Vanilla fragrance type composition as well as preparation method and application thereof

Abstract

The invention discloses a vanilla fragrance type composition as well as a preparation method and application thereof. The composition is prepared from strong vanillin, ethyl vanillin, vanillin isobutyrate, menthyl acetate and a solvent, the vanillin which is listed as an allergen component is replaced by matching of the strong vanillin, the ethyl vanillin, the vanillin isobutyrate and the menthyl acetate, so that a relatively safe vanillin base is provided; meanwhile, when being applied to a product containing volatile and flavor-changing spices to test high-temperature stability, for example, when being applied to a hot-filling cosmetic machine type needing long-time heating, the essence is proved to be capable of prolonging the diffusion time of the fragrance and is beneficial to improving the temperature resistance of the spices; besides, the vanilla fragrance type composition is subjected to an illumination stability test, and it is proved that the vanilla fragrance type composition further has illumination stability and can be used for preparing essence and cosmetics.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of daily chemical products, in particular to a vanilla fragrance type composition, a preparation method and application thereof. BACKGROUND

[0002] Cosmetics refer to chemical industrial products or fine chemical products which are spread on any part of human body surface such as skin, hair, hands and feet nails, lips and teeth by means of smearing, spraying and the like, so as to achieve the purpose of cleaning, maintaining, beautifying, modifying and changing appearance, or correcting body odor, and keeping good state. Fragrance refers to a mixture of various fragrances, which has a certain fragrance type and can be applied to multiple fields such as cosmetics, food, daily necessities and the like. Vanilla bean, also known as vanilla, is mainly produced in Indonesia, Madagascar and other places with warm and humid climate, and is widely used in baking, chocolate, tobacco, high-grade perfume and cosmetics. The main volatile components of vanilla include vanillin, guaiacol, 2-pentadecyl-1, 3-dioxolane, 2, 3-butanediol, acetic acid, furfural and the like. Traditional vanilla fragrance mainly adds vanillin to complete the blending, but as vanillin is listed as an allergen ingredient that needs to be marked in some regions or countries, it is urgent to develop a new vanilla fragrance type composition to meet the application demand of safer fragrance in the market. SUMMARY

[0003] The purpose of the present application is to overcome one or more deficiencies in the prior art, provide a new vanilla fragrance type composition capable of simulating the odor of natural vanilla bean, and also help to improve the stability of other fragrances (such as light resistance, temperature resistance and the like).

[0004] The present application also provides a preparation method of the above-mentioned vanilla fragrance type composition and application thereof in preparing fragrance and cosmetics.

[0005] To achieve the above-mentioned purpose, one technical solution adopted by the present application is as follows:

[0006] A vanilla fragrance type composition, comprising vanillin, ethyl vanillin, vanillin isobutyrate, menthyl acetate and a solvent; wherein the mass ratio of vanillin, ethyl vanillin, vanillin isobutyrate and menthyl acetate is 1:1.5-3:1.5-3.5:0.1-1.0; and the content of vanillin in the composition is less than or equal to 6% in terms of mass percentage.

[0007] In some embodiments of the present application, the composition comprises vanillin 0.5%-6%, ethyl vanillin 4%-9%, vanillin isobutyrate 5%-15% and menthyl acetate 0.1%-4% in terms of mass percentage.

[0008] Further, the composition comprises, in mass percentage: vanillin 2%-4%, ethyl vanillin 6%-8%, vanillin isobutyrate 7.5%-9.5%, menthyl acetate 1%-2%.

[0009] According to some preferred and specific aspects of the present application, the mass ratio of the vanillin, the ethyl vanillin, the vanillin isobutyrate and the menthyl acetate is 1:1.8-2.8:2.5-3.0:0.3-0.8.

[0010] In some embodiments of the present application, the solvent includes but is not limited to a combination of one or more selected from dipropylene glycol (DPG), glyceryl triacetate (TA), octodecanol (ODO), ethanol, isopropyl myristate (IPM), triethyl citrate (TEC).

