Method for extracting lemon aroma components of perfume

Abstract

The invention discloses a method for extracting lemon aroma components of perfume, and relates to the technical field of food processing. The extraction method of the perfume lemon aroma component comprises the following steps: (1) drying, grinding and sieving perfume lemon peel to obtain perfume lemon peel powder; (2) the perfume lemon peel powder is added into a supercritical carbon dioxide extraction kettle for extraction, a perfume lemon extract is obtained, a sample basket is arranged in the supercritical carbon dioxide extraction kettle, the perfume lemon peel powder is filled with a degreasing cotton pad, and a through hole is formed in the center of the degreasing cotton pad; and (3) centrifuging the perfume lemon extract, and collecting to obtain perfume lemon aroma components. The perfume lemon aroma components are extracted by adopting a supercritical carbon dioxide extraction method, and the yield of the extracted perfume lemon extract is analyzed by adopting a specific absorbent cotton pad filling method, so that the extraction efficiency of the subsequent supercritical carbon dioxide perfume lemon extraction process is optimized.

Description

Technical Field

[0001] The present invention relates to the technical field of food processing, and in particular to a method for extracting the aroma components of perfume lemons. Background Art

[0002] With its unique appearance, taste and nutritional value, the perfume lemon has become a leader in the lemon family. The perfume lemon is now often used as a key aroma component and incorporated into freshly made drinks such as fresh lemon tea. Although the freshly made lemon tea has less stringent requirements for flavor consistency, when applied to non-freshly made drinks such as soft drinks, due to the differences in the origin, production batches and individuals of the perfume lemons, it often leads to significant fluctuations in the taste of the drinks, which is contrary to the principle of maintaining consistent food flavors. Therefore, in order to ensure the stability and uniformity of the drink aroma, it is necessary to carefully blend with aroma components with long-lasting and stable aromas.

[0003] Currently, the mainstream extraction techniques for the aroma components of citrus peels including perfume lemons cover organic solvent extraction, steam distillation and pressing. However, these three methods generally face the problems of low purity of the extracted aroma components, long time consumption and difficulty in completely removing solvent residues. Summary of the Invention

[0004] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a method for extracting the aroma components of perfume lemons. The present invention uses supercritical carbon dioxide extraction to extract the aroma components of perfume lemons, and adopts a specific method for loading the degreased cotton pads, and analyzes the yield of the perfume lemon extract after extraction, so as to optimize the extraction efficiency of the subsequent supercritical carbon dioxide extraction process for perfume lemons.

[0005] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0006] The present invention provides a method for extracting the aroma components of perfume lemons, including the following steps:

[0007] (1) Dry, grind and sieve the perfume lemon peel to obtain perfume lemon peel powder;

[0008] (2) Add the perfume lemon peel powder into a supercritical carbon dioxide extraction kettle for extraction to obtain a perfume lemon extract. A sample basket is provided in the supercritical carbon dioxide extraction kettle. A degreased cotton pad is loaded in the perfume lemon peel powder. The height of the degreased cotton pad is 50% of the effective height of the sample basket, and a through hole is provided in the center of the degreased cotton pad;

[0009] (3) Centrifuge the perfume lemon extract and collect to obtain the perfume lemon aroma components.

[0010] Preferably, in the step (1), the particle size of the perfume lemon peel powder is 30 mesh.

[0011] Preferably, in the step (2), the volumetric flow rate of the supercritical carbon dioxide is 13 - 14 mL / min. Preferably, it is 13.92 mL / min.

[0012] Preferably, in the step (2), the extraction temperature is 40 - 45 °C, the extraction pressure is 250 bar, and the extraction time is 1.5 - 2 h.

[0013] Preferably, in the step (2), the sample basket is cylindrical and made of stainless steel.

[0014] Preferably, in the step (2), the diameter of the absorbent cotton pad is 80 - 90 mm, and the thickness is 9 - 10 mm.

[0015] Preferably, in the step (2), the diameter of the through - hole is 15 mm.

[0016] Preferably, in the step (2), the effective height of the sample basket is 152 mm.

[0017] Preferably, in the step (2), absorbent cotton pads are filled at both the inlet end and the outlet end of the sample basket.

[0018] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0019] (1) The present invention adopts the supercritical carbon dioxide extraction method to study and analyze the perfume lemon extract. By comparing the differences in the yields of the extracts obtained by supercritical carbon dioxide extraction of perfume lemon under different filling methods, the extraction efficiency of the subsequent supercritical carbon dioxide extraction process of perfume lemon is optimized.

[0020] (2) The present invention adjusts the material density through the absorbent cotton pad provided with through - holes, optimizing the contact area and contact time between the supercritical fluid and the material; moreover, the design of the through - hole structure effectively inhibits the "short - circuit flow" of the fluid along the inner wall of the sample basket, strengthening the uniform distribution of the fluid in the material layer; at the same time, the present invention shows stability in repeated experiments, verifying the reliability of its process.

