Patent ID: 12251412

DESCRIPTION OF EXEMPLARY EMBODIMENTS

Hereinafter, embodiments of the present disclosure will be described in detail with reference to the accompanying drawings so that a person of ordinary skill in the art to which the present disclosure pertains can easily implement the embodiments of the present disclosure. However, the present disclosure may be embodied in various different forms and is not limited to the embodiments and drawings described herein.

The present disclosure has been completed by paying attention to the fact that a cold brew method of extracting with cold water for a long time even when extracting with the same coffee beans has a higher caffeine content and less bitter taste while researching a low-temperature extraction method in order to more safely and efficiently extract physiologically active ingredients of natural products that are weak to heat.

A method for extracting caffeic acid and rosmarinic acid fromRosmarinus officinalisL. according to an embodiment of the present disclosure will be described in detail with reference to the accompanying drawings.

FIG.1is a view showing a process for extracting caffeic acid and rosmarinic acid fromRosmarinus officinalisL., according to an embodiment of the present disclosure, andFIGS.2and3are views schematically showing extraction apparatuses for extracting caffeic acid and rosmarinic acid fromRosmarinus officinalisL., according to embodiments of the present disclosure.

Referring toFIGS.1to3, an extraction apparatus capable of extracting caffeic acid and rosmarinic acid fromRosmarinus officinalisL. is first prepared (step S1).

As can be seen inFIG.2, the extraction apparatus100has an extractor10positioned in an upper part thereof, and a receiver20is positioned in a lower part of the extractor10.

The extractor10passes a solution contained in a main body unit11through a filtration membrane12to obtain a filtered solution, and drops the filtered solution to the lower outside through a dropping unit13connected to a lower portion of the main body unit11.

The extractor10is a reactor for extracting active ingredients from the solid by containing a solid such as driedRosmarinus officinalisL.,Rosmarinus officinalisL. powder, or the like and a solvent together, and includes a filtration membrane12capable of preventing loss of the solid and filtering the extracted solution. Preferably, a stopcock valve is located in the dropping unit13to enable the dropping speed of the filtered solution containing the active ingredients to be adjusted.

The receiver20is located in the lower part of the extractor10and is for collecting the filtered solution containing the active ingredients ofRosmarinus officinalisL. dropped from the dropping unit13, and the types of the receiver is not limited.

Further, it is important to constantly maintain the amount of an extraction solvent in order to increase the extraction efficiency of a raw material in the main body unit11, and it is good to continuously replenish a new solution to the main body unit11by the amount of the solution decreased when the solution that contains the active ingredients and is contained in the main body unit11is discharged to the bottom. For this purpose, a reservoir30capable of storing the new solvent may be further included, and the reservoir30may be positioned above the extractor10as can be seen inFIG.3. It is preferably for the reservoir30to include a stopcock valve so as to control the dropping speed of the new solvent.

Subsequently, the driedRosmarinus officinalisL. is put into the main body unit11, and a solvent is added to the main body unit11to immerse the driedRosmarinus officinalisL. at room temperature (step S2).

The driedRosmarinus officinalisL. may be cut to a predetermined size or may be powdered in order to increase the extraction efficiency.

When extracting the driedRosmarinus officinalisL., the extraction efficiency of caffeic acid and rosmarinic acid can be increased by puttingRosmarinus officinalisL. and a solvent in the main body unit11and immersingRosmarinus officinalisL. at room temperature.

Here, immersion is for impregnating the solvent in the cell membrane of a dried raw material, that is, soaking the raw material, and it is much more efficient to perform extraction after immersion than to perform extraction immediately in a dried state.

Further, the solvent may be alcohols, and more specifically, it may include any one selected from the group consisting of C1-C5monohydric alcohols, C2-C5dihydric alcohols, and C3-C5trihydric alcohols, or mixtures of two or more thereof.

Although the monohydric alcohols may be methanol, ethanol, propanol, isopropanol, butanol, t-butanol and pentanol, the dihydric alcohols may be ethylene glycol, propylene glycol, butylene glycol, and pentylene glycol, and the trihydric alcohols may be glycerol, the types thereof are not limited.

