METHOD AND TEST KIT FOR RECREATION OF AN ODOR

Abstract

Suggested is a method for the extraction of fragrances from natural starting material consisting of the following steps: (a) providing a sample of the natural starting material in a pressure proof sample container; (b) bringing in the sample in contact with liquefied petroleum gas of propane and/or butane gas, preferably; (c) extracting the fragrances from the natural starting material provided in step (b); (d) venting of the pressure proof sample container, while the liquefied petroleum gas is evaporated and the fragrances is maintained as residue in the container; and optionally (e) dissolving the fragrances in a suitable solvent.

Claims

1. A method for the extraction of fragrances from natural starting material comprising the following steps: (a) providing a sample of the natural starting material in a pressure proof sample container; (b) bringing in the sample in contact with liquefied petroleum gas of propane and/or butane gas, preferably; (c) extracting the fragrances from the natural starting material provided in step (b); (d) venting of the pressure proof sample container, while the liquefied petroleum gas is evaporated and the fragrances is maintained as residue in the container; and optionally (e) dissolving the fragrances in a suitable solvent.

2. The method of claim 1, wherein step (b) is conducted at a temperature of from about 5 C. to about 70 C. and/or a pressure of from about 0.5 bar to about 10 bar.

3. The method of claim 1, wherein the natural starting material is selected from the group consisting of a whole plant, leaves, blossoms, stems, seeds, bark, wood, resins, petals, stamen, pollen, fruits, root or a shoot of the plant, parts of fruits or blossoms and mixtures thereof.

4. The method of claim 1, wherein said natural starting material is put into a sachet before the extraction (step c).

5. The method of claim 1, wherein said solvent is an alcohol, an ester, a ketone each of them having 1 to 5 carbon atoms or an alkane having 5 to 8 carbon atoms.

6. The method of claim 5, wherein said solvent is methanol and/or ethanol.

7. The method of claim 5, wherein the extract obtained from step (c) comprises a mixture of fragrances.

8. The method of claim 1 which is a micro-extraction method for odor test.

9. The method of claim 1, wherein said sample of said natural starting material has a maximum weight of 50 g.

10. A kit for a micro-extraction of fragrances from natural starting materials, comprising: (i) a pressure proof sample container with an exchangeable valve; (ii) a pressure vessel or container, containing liquefied petroleum gas of propane and/or butane gas, equipped with an outlet device; (iii) a coupler for the connection of (i) and (ii); (iv) a sachet, suitable for the intake of sample materials and optionally (v) a storage container suitable for absorbing the extracted compounds.

11. The kit of claim 10, wherein the pressure vessel or container is double-walled having an inner wall and an outer wall.

12. The kit of claim 11, wherein the inner wall is made of glass and the outer wall is made of synthetic, thermoplastic materials.

13. The kit of claim 11, wherein the inner wall is made of borosilicate glass.

14. The kit of claim 11, wherein the ground of the inner wall is rounded for easy removal of the fragrance extract.

15. The kit of claim 11, wherein the outer wall is made from polypropylene glycol.

Description

EXAMPLES

Example 1

General Procedure for Extraction of a Plant

[0037] Various extraction materials were placed first into a sachet and the sachet then placed into a pressure proof sample container (extraction container) which possesses a gas-tight seal (septum). The extraction was performed in that compacted n-butane from a pressure vessel was transferred through the valve of the septum into the extraction container, thus the liquid n-butane gas could wet the plant material. The extraction container was set into rotation in order to let liquid butane wet all parts of the plant material for about 5 to 10 minutes. Subsequently, n-butane gas was leaked from the extraction container by opening the valve slowly. Subsequently ethanol was sprayed into the extraction container and the alcoholic extract was transferred into a storage container