[0021] (3) The present invention reveals the regulation mechanism of the structure of the absorbent cotton pad on the supercritical fluid dynamics, providing a theoretical basis and technical reference for the development of high - efficiency extraction processes for natural products. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the supercritical carbon dioxide extraction kettle and the absorbent cotton pad of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0023] To better illustrate the purpose, technical solution and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments. However, the protection scope and implementation manner of the present invention are not limited thereto.

[0024] For the materials, reagents, etc. used in the following embodiments, unless otherwise specified, they are reagents and materials that can be obtained from commercial channels.

[0025] As Figure 1 As shown, the extraction kettle of the present invention is a 1000 mL supercritical carbon dioxide extraction kettle. There is a sample basket with an inner diameter of 68 mm and an inner height of 190 mm in the extraction kettle. The sample basket is cylindrical and made of stainless steel. Since the material loading does not exceed 80% of the height of the sample basket, the effective height of the sample basket is 152 mm. Figure 1 In

[0026] The sample basket is filled with a disc-shaped absorbent cotton pad. The diameter of 1 unit of absorbent cotton pad is 80 mm, the thickness is 10 mm, and the weight is 2 g.

[0027] The above extraction kettle and absorbent cotton pad are used in the following examples and comparative examples.

[0028] Example 1

[0029] A method for extracting the aroma components of lemon perfume, comprising the following steps:

[0030] (1) Dry, grind and sieve the lemon perfume peel to obtain lemon perfume peel powder with a mesh size of 30.

[0031] (2) Add 250 ± 2 g of lemon perfume peel powder to the supercritical carbon dioxide extraction kettle for extraction, and collect the lemon perfume extraction solution after extraction.

[0032] The extraction conditions are: extraction temperature is 45 °C, extraction pressure is 250 bar, and extraction time is 2 h; the collection conditions are: ambient temperature 25 °C, and the flow rate of the outlet valve is 5 L / min (the volume flow rate of liquid carbon dioxide is 13.92 ml / min).

[0033] (3) Centrifuge the lemon perfume extraction solution and collect the supernatant to obtain the aroma components of lemon perfume.

[0034] In this embodiment, the loading order of the sample is: first, put 1 unit of absorbent cotton pad into the inlet end of the sample basket to isolate the sample, then add half of the amount of lemon perfume peel powder into the sample basket, then put 2 units of absorbent cotton pad at 50% of the effective height of the sample basket, then add the remaining half of the amount of lemon perfume peel powder into the sample basket, and finally put 1 unit of absorbent cotton pad into the outlet end of the sample basket to isolate the sample.

[0035] The height of the absorbent cotton pad in the sample is 50% of the effective height of the sample basket, that is, 2 units of absorbent cotton pads are filled from the bottom of the sample basket to 76 mm, and a through-hole with a diameter of 15 mm is expanded at the center of the absorbent cotton pad using a stainless steel metal rod. The position and diameter of the through-hole are consistent with the upper and lower interfaces of the extraction kettle.

[0036] Comparative Example 1

[0037] A method for extracting the aroma components of perfume lemon includes the following steps:

[0038] (1) Dry, grind, and sieve the perfume lemon peel to obtain perfume lemon peel powder with a mesh size of 30.

[0039] (2) Add 250 ± 2 g of perfume lemon peel powder to a supercritical carbon dioxide extraction kettle for extraction, and collect the perfume lemon extract after extraction.

[0040] The extraction conditions are: extraction temperature is 45 °C, extraction pressure is 250 bar, and extraction time is 2 h; the collection conditions are: ambient temperature 25 °C, outlet valve flow rate is 5 L / min (the volume flow rate of liquid carbon dioxide is 13.92 ml / min).

[0041] (3) Centrifuge the perfume lemon extract and collect the supernatant to obtain the aroma components of perfume lemon.

[0042] In this comparative example, the loading order of the sample is: first, load 1 unit of absorbent cotton pad into the inlet end of the sample basket to isolate the sample, then add the perfume lemon peel powder into the sample basket, and finally load 1 unit of absorbent cotton pad into the outlet end of the sample basket to isolate the sample.

[0043] Comparative Example 2

[0044] A method for extracting the aroma components of perfume lemon includes the following steps:

[0045] (1) Dry, grind, and sieve the perfume lemon peel to obtain perfume lemon peel powder with a mesh size of 30.

[0046] (2) Add 250 ± 2 g of perfume lemon peel powder to a supercritical carbon dioxide extraction kettle for extraction, and collect the perfume lemon extract after extraction.

[0047] The extraction conditions are: extraction temperature is 45 °C, extraction pressure is 250 bar, and extraction time is 2 h; the collection conditions are: ambient temperature 25 °C, outlet valve flow rate is 5 L / min (the volume flow rate of liquid carbon dioxide is 13.92 ml / min).