[0011] The present application provides still another technical solution: a preparation method of the vanilla-flavored composition described above, which comprises: mixing and dispersing vanillin, ethyl vanillin and a solvent, and then adding the remaining components and mixing uniformly.

[0012] The present application provides still another technical solution: a fragrance, which comprises the vanilla-flavored composition described above and / or the vanilla-flavored composition described above.

[0013] Further, the fragrance further comprises a perfume, which has an aroma different from that of the vanilla-flavored composition.

[0014] In some embodiments of the present application, the perfume includes but is not limited to sweet orange aldehyde, sweet orange essential oil, bergamot essential oil, lemon essential oil, etc.

[0015] In some embodiments of the present application, the preparation method of the fragrance comprises: mixing and dispersing vanillin, ethyl vanillin and a solvent, and then adding the remaining components and mixing uniformly. That is, the preparation method of the fragrance of the present application is basically the same as that of the vanilla-flavored composition, and the additional perfume is also added together with the remaining raw materials at the end.

[0016] The present application provides still another technical solution: a cosmetic product, which comprises the vanilla-flavored composition described above and / or the fragrance described above.

[0017] In some embodiments of the present application, the cosmetic product further comprises a combination of one or more of oil, wax and polyol.

[0018] The present application provides still another technical solution: a lipstick composition, which comprises the vanilla-flavored composition described above and / or the fragrance described above, beeswax, synthetic wax and squalane.

[0019] Wherein, in the lip balm composition, the vanilla fragrance type composition and / or essence accounts for 0.01%-15% by mass percentage, beeswax accounts for 10%-35%, synthetic wax accounts for 0.5%-5%, and squalane accounts for 45%-85%.

[0020] Due to the above technical solution, the present application has the following advantages compared with the prior art:

[0021] The main component of the vanilla essence circulating in the market at present is vanillin, which is listed as an allergen component that needs to be labeled in some regions or countries. The present application replaces vanillin, which is listed as an allergen component, with the combination of vanillin, ethyl vanillin, isobutyric acid vanillin ester, and menthyl acetate, to provide a safer vanilla fragrance. At the same time, it is applied to products containing volatile and flavor-changing fragrances to test high-temperature stability, such as hot-filled cosmetic machines that need to be heated for a long time. It is confirmed that the present application can prolong the emission time of fragrance, indicating that it helps to improve the temperature resistance of fragrances, i.e. it can improve the high-temperature durability of volatile and flavor-changing fragrance components. In addition, the present application also tests the light stability of the vanilla fragrance type composition, confirming that the product of the present application also has light stability. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 The dissolution photos of the composition prepared in Example 1 of the present application;

[0023] Figure 2 The dissolution photos of the composition prepared in Comparative Example 2 of the present application;

[0024] Figure 3 The dissolution photos of the composition prepared in Comparative Example 3 of the present application;

[0025] Figure 4 The dissolution photos of the composition prepared in Comparative Example 4 of the present application;

[0026] Figure 5 The photos after light stability test of Example 1 and Comparative Examples 2-4 of the present application;

[0027] Figure 6 The comparison photos of Comparative Example 3 of the present application before and after light stability test. DETAILED DESCRIPTION

[0028] The above scheme will be further described in combination with specific examples; it should be understood that these examples are used to illustrate the basic principles, main features and advantages of the present application, and the present application is not limited in scope by the following examples; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not noted are usually the conditions in conventional experiments.

[0029] All raw materials in the following examples are commercially available or prepared by conventional methods in the art, unless otherwise specified.

[0030] In the following examples, "%" means mass percent, unless otherwise specified. Beeswax was purchased from JEONG NAM FAT AND OIL CHEMICAL CO., LTD, with the brand name BeesWax; Synthetic wax was purchased from SASOL CHEMICAL INDUSTRIES, with the brand name TITANEL; Squalane was purchased from DONGGUAN WINKEY TECHNOLOGY CO., LTD, with the brand name Camellia Squalane Camellia squalane; CITRUS AURANTIUM DULCIS oil was purchased from Shanghai Zhongxiang Fragrance & Flavor Co., Ltd, with the brand name Sweet Orange Oil; CITRUS AURANTIUM BERGAMIA fruit oil was purchased from KIMEX CO., LTD., with the brand name Bergamot Oil New CSN056199.