When dihydric alcohols and trihydric alcohols except ethanol were used alone, caffeic acid and rosmarinic acid have not been detected at all in the case of performing extraction by a conventional room temperature immersion method for 24 hours, but remarkably higher amounts of caffeic acid and rosmarinic acid have been detected in the case of performing extraction by the method according to the present disclosure.

Further, caffeic acid and rosmarinic acid have not been detected at all even if stirring was performed when the solvent was water, or when the content of water in the solvent was more than half, for example, 80% by weight or more in the case of performing extraction by the conventional room temperature immersion method. However, large amounts of caffeic acid and rosmarinic acid have been detected when a solvent obtained by mixing water and the alcohols was used, and even when the content of water in the solvent was more than half, for example, 80% by weight or more in the case of performing extraction by the method according to the present disclosure.

Subsequently, a solution in which the driedRosmarinus officinalisL. is immersed is dropped from the dropping unit13to the receiver20(step S3).

When the driedRosmarinus officinalisL. sufficiently contains an extraction solvent, the solution is dropped into the receiver through the dropping unit13located at the lower portion of the extractor10. At this time, the dropping solution is collected in the receiver by performing dropping extraction while adjusting the dropping speed by opening the stopcock valve located in the dropping unit13.

At this time, the dropping extraction may be performed again by transferring the solution contained in the receiver20to the main body unit11after the step (S3). The solution contained in the receiver20may be transferred to the main body unit11, and may further be transferred even to the reservoir30. The extraction efficiency of caffeic acid and rosmarinic acid can be further increased through such a process.

As described above, a method for extracting caffeic acid and rosmarinic acid fromRosmarinus officinalisL. according to the present disclosure is a very efficient method for extracting caffeic acid and rosmarinic acid through alcohols or a mixed solvent of the alcohols and water while minimizing loss of active ingredients weak to heat by performing extraction at room temperature.

Hereinafter, the present disclosure will be described in more detail through specific Examples. The following Examples are intended to illustrate the present disclosure, but the present disclosure is not limited by the following Examples.

Example: Dropping Extraction

As an extractor for passing a solution contained in the main body unit through the filtration membrane to obtain a filtered solution, and dropping the filtered solution to the lower outside through the dropping unit connected to the lower portion of the main body unit, an extractor capable of adjusting the dropping speed of the solution was installed in the upper part, and a receiver for collecting the filtered solution dropped from the dropping unit of the extractor was installed in the lower part of the extractor.

After putting 50 g of driedRosmarinus officinalisL. and 950 g of each solvent shown in Table 2 into the main body unit of the prepared extractor, and immersing the driedRosmarinus officinalisL. in the solvent at room temperature for 1 hour so that the driedRosmarinus officinalisL. could sufficiently absorb the solvent, an extract was obtained by slowly dropping the solution of the extractor into the receiver in the lower part for 30 minutes.

For reference, the extracted extract was extracted once more (extracted twice) by injecting an extract extracted in Example 5c into the extractor again in Example 6a of Table 2 below, and the extracted extract was extracted one more time (extracted three times) by injecting an extract extracted in Example 6a into the extractor again in Example 6b.

Comparative Example: Immersion Extraction

After putting 50 g of driedRosmarinus officinalisL. and 950 g of each solvent shown in Table 2 below into a general container and immersing the driedRosmarinus officinalisL. in the solvent at room temperature for 24 hours, aRosmarinus officinalisL. extract was obtained by performing filtration.

Experimental Example: Analysis of Extract Ingredients

The contents of ingredients were checked depending on the following analysis conditions.

After dissolving standard products of caffeic acid and rosmarinic acid in an HPLC mobile phase to prepare a solution with a concentration of 100 ppm, a standard solution was prepared by filtering the solution with a PVDF membrane filter having a thickness of 0.45 μm.

