2) is to identify which inactive material in the test mixture selected from step 1 is most different from the candidate material. Identification of the most different inactive material is optional, however, it is preferred to identify this component so as to maximise the difference. The identified "most different" material will be replaced by a known active from the same odour class.
• the third step is to reformulate the selected test mixture by replacing at least one, and desirably both of the two inactives (the most similar inactive and the most different inactive) identified in steps 1 & 2 above.
• the most similar inactive the most similar inactive
• step 1 (identified from step 1) may be removed and replaced with iso-intense concentrations of the candidate material and the most dissimilar material may be removed and replaced with an iso-intense concentration of the known active from step 2. Examples of suitable concentrations for actives are described above.
• the threshold concentration of the candidate material can be found using the method described above.
• step four the intensity of the new mixture from step 3 may be assessed using the preferred method described in the paragraph below. If the new mixture is a mixture of the new mixture from step 3
• the candidate material is considered to have demonstrated resilient activity.
• This conclusion may be used to develop a perfume composition including the candidate material. Therefore, it may be useful to use the present method to develop a modified perfume composition whereby at least one component has been substituted, for example, an active component substituted for an inactive component or vice versa.
• the intensity of the new mix, with the new test material and a standard active incorporated, should be assessed versus the intensity of the related mixture of five inactive materials. It is preferred to use the intensity scale employed in the experimental section below. This is a sensory scale where sensory scores are illustrated by standard concentrations of benzyl acetate in dipropylene glycol. If the new mixture is significantly more intense than the blend of inactives (e.g. by more than 1 unit using this scale) then the new test material may be considered to be demonstrating 'resilient' activity. A composition including the resilient material can then be prepared.
• Assessors were presented with a segment of the samples in a series of sessions, in order to reduce the fatigue and inconsistency of assessment associated with a large number of samples. Order of sample presentation was from presumed weakest intensity to presumed strongest intensity, to minimise carry-over from intense samples. Baseline mixtures were presented first, and all other test mixtures were randomised thereafter.
• the Set 1 samples were made from odd-numbered odour groups only; Set 2 samples were made from even-numbered odour groups only. This precaution ensured that all samples were made from ingredients selected from non-adjacent odour groups and thus minimised any overlap in odour character between the inactive components in each mix. All ingredients were incorporated at their estimated threshold concentration in dpg, using the method described above. Each set consisted of 5 samples:
• This second, "b” mixture formed the basis of a third mix (c), where a second inactive ingredient was substituted with a known-active ingredient, resulting in a mix of 3 inactive and 2 active ingredients (eg mix lc contains an active material from groups 7 & 9, 7act and 9act, in the table overleaf).
• the intensity scores for each sample set were entered as the dependent variable of two-way analyses of variance (ANOVA). Each analysis had the same two factors: 1) "observation”, with 15 levels, corresponding to each set of panellist ratings and 2) "sample”, with 5 levels, corresponding to samples a-c in the corresponding set of sample mixtures.
• Figure 5 shows a means plot of intensities for mixes in Set 1.
• bars labelled with differing letters e.g., A, B or AB vs. C, but not A vs. AB
• Type I SS analysis reveals significant main effects for observation and sample factors, revealing pertinent but consistent differences between samples as well as the individual panellist's use-of-scale.
• Set 1 Sums-of-Squares analysis
• an unknown material can be tested for Resilient character by substitution along with a known active in a mix with other non-resilient materials of different odour character, all materials present at threshold concentration. If the substitutions result in a significant increase in odour intensity of greater than one unit on the standard benzyl acetate scale relative to a mix of 5 non-active materials then the unknown material can be assigned as a Resilient material by the definition set forth above.
• perfume it is meant a balanced blend of materials that demonstrates a homogenous, if multi-faceted, odour character.
• odorant mixes which are used as single ingredients, for example the natural oils; these have a combined odour character theme despite being composed of individual ingredients which cover a range of different odour characters.
• Commercial perfumes also frequently have a clear odour theme, to the extent that they can be placed into 'genealogies of perfume' and discussed relative to the history and practices from which they evolved. It would not be unusual to discuss a perfume in terms such as: sweet, floral fruity; or fresh, spicy, musk, and so on.
• perfumes tend to show reasonable uniformity between the odour character just above threshold and that at higher concentrations. As a result, it is possible to treat them as though they were an ingredient such as an essential oil, and to see whether they might act as a resilient material, or not.
• the perfume is perceived not as a complex combination of tens of ingredients but as a single odour with a variety of facets.
• a brief exposure is sufficient to allow enough information to be received about the odour character for the subject to be able to make useful comparisons between perfumes some time after first perceived.
• the initial exposure can be augmented by a deeper examination and introspection of the perceived character to decompose the overall event into potential sensory components. This process is akin to perceiving purple colour, then assessing the relative levels of red and blue from which it is composed. The ability to dissect the colour analytically in no way detracts from the ability to perceive the blend as a single percept.
• Perfume Behaviour Measuring the Resilience of a Perfume
• Resilient materials can be identified using the procedures outlined above. That procedure is useful in that it uses materials incorporated in mixes at their threshold concentration. The resulting perfumes themselves may be assessed using their threshold concentration, as would be done for an essential oil ingredient. The perfumes can therefore be incorporated into the test mixtures at threshold concentration.
• any issues associated with detecting minor components at a lower concentration than that of the main olfactory note of the perfume may be minimised by using a descending concentration series to measure the threshold.
• the test subject starts at a concentration above threshold and assesses successive dilutions until the perfume character is no longer detected. The last concentration at which the target odour character was perceived is recorded as the threshold for that assessment.
• the subject should take care to avoid becoming adapted to the odour by using short sniffs, 2 seconds should be enough, and frequent rests.
• the subject can confirm the threshold by repeating the process for a few samples close to the threshold.
• the consensus threshold is then calculated as that concentration where a 50% detection rate would be achieved. Perfumes diluted to the consensus threshold were then used in the Test for New Actives as for other perfume ingredients.
• the panel was equivalent to that in Experimental Section 1, and assessed the samples for intensity only, based on the same 8-point scale and using the standard dilutions of Benzyl Acetate for reference.
• Sample Preparation Samples consisted of lOmL of mixture solution, presented in lOOmL amber powder jars, lidded and equilibrated for 2+ hours, as described in Experimental Section 1.
• t Four experimental samples were made; t, u, v and w, which consisted of the following: (t) A baseline mixture (t) made solely of 5 known-inactive ingredients, each selected from different, non-adjacent odour groups.
• Figure 7 shows a means plot of intensities for mixes t, u, v and x, with error bars representing the 95% confidence interval of the mean.
• Post-hoc mean comparisons by Duncan method showed that all sample intensity means were significantly different from each other (p ⁇ 0.05).
• Mixture w made with model Rl
• v made from model 5, a variant of the same perfume.

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