[0031] (Vanilla fragrance composition and preparation thereof)

[0032] Example 1

[0033] This example provides a vanilla fragrance composition and a preparation method thereof. The formula of the vanilla fragrance composition is shown in Table 1.

[0034] Table 1

[0035] Ingredient Chinese Name CAS No. Example 1 Vanillin 94-86-0 3％ Ethyl vanillin 121-32-4 7％ Raspberry ketone 20665-85-4 8.5％ Menthol acetate 89-48-5 1.5％ Dipropylene glycol 25265-71-8 80％

[0036] The preparation method of the vanilla fragrance composition comprises: vanillin and ethyl vanillin are weighed using a weighing paper and placed in a bottle; dipropylene glycol is added and stirred until there is no powder; the remaining raw materials are added and stirred until uniform, to obtain the vanilla fragrance composition.

[0037] Example 2

[0038] This example provides a vanilla fragrance composition and a preparation method thereof. The formula of the vanilla fragrance composition is shown in Table 2.

[0039] Table 2

[0040] Ingredient Chinese Name CAS No. Example 2 Vanillin 94-86-0 3％ Ethyl vanillin 121-32-4 7％ Raspberry ketone 20665-85-4 7％ Menthol acetate 89-48-5 3％ Dipropylene glycol 25265-71-8 80％

[0041] The preparation method of the vanilla fragrance composition is the same as that of Example 1.

[0042] Comparative Example 1

[0043] This example provides a vanilla fragrance composition and a preparation method thereof. The formula of the vanilla fragrance composition is shown in Table 3.

[0044] Table 3

[0045] Ingredient Chinese Name CAS No. Comparative Example 1 Vanillin 94-86-0 3％ Ethyl vanillin 121-32-4 7％ Raspberry ketone 20665-85-4 10％ Menthol acetate 89-48-5 - Dipropylene glycol 25265-71-8 80％

[0046] The vanilla fragrance composition is prepared according to the method of Example 1.

[0047] Comparative Example 2

[0048] This example provides a vanilla fragrance composition and a method for preparing the same, the formula of which is shown in Table 4.

[0049] Table 4

[0050] Ingredient Chinese Name CAS No. Comparative Example 2 Vanillin 94-86-0 10％ Ethyl vanillin 121-32-4 - Raspberry ketone 20665-85-4 8.5％ Menthol acetate 89-48-5 1.5％ Dipropylene glycol 25265-71-8 80％

[0051] The vanilla fragrance composition is prepared according to the method of Example 1.

[0052] Comparative Example 3

[0053] This example provides a vanilla fragrance composition and a method for preparing the same, the formula of which is shown in Table 5.

[0054] Table 5

[0055] Ingredient Chinese Name CAS No. Comparative Example 3 Vanillin 94-86-0 - Ethyl vanillin 121-32-4 10％ Raspberry ketone 20665-85-4 8.5％ Menthol acetate 89-48-5 1.5％ Dipropylene glycol 25265-71-8 80％

[0056] The vanilla fragrance composition is prepared according to the method of Example 1.

[0057] Comparative Example 4

[0058] This example provides a vanilla fragrance composition and a method for preparing the same, the formula of which is shown in Table 6.

[0059] Table 6

[0060] Ingredient Chinese Name CAS No. Comparative Example 4 Vanillin 94-86-0 3％ Ethyl vanillin 121-32-4 7％ Raspberry ketone 20665-85-4 - Menthol acetate 89-48-5 1.5％ Dipropylene glycol 25265-71-8 88.5％

[0061] The vanilla fragrance composition is prepared according to the method of Example 1.

