KR102046164B1 - Method for preparing saussurea involucrata extract using focused ultrasonic treatment, and saussurea involucrata extract obtained therefrom - Google Patents

Abstract

The present invention relates to a method for preparing a Saussurea involucrata extract containing syringin as a physiologically active ingredient in high yield and high purity by using focused ultrasound. In addition, the present invention relates to a Saussurea involucrata extract obtained by the method. The extract contains a high content and high purity of syringin as a physiologically active ingredient, thereby being excellent as a cosmetic ingredient.

Description

METHOD FOR PREPARING SAUSSUREA INVOLUCRATA EXTRACT USING FOCUSED ULTRASONIC TREATMENT, AND SAUSSUREA INVOLUCRATA EXTRACT OBTAINED THEREFROM}

The present invention relates to a method for producing a sulfonylisation extract containing syringin as a physiologically active ingredient in high yield and high purity by using focused ultrasound. In addition, the present invention relates to a snow softened extract obtained according to the above method, the extract contains a high content and high purity of a syringe as a physiologically active ingredient, it is excellent as a cosmetic.

Siringin (syringin) is also known as Eleutheroside B, and has the following formula.

Sirinjin has been proved through various studies to anti-inflammatory, anti-tumor, energy-enhancing, anti-aging and improving vision and hearing, Korean Patent No. 10-0214883 "Pharmaceutical composition of sirin with liver function protection" Syringin is recognized as a valuable treatment in medicine. In addition, it is used in cosmetics, foods, and the like, as a syringe contains an active ingredient for strengthening bio-resistance through fatigue recovery.

On the other hand, with increasing interest in health and beauty, consumers have increased their preference for products containing natural extracts as ingredients rather than synthetic products. As described above, sirin, which can act as a bioactive component, is known to be contained in snow softening. Therefore, the sulfonylisation extract containing sirin is highly useful as a raw material for cosmetics, foodstuffs, and pharmaceuticals.

Accordingly, the need for a method of preparing an extract containing a large amount of a bioactive component from a small amount of natural products is greatly increased in the art.

The widely used methods for extracting natural products include hot water extraction, hot water extraction to elute the active ingredients contained in natural products, solvent extraction using alcohols and solvents to dissolve and separate the active ingredients in solid or liquid samples. Supercritical extraction using a critical fluid. However, due to low yield or high temperature heat applied to natural products, bioactive components are destroyed or denatured, or organic solvents remaining after extraction do not satisfy the degree of safety suitable for use in human cosmetics. Problems exist.

In addition, as a method used for extracting natural products, a method of extracting using ultrasonic waves is also disclosed. For example, Korean Unexamined Patent Publication No. 10-2014-0031662 (2014.03.13) discloses a method for preparing red ginseng extract of an organic saponin component, and extracts red ginseng residue after heating red ginseng at high temperature for 4 to 6 times. And adding the organic acid mixed with citric acid and succinic acid and aging, and extracting while giving ultrasonic vibration and microbubbles.

As such, a method of extracting using ultrasonic waves is already known. However, if an organic solvent is used in the extraction process, it is impossible to completely remove the organic solvent from the final product extract, and thus the organic solvent remaining in the extract does not meet the criteria for use as a cosmetic for application to human skin. In addition, when water is used as the extraction solvent without using the organic solvent, the yield is significantly reduced.

In particular, natural extracts vary greatly in the extraction yield and the content of physiologically active ingredients depending on which plant is the raw material, so even if the extraction method is effective for a specific plant, the same or similar level of effect may be applied to other plants. In most cases it does not represent.

Korean Patent Publication No. 10-1998-0072707 (1998.11.05) Korean Patent Publication No. 10-2014-0031662 (2014.03.13)

The present inventors have recognized the problems of the prior art, and went through a number of trials and errors to find a method for producing a snow softened extract containing a high content of the physiologically active sirin. As a result, even when water is used as a solvent, it proved the specific conditions to prepare a sulfonylisation extract containing a bioactive component in a significantly high yield and came to complete the present invention.