Sample solutions of Examples and Comparative Examples were prepared by filtering undiluted solutions ofRosmarinus officinalisL. extracts (immersion extraction and dropping extraction) with a filter having a thickness of 0.45 μm, analysis was carried out depending on the following HPLC analysis conditions, and the results are shown in Table 2.

1. Analysis Equipment

High Performance Liquid Chromatography (Waters 2695, 2998 PDA detector)

2. Analysis Conditions

(1) column: C18, 4.6*250 mm, 5 μm(2) flow: 1 ml/min(3) injection volume: 10 μl(4) detection: 327 nm (rosmarinic acid), 323 nm (caffeic acid)(5) Mobile phase

TABLE 1Time(min)A(0.1% acetic acid in water)B(acetonitrile)08020403070450100508020608020(6) Standard: rosmarinic acid, caffeic acid

The ingredients of Examples and Comparative Examples shown in Table 2 below were analyzed depending on the analysis conditions, and the results are shown in Table 2 below.

TABLE 2RosmarinicCaffeicExtractionacidacidClassificationSolventRatiomethod(ppm)(ppm)ComparativeWaterImmersion00Example 1extractionComparativeEthanolImmersion165Example 2extractionComparativeWater +20:80Immersion206Example 3ethanolextractionComparativeWater +80:20Immersion00Example 4propanediolextractionExample 1EthanolDropping3010extractionExample 2GlycerinDropping103extractionExample 3ButyleneDropping152GlycolextractionExample 4Water +20:80Dropping5510ethanolextractionExample 5aWater +20:80Dropping203propanediolextractionExample 5bWater +50:50Dropping164propanediolextractionExample 5cWater +80:20Dropping144propanediolextractionExample 6aWater +80:20Dropping236propanediolextractionExample 6bWater +80:20Dropping6010propanediolextraction

Looking at Table 2 above, extraction contents of caffeic acid and rosmarinic acid are higher in the case of performing extraction by the dropping extraction method according to the present disclosure when the same solvent is used if Comparative Examples 2 to 4 using a general immersion extraction method are compared with Examples 1, 4, and 5c using a dropping extraction method according to the present disclosure. Caffeic acid and rosmarinic acid were not extracted in Comparative Example 4 which is the general immersion extraction method, whereas significant amounts of caffeic acid and rosmarinic acid were extracted in Example 5c using the same solvent, and it can be confirmed that the dropping extraction method is a very effective method compared to the general immersion extraction method.

Further, although caffeic acid and rosmarinic acid were not extracted at all in the case of Comparative Example 1 in whichRosmarinus officinalisL. was immersed in water as a solvent and in the case of Comparative Example 4 in which immersion extraction were performed using a solvent having a content of water as the solvent of 80% by weight, it can be confirmed that the dropping extraction method according to the present disclosure is a very effective method considering that significant amounts of caffeic acid and rosmarinic acid were extracted even if the ratios of water were high in Examples 5b and 5c.

Further, looking at Examples 5a to5cin which use amounts of water and alcohols were compared, the contents of caffeic acid were not decreased at all, but rather showed an increasing trend, even if the contents of water were increased.

Furthermore, looking at Examples 6a and 6b in which the extraction step was repeated with respect to the extract extracted in Example 5c, it can be confirmed that the contents of caffeic acid and rosmarinic acid are remarkably increased as the number of extractions is increased.

Therefore, it can be seen that the dropping extraction method according to the present disclosure is very effective in extracting caffeic acid and rosmarinic acid fromRosmarinus officinalisL.

The above description merely exemplarily describes the present disclosure, and a person of ordinary skill in the art to which the present disclosure pertains will be able to understand that the present disclosure may be implemented in a modified form within a range that does not depart from the essential characteristics of the present disclosure. Therefore, the disclosed Examples and Experimental Examples should be considered in an explanatory point of view rather than a limited point of view. The scope of the present disclosure is indicated in the patent claim scope rather than the foregoing description, and all differences within the scope equivalent thereto should be construed as being included in the present disclosure.

EXPLANATION OF MARKS

10: Extractor11: Main body unit12: Filtration membrane13: Dropping unit20: Receiver30: Reservoir100: Extraction apparatus