[0062] Performance Test 1:

[0063] (1) The aroma of Comparative Examples 1-2 and Comparative Example 1 is compared, and it is found that the aroma of Example 1 is consistent with the smell of vanillin; the aroma of Example 2 is relatively close to the smell of vanillin, but has more obvious mint breath; no menthyl acetate is added in Comparative Example 1, and the aroma diffusion ability is poor, and the smell is very weak.

[0064] (2) The dissolution of the compositions obtained in Example 1, Comparative Examples 2-4 is evaluated, which can be seen in Figure 1 to Figure 4 , Figure 1 Example 1, Figure 2 Comparative Example 2,Figure 3 Example 1-2 and Comparative Examples 1-4 were further subjected to sensory questionnaire survey on the smell of the compositions obtained and vanilla beans. The population participating in the test was 10 persons of general male and female aged 25-35 years old. The vanilla bean and the vanilla-scented composition were respectively smelled, and the contents in the following table were scored to calculate the average score to determine the similarity and coordination of the smell of the vanilla-scented composition and the natural vanilla bean. Figure 4 Comparative Example 4, it can be found that Comparative Example 2 has obvious solubility problem, and there are unsolved crystals in the composition system.

[0065] (3) Further sensory questionnaire survey on the smell of the compositions obtained in Example 1-2 and Comparative Examples 1-4 and vanilla beans was conducted. The population participating in the test was 10 persons of general male and female aged 25-35 years old. The vanilla bean and the vanilla-scented composition were respectively smelled, and the contents in the following table were scored to calculate the average score to determine the similarity and coordination of the smell of the vanilla-scented composition and the natural vanilla bean.

[0066] Specifically, there are two indexes, which are shown in Table 7.

[0067] Table 7

[0068]

[0069] The evaluation results are shown in Tables 8-9.

[0070] Table 8

[0071]

[0072] Table 9

[0073]

[0074] From the above evaluation results, it can be seen that the effect of Example 1 of the present application is the best, and the smell similarity and coordination are both high, Example 2 is slightly less, and the smell of other cases is not good, and the smell difference from vanilla beans is relatively obvious.

[0075] (4) Light stability test was conducted on Example 1 and Comparative Examples 2-4, and the test results are shown in Figure 5 It can be seen that Comparative Example 3 has obvious discoloration (in the figure, bottle C corresponds to Example 1, bottle C-1 corresponds to Comparative Example 2, bottle C-2 corresponds to Comparative Example 3, and bottle C-3 corresponds to Comparative Example 4), Figure 6 is the comparison diagram of the composition of Comparative Example 3 after storage in the dark and under natural light (left side is the bottle C-2 under dark condition, and right side is the bottle C-2 under natural light), and no discoloration occurs under dark storage, indicating that ethyl vanillin will affect the stability of the whole composition under light in the case of too high content.

[0076] (perfume and preparation thereof)

[0077] Example 3

[0078] This example provides a perfume and a preparation method thereof, and the formula of the perfume is shown in Table 10. This example provides a perfume and a preparation method thereof, and the formula of the perfume is shown in Table 10.

[0079] Table 10

[0080] Ingredient Chinese Name CAS No. Example 3 Orange sweet 17909-77-2 10％ Vanillin 94-86-0 3％ Ethyl vanillin 121-32-4 7％ Raspberry ketone 20665-85-4 8.5％ Menthol acetate 89-48-5 1.5％ Dipropylene glycol 25265-71-8 70％

[0081] The preparation method of the essence comprises the following steps: vanillin and ethyl vanillin are weighed by using a weighing paper, and then are put into a bottle; dipropylene glycol is added and stirred until no powder is left; and the remaining raw materials are added and stirred until uniform, so as to obtain the essence.

[0082] Example 4

[0083] The example provides an essence and a preparation method thereof, and a formula of the essence is shown in Table 11.