According to one aspect of the present invention, the present invention provides a method for preparing a sulfonated extract, comprising the following steps:

a) mixing snow softening with a water solvent;

b) sonicating the mixture obtained in step a); And

c) irradiating focused ultrasound to the mixture sonicated in the step b);

The snow softening extract is a manufacturing method comprising a syringe (syringin) as a bioactive component.

The sulyeonhwa (Saussurea involucrata) is a perennial herb belonging to the chrysanthemum (compositae) family, the sulyeonhwa used as herbal medicine includes cannonsulyeon softening, sulphyeon softening, sclerol softening. It has been reported that the snow softening has an effect of inhibiting the growth of melanocytes and exhibits whitening activity, and also has the potential to be used as an antioxidant, an anti-fatigue agent, an anti-aging agent, a skin neuroprotective agent and a skin immune protective agent. Reported.

Snow softening includes flavonoids, alkanoids and the like, such as syringes and rutin, and has been reported to have antioxidant, anti-fatigue, anti-aging, neuroprotective and skin immune effects. In addition, research results have been reported that the extract of sulphylated extract has the effect of inhibiting the growth of melanocytes (Qing Mu et al., (2007) .Inhibitory Effects of Saussurea involucrata. Against Melanogenesis of Mouse-Derived Melanocyte Cells).

Each step of the method for producing a sulfonylisation extract containing a large amount of the physiologically active ingredient of serine jinjeol by using focused ultrasound according to the present invention will be described in detail.

In the production process according to the invention, step a) is a step of sulfidation and mixing of the solvent.

In the manufacturing method according to the present invention, snow softening may be prepared by pulverizing before step a), and may be used by purchasing a prototype that is already prepared in powder form.

In the preparation method according to the present invention, the solvent is water. Preferably, organic solvents such as methanol, ethanol, hexane, chloroform, ethyl acetate and the like are excluded from the preparation method according to the present invention.

It is common to use an organic solvent as the extraction solvent to achieve higher extraction yield of the active ingredient than to use water. In particular, snow softening has a problem that the syringe is destroyed when using the hot water extraction method in the extract preparation, it is common to extract with an organic solvent at room temperature. However, since the sulfonylisation extract according to the present invention has a purpose for use in cosmetics, it excludes the use of an organic solvent in the extraction process and water is used as the only extraction solvent. The organic solvent may cause denaturation of the bioactive component in the sulfidation in the course of extraction, or may be reacted with a component of the sulfidation to produce an adduct, or may be derived from the organic solvent or derived from the extract obtained as a final product. Because the remaining substances remain, the extract obtained as the final product does not meet the criteria for use in cosmetics. If the final product obtained by the organic solvent extraction method is used as a cosmetic, an additional step is required to prove that there is no harmful substance to the human body in the final product, or a tablet which completely removes the harmful substance to the human body from the final product. Since further steps are required, it is disadvantageous in terms of the efficiency of the overall process for the production of cosmetics.

The term focused ultrasound used in the present invention is a high intensity focused ultrasound (HIFU, High Intensity Focused Ultrasound) of 1,000 W / cm ² or more according to the focusing area intensity and low intensity focused ultrasound in the range of 10 mW / cm ² to 50 W / cm ² ( LIFU, Low Intensity Focused Ultrasound). The focused ultrasound used in the method of the present invention is preferably a high intensity focused ultrasound. In particular, the focused ultrasound used in the method of the present invention is more preferably a high intensity focused ultrasound of 1,500 W / cm ³ to 2,000 W / cm ³ . In contrast, the term "ultrasound" refers to sound waves exceeding 20kHz in the audible range of human hearing.

As shown in the following examples, the present inventors performed an experiment to compare the yield of the bioactive components when using high-intensity focused ultrasound at room temperature and the yield of the bioactive components when using general ultrasonic waves. As a result, the yield of the syringin was significantly increased when the sulfonated extract was prepared according to the method of the present invention, while the non-syringin inactive ingredients were removed in a larger amount, thereby increasing the purity of the bioactive component in the final product.

In analyzing the rationale for obtaining these results without being bound by a particular theory, focused ultrasound is a symptom contained in sulfonylation by a complex action that stimulates the cell walls of sulfonylation to increase activity and increase solvent fluidity. It is believed that the gin component can be separated more easily.