[0048] (3) Centrifuge the perfume lemon extract and collect the supernatant to obtain the aroma components of perfume lemon.

[0049] In this comparative example, the loading sequence of the sample is as follows: First, load 1 unit of absorbent cotton pad into the inlet end of the sample basket to isolate the sample. Then, add one-third of the amount of lemon peel powder into the sample basket. Next, load 1 unit of absorbent cotton pad at 30% of the effective height of the sample basket. Subsequently, add one-third of the amount of lemon peel powder into the sample basket. Then, load 1 unit of absorbent cotton pad at 60% of the effective height of the sample basket. Next, add the remaining one-third of the amount of lemon peel powder into the sample basket. Finally, load 1 unit of absorbent cotton pad into the outlet end of the sample basket to isolate the sample.

[0050] The height of the absorbent cotton pad in the sample is 30% and 60% of the effective height of the extraction kettle, that is, load 1 unit of absorbent cotton pad at 45 mm and 91 mm from the bottom of the extraction kettle respectively, and use a stainless steel metal rod to expand a through-hole with a diameter of 15 mm in the center of the absorbent cotton pad. The position and diameter of the through-hole are consistent with the upper and lower interfaces of the extraction kettle.

[0051] Comparative Example 3

[0052] A method for extracting the aroma components of lemon includes the following steps:

[0053] (1) Dry, grind and sieve the lemon peel to obtain lemon peel powder with a mesh size of 30.

[0054] (2) Add 250 ± 2 g of lemon peel powder into a supercritical carbon dioxide extraction kettle for extraction, and collect the lemon extract after extraction.

[0055] The extraction conditions are: extraction temperature is 45 °C, extraction pressure is 250 bar, and extraction time is 2 h; the collection conditions are: ambient temperature 25 °C, outlet valve flow rate is 5 L / min (the volume flow rate of liquid carbon dioxide is 13.92 ml / min).

[0056] (3) Centrifuge the lemon extract and collect the supernatant to obtain the aroma components of lemon.

[0057] In this comparative example, the loading sequence of the sample is as follows: First, load 1 unit of absorbent cotton pad into the inlet end of the sample basket to isolate the sample. Then, add half of the amount of lemon peel powder into the sample basket. Next, load 2 units of absorbent cotton pad at 50% of the effective height of the sample basket. Subsequently, add the remaining half of the amount of lemon peel powder into the sample basket. Finally, load 1 unit of absorbent cotton pad into the outlet end of the sample basket to isolate the sample.

[0058] The height of the absorbent cotton pad in the sample is 50% of the effective height of the extraction kettle, that is, load 2 units of absorbent cotton pad at 76 mm from the bottom of the extraction kettle, and the absorbent cotton pad is not provided with a through-hole.

[0059] Comparative Example 4

[0060] A method for extracting the aroma components of perfume lemons, comprising the following steps:

[0061] (1) Dry, grind, and sieve the perfume lemon peel to obtain perfume lemon peel powder with a mesh size of 30.

[0062] (2) Add 250 ± 2 g of the perfume lemon peel powder into a supercritical carbon dioxide extraction kettle for extraction, and collect the perfume lemon extract after extraction.

[0063] The extraction conditions are: extraction temperature is 45 °C, extraction pressure is 250 bar, and extraction time is 2 h; the collection conditions are: ambient temperature is 25 °C, and the flow rate of the outlet valve is 5 L / min (the volume flow rate of liquid carbon dioxide is 13.92 ml / min).

[0064] (3) Centrifuge the perfume lemon extract and collect the supernatant to obtain the aroma components of the perfume lemon.

[0065] In this comparative example, the loading order of the sample is as follows: First, load 1 unit of absorbent cotton pad into the inlet end of the sample basket to isolate the sample, then add one-third of the amount of perfume lemon peel powder into the sample basket, then load 1 unit of absorbent cotton pad at 30% of the effective height of the sample basket, then add one-third of the amount of perfume lemon peel powder into the sample basket, then load 1 unit of absorbent cotton pad at 60% of the effective height of the sample basket, then add the remaining one-third of the amount of perfume lemon peel powder into the sample basket, and finally load 1 unit of absorbent cotton pad into the outlet end of the sample basket to isolate the sample.

[0066] The height of the absorbent cotton pad in the sample is 30% and 60% of the effective height of the extraction kettle, that is, 1 unit of absorbent cotton pad is loaded at 45 mm and 91 mm from the bottom of the extraction kettle respectively, and the absorbent cotton pad is not provided with through holes.

[0067] Detection method

[0068] Weigh the masses of the perfume lemon extracts obtained in the above-mentioned examples and comparative examples respectively, and then calculate the yield of the perfume lemon extract after extraction. The yield = (mass of the perfume lemon extract) / (mass of the perfume lemon peel powder sample) × 100%.