[0084] Table 11

[0085] Ingredient Chinese Name CAS No. Example 4 Orange sweet 17909-77-2 10％ Vanillin 94-86-0 3％ Ethyl vanillin 121-32-4 7％ Raspberry ketone 20665-85-4 7％ Menthol acetate 89-48-5 3％ Dipropylene glycol 25265-71-8 70％

[0086] The preparation method of the essence is the same as that in Example 3.

[0087] (Lipstick composition and preparation thereof)

[0088] Example 5

[0089] The example provides a lipstick composition and a preparation method thereof, and a formula of the lipstick composition is shown in Table 12.

[0090] Table 12

[0091] Ingredient Chinese Name Example 5 Beeswax 22％ Synthetic wax 3％ Squalane 74.8％ Fragrance of Example 3 0.2％

[0092] The preparation method of the lipstick composition comprises the following steps: beeswax, synthetic wax and squalane are weighed into a beaker and heated to 90 DEG C, and then are stirred until completely melted; the essence in Example 3 is added and mixed uniformly; and the temperature is reduced to solidify, so as to obtain the lipstick composition.

[0093] Comparative Examples 5-6

[0094] The example provides a lipstick composition and a preparation method thereof, and a formula of the lipstick composition is shown in Table 13.

[0095] Table 13

[0096]

[0097] The preparation method of the lipstick composition comprises the following steps: beeswax, synthetic wax and squalane are weighed into a beaker and heated to 90 DEG C, and then are stirred until completely melted; the essence in Example 3 is added and mixed uniformly; and the temperature is reduced to solidify, so as to obtain the lipstick composition.

[0098] Performance test 2:

[0099] (1) The Example 5 and Comparative Examples 5-6 were subjected to the following tests, respectively:

[0100] The heating was repeated to 90°C for one hour, and the aroma presentation was compared after cooling and solidification. The simulation of the hot filling process was repeated four times. The formula was a high-hardness lipstick base formula with a high content of wax, which required long-time heating during filling. Therefore, the formula was suitable for investigating the high-temperature resistance of the fragrance. The specific aroma performance is shown in Table 14.

[0101] Table 14

[0102]

[0103] Note: Base odor refers to the characteristic odor of the composition of beeswax, synthetic wax, and squalane.

[0104] From the above experiments, it can be seen that repeated heating has little effect on the odor of Example 5; on the contrary, the high-temperature odor stability of Comparative Examples 5 and 6 is weak. It is shown that the vanilla fragrance composition of Example 3 has better high-temperature resistance than natural citrus essential oil. Example 3 not only can prepare a high-temperature resistant fragrance, but also can continuously cover the characteristic odor of the base under the condition of repeated heating, further lasting the fragrance.

[0105] Example 6

[0106] This example provides a lipstick composition and a preparation method thereof. The formula of the lipstick composition is shown in Table 15.

[0107] Table 15

[0108] Ingredient Chinese Name Example 6 Beeswax 22％ Synthetic wax 3％ Squalane 74.8％ Vanilla fragrance composition of Example 1 0.2％

[0109] The preparation method of the lipstick composition comprises: weighing beeswax, synthetic wax, and squalane into a beaker and heating to 90°C, stirring until completely melted, adding the vanilla fragrance composition of Example 1, mixing, cooling and solidifying, to obtain a lipstick composition.

[0110] Comparative Examples 7-9

[0111] This example provides a lipstick composition and a preparation method thereof. The formula of the lipstick composition is shown in Table 16.

[0112] Table 16

[0113] Ingredient Chinese Name Comparative Example 7 Comparative Example 8 Comparative Example 9 Beeswax 22％ 22％ 22％ Synthetic wax 3％ 3％ 3％ Squalane 74.8％ 74.8％ 74.8％ Vanilla fragrance composition of Comparative Example 2 0.2％ - - Vanilla fragrance composition of Comparative Example 3 - 0.2％ - Vanilla fragrance composition of Comparative Example 4 - - 0.2％

[0114] The preparation method of the lipstick composition comprises: weighing beeswax, synthetic wax, and squalane into a beaker and heating to 90°C, stirring until completely melted, adding the vanilla fragrance composition of Comparative Example 2 or 3 or 4, mixing, cooling and solidifying, to obtain a lipstick composition.