Example 2

Sampling Procedure

[0038] 1. Using gloves take the object you would like to sample, pick it to pieces and fill it into a filter-bag (for better handling use the attached tweezer). The amount depends on the intensity of the smell of the object. If the smell is quite low you can fill the bag completely. If the smell is more intensive you need lower amounts. [0039] 2. Open the extraction-tube by screwing the screw cap and enter the bag into the tube (FIG. 1). Take care that the end of the bag containing the object is close to the bottom of the tube. The other end has to be near the screw cap (FIG. 2). Close the tube using the screw cap again. [0040] 3. Take one of the gas-adapters and connect it to one of the bottles of butane-gas (FIG. 3). [0041] 4. Connect the gas-bottle to the extraction-tube (FIGS. 4 and 5). [0042] 5. Press the gas-bottle toward the extraction-tube and fill up the tube to the black mark (FIGS. 6 and 7) [0043] 6. Extract the object by holding the tube at the end with the screw cap and swinging round the other end of the tube for 10 minutes. [0044] 7. Open the tube carefully. Remove the bag and squeeze out the butane from the bag to the tube by pushing the bag against the inner wall of the tube. [0045] 8. Add approximately 2 ml of ethanol (10 times pushing the pump valve of the ethanol-bottle) to the inner wall of the tube before the gas is completely evaporated (FIG. 8). [0046] 9. Wait until the butane in the solvent mixture is evaporated. [0047] 10. Solve the extract by slewing the tube and transfer the extract-solution using a pipette to one of the brown glass-bottles (FIGS. 9 and 10). Repeat this solving a second time to the same brown glass-bottle using 2 ml ethanol. [0048] 11. Close the brown glass-bottle and fill in the corresponding information sheet. Please note all possible information! [0049] 12. To use the extraction-tube again clean the tube and the seal well and replace the gas-valve in the screw cap. For cleaning use hot water and any solvent available (e.g. acetone). [0050] 13. Use the attached smelling strips to check the smell of the extract.

Example 3

Sensory Test

[0051] The sensorial profiles of the extracts obtaining according to the general extraction procedure described in Example 1 were compared with the respective sensorial profiles of extraction samples of the same plant starting material which has been extracted by a two-step process using first n-butane and then supercritical carbon dioxide as disclosed in EP 0711508 B1. The odors were evaluated by a panel consisting of 20 experienced perfumers and rated on the following scale (10)=both odors are identical to (1)=both odors are completely different. The results represent the average over all panelists and are compiled in the following Table 1:

TABLE-US-00001 TABLE 1 Comparison of odors Example Plant Part Accordance 1 Rose blossom 8.9 2 Fig leaves 8.5 3 Clove fruits 9.1 4 Pepper seeds 9.5 5 Lavender blossom 9.5 6 Seringat blossom 9.1 7 Vetiver roots 9.2

[0052] The results clearly demonstrate that the extracts obtained from the micro-process according to the present invention provide a rather similar to identical odour compared to the extracts that are obtained under industrial conditions

Example 4

Comparison of Butane Extraction, Soxhlet Extraction and SDE

[0053] 20 g peels taken from 4 oranges were subjected to a butane extraction according to the present invention, a standard Soxhlet extraction and SDE (pH=7, 4 h, 2 g defoamer). The extracts were evaluated both in terms of sensory profile and analytical composition. The results are compiled in Table 2.

TABLE-US-00002 TABLE 2 Analytical compositions (components above 0.05%) Example 3 Example 3 Orange oil Component (Run A) (Run B) SDE (BR) Limonen 89.116 91.483 95.095 95.317 Myrcen, beta 1.766 1.503 1.727 1.972 Linalool 0.331 0.727 0.334 0.484 Sabinen 1.067 0.548 0.727 0.273 Valencen 0.544 0.419 0.204 0.038 Pinen, alpha 0.405 0.093 0.422 0.515 Pinen, beta 0.055 0.023 0.040 0.021

[0054] Although all processes showed an acceptable accordance with regard to a standard orange oil from Brazil only the products obtained from the process according to the present invention provided a sensory profile similar to orange oil.