[0069] The detection results are shown in Table 1.

[0070] Table 1

[0071]

[0072] From the comparison between Comparative Example 1 and Example 1, it can be seen that in Comparative Example 1, no absorbent cotton pad was loaded in the sample, and the average yield of the perfume lemon extract was only 3.25%, indicating that if no absorbent cotton is loaded in the sample, the yield of the perfume lemon extract is very low.

[0073] It can be obtained by comparing Comparative Example 2 with Example 1 that under the same extraction conditions, the average yield of Example 1 is 16% higher than that of Comparative Example 2, indicating that filling 1 unit of absorbent cotton pads at 30% and 60% of the effective height of the sample basket cannot significantly improve the yield of the lemon extract, and the filling height of the absorbent cotton pads will affect the yield of the lemon extract. The reason is that: in the extraction state, the density of the upper material is relatively lower than that of the lower material, which reduces the contact time and contact area between the supercritical fluid and the material, and thus reduces the yield of the lemon extract.

[0074] It can be obtained by comparing Comparative Example 3 with Example 1 that under the same filling height, the average yield of Example 1 is 18% higher than that of Comparative Example 3, indicating that providing a through hole in the center of the absorbent cotton pad is beneficial to improving the yield of the lemon extract.

[0075] It can be obtained by comparing Comparative Example 4 with Example 1 that under the same extraction conditions, the average yield of Comparative Example 4 is only 3.38%, while the average yield of Example 1 can reach 4.12%, indicating that filling 1 unit of absorbent cotton pads at 30% and 60% of the effective height of the sample basket and not providing a through hole in the center of the absorbent cotton pad cannot significantly improve the yield of the lemon extract. The reason is that the density of the upper material is relatively low, and the filling of the upper absorbent cotton hinders the fluid penetration, resulting in a yield of only 3.38% for Comparative Example 4, indicating that the synergistic effect of the absorbent cotton highly depends on the material distribution characteristics.

[0076] In summary, in the present invention, by filling 2 units of absorbent cotton pads at 50% of the effective height of the sample basket and providing a 15-mm through hole in the center of the absorbent cotton pad, the yield of the lemon extract reaches the highest. The reason is that: adding the absorbent cotton pad at 50% of the effective height of the sample basket can prevent the material density from being too high, increase the contact area and contact time between the supercritical fluid and the material. At the same time, the through hole in the middle of the absorbent cotton pad can reduce the situation where the supercritical fluid of the lower material flows along the inner wall of the extraction kettle to the upper material, thereby further increasing the contact area and contact time between the supercritical fluid and the material, and thus increasing the yield of the product. Moreover, the RSD of Example 1 is only 2.30%, indicating that the method of the present invention has high stability.

[0077] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for extracting the aroma components of perfume lemon, characterized in that, It includes the following steps: (1) Dry, grind, and sieve the perfume lemon peel to obtain perfume lemon peel powder; (2) Add the perfume lemon peel powder into a supercritical carbon dioxide extraction kettle for extraction to obtain a perfume lemon extract. There is a sample basket in the supercritical carbon dioxide extraction kettle. The perfume lemon peel powder is filled with a degreased cotton pad. The height of the degreased cotton pad is 50% of the effective height of the sample basket, and a through hole is provided at the center of the degreased cotton pad; (3) Centrifuge the perfume lemon extract and collect the perfume lemon aroma components.

2. The extraction method of the perfume lemon aroma components according to claim 1, wherein, In step (1), the particle size of the perfume lemon peel powder is 30 mesh.

3. The extraction method of the perfume lemon aroma component according to claim 1, characterized in that In step (2), the volume flow rate of the supercritical carbon dioxide is 13 - 14 mL / min.

4. The extraction method of the perfume lemon aroma component according to claim 1, characterized in that, In step (2), the extraction temperature is 40 - 45 °C, the extraction pressure is 250 bar, and the extraction time is 1.5 - 2 h.

5. The extraction method of the perfume lemon aroma component according to claim 1, characterized in that, In step (2), the sample basket is cylindrical and made of stainless steel.

6. The extraction method of the perfume lemon aroma component according to claim 1, characterized in that, In step (2), the diameter of the degreased cotton pad is 80 - 90 mm, and the thickness is 9 - 10 mm.

7. The extraction method of the aroma components of lemon perfume according to claim 1, characterized in that, In step (2), the effective height of the sample basket is 152 mm.

8. The extraction method of the perfume lemon aroma components according to claim 1, characterized in that, In step (2), the diameter of the through hole is 15 mm.

9. The extraction method of the perfume lemon aroma component according to claim 1, characterized in that, In step (2), both the inlet end and the outlet end of the sample basket are filled with degreased cotton pads.

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