[0115] To ensure the compatibility of the formulation of Example 1, no additional flavor was added, which was directly added to the lip balm composition, and the above-mentioned high-temperature resistance test was carried out with Comparative Examples 2-4 (i.e. repeated heating to 90°C for one hour, and after cooling and solidification, the aroma presented was compared, and the simulation of hot filling engineering was repeated four times).

[0116] The test results are shown in Table 17.

[0117] Table 17

[0118]

[0119] From the above experiments, it can be seen that repeated heating has little effect on the smell of Example 1, and it also has high-temperature resistance.

[0120] The above examples are only for illustrating the technical concept and characteristics of the present application, and the purpose is to enable those skilled in the art to understand the content of the present application and to implement it, and it cannot limit the protection scope of the present application. Any equivalent changes or modifications made in accordance with the spirit and essence of the present application should be covered within the protection scope of the present application.

[0121] The endpoints of the ranges and any values disclosed herein are not limited to the precise values recited as the exact dimensions are not considered critical for the present application. The endpoints of the ranges of values and the values of the ranges themselves should be understood to be approximate. The exact numerical values of the endpoints of the ranges and the individual points of the ranges can be combined with one or more of the other ranges or points to form new ranges or points that are not expressly disclosed.

Claims

1. A vanilla-scented composition, characterized in that, The composition comprises a concentrated vanillin, ethyl vanillin, vanillin isobutyrate, menthyl acetate, and a solvent; wherein the mass ratio of the concentrated vanillin, ethyl vanillin, vanillin isobutyrate, and menthyl acetate is 1:1.5-3:1.5-3.5:0.1-1.0; and the content of the concentrated vanillin in the composition is less than or equal to 6% by mass percentage.

2. The vanilla-scented composition according to claim 1, characterized in that, The composition comprises, by weight percentage: 0.5%-6% concentrated vanillin, 4%-9% ethyl vanillin, 5%-15% vanillin isobutyrate, and 0.1%-4% menthyl acetate.

3. The vanilla-scented composition according to claim 1 or 2, characterized in that, The composition comprises, by weight percentage: 2%-4% concentrated vanillin, 6%-8% ethyl vanillin, 7.5%-9.5% vanillin isobutyrate, and 1%-2% menthyl acetate.

4. The vanilla-scented composition according to claim 1, characterized in that, The mass ratio of the concentrated vanillin, the ethyl vanillin, the vanillin isobutyrate ester, and the menthyl acetate is 1:1.8-2.8:2.5-3.0:0.3-0.8; and / or, the solvent comprises one or more combinations selected from propylene glycol, triacetin, caprylic / capric triacetin, ethanol, isopropyl myristate, and triethyl citrate.

5. A method for preparing the vanilla-scented composition according to any one of claims 1-4, characterized in that, The preparation method includes: mixing and dispersing concentrated vanillin, ethyl vanillin and solvent, then adding the remaining components and mixing well.

6. A fragrance, characterized in that, The flavoring comprises the vanilla-scented composition according to any one of claims 1-4.

7. The fragrance according to claim 6, characterized in that, The flavoring also includes a fragrance that has an aroma different from that of the vanilla-scented composition.

8. A cosmetic product, characterized in that, The cosmetic comprises the vanilla-scented composition of any one of claims 1-4 and / or the fragrance of claim 6 or 7.

9. The cosmetic product according to claim 8, characterized in that, The cosmetics also contain one or more of the following: oils, waxes, and polyols.

10. A lipstick composition, characterized in that, The lipstick composition comprises the vanilla-scented composition of any one of claims 1-4 and / or the fragrance, beeswax, synthetic wax and squalane of claim 6 or 7; The lipstick composition, by weight percentage, comprises 0.01%-15% vanilla flavoring and / or fragrance, 10%-35% beeswax, 0.5%-5% synthetic wax, and 45%-85% squalane.

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