The focused ultrasound apparatus used in the method according to the present invention includes an ultrasound generating module capable of generating focused ultrasound having a focus at a specific position, the ultrasound generating module including an ultrasonic transducer having an elliptical oscillator.

Preferably, the focused ultrasound apparatus may include a sulfidation-containing solution in order to prevent the temperature of the medium from increasing and the bioactive component of the sulfidation from being destroyed or denatured as the focused ultrasound is focused on a specific position and the focused ultrasound is irradiated. It is possible to have a device for continuously stirring. The stirring device may be, for example, a stirring blade.

Preferably, the focused ultrasound device may be equipped with a cooling device so as to be able to maintain a certain range of temperatures when the method according to the invention is carried out. The cooling device suppresses the temperature rise of the medium by ultrasonic waves or focused ultrasonic waves.

Specific examples of the focused ultrasound device are shown in FIGS. 1 to 7, but are not limited to the devices shown in these drawings.

1 is an example of a focused ultrasound device. As shown in FIG. 1, the ultrasonic processing apparatus 100 includes a processing container 102 in which raw materials to be ultrasonicated are stored, and an ultrasonic wave generating module for irradiating focused ultrasound having a focus on a specific position of the processing container 102 ( 110). For convenience of understanding in FIG. 1, the processing container 102, the ultrasonic wave generating module 110, and the like are shown in cross-sectional view. The ultrasonic wave generating module 110 includes an ultrasonic transducer 116, a cartridge housing 112, an ultrasonic medium 113, and the like. The ultrasonic transducer 116 is provided with an ellipsoidal oscillator 117 to generate focused ultrasound. An ultrasonic transducer 116 is installed inside the cartridge housing 112. The cartridge housing 112 has an opening formed at a lower portion thereof, and a cartridge window 114 for transmitting ultrasonic waves is attached to the opening. The ultrasonic medium 113 is filled inside the cartridge housing 112 and delivers the ultrasonic waves generated by the ultrasonic transducer 116 to the cartridge window 114. In the processing container 102, a coupling part 104 in which the ultrasonic wave generating module 110 is detachably mounted is installed, and the raw material to be ultrasonicated is stored. The ultrasonic wave generation module 110 irradiates focused ultrasound to extract physiologically active components from natural product snow softening stored in the processing container 102. A moving mechanism 118 for moving the ultrasonic transducer 116 is installed inside the ultrasonic wave generating module 110 so that the focused ultrasound can be evenly irradiated to the raw material stored in the processing container 102, or the processing container 102 is provided. A raw material flow device (not shown) that transmits and shakes vibrations to the raw materials therein is installed in the processing container 102. The ultrasonic wave generating module 110 is installed such that the cartridge window 114 through which ultrasonic waves pass is in contact with the water surface of the raw material 103 or partially immersed in the raw material. Therefore, the ultrasonic waves generated by the ultrasonic wave generation module 110 are irradiated onto the raw material 103 without passing through the air. The cartridge window 114 is a film of translucent or transparent material that can transmit ultrasonic waves. In this embodiment, the cartridge window 114 may be a Kapton film or another material known to smoothly pass ultrasonic waves. The moving mechanism 118 moves the ultrasonic transducer 116 so that the focused ultrasound generated by the ultrasonic transducer 116 is evenly irradiated to the raw material 103 in the processing container 102. The moving mechanism 118 includes an X axis moving part 118a for moving the ultrasonic transducer 116 in the X axis direction, a Y axis moving part 118b for moving in the Y axis direction, and a Z axis moving for moving in the Z axis direction. It consists of a part 118c. The moving mechanism 118 is configured so that the ultrasonic transducer 116 performs linear movement along the X / Y / Z axis, but the ultrasonic transducer 116 may be configured to move in various forms such as pivot movement, clock movement, spiral movement, and the like. . The moving mechanism 118 is located inside the cartridge housing 112 and is configured to be connected to the ultrasonic transducer 116 to move the ultrasonic transducer 116, but the moving mechanism 118 is the cartridge housing 112. It may be configured to move the cartridge housing 112 to the outside of the. In addition, a raw material flow device (not shown) may be provided to shake the raw material in the processing container 102 so that the focused ultrasound can be evenly irradiated onto the raw material. The raw material flow device may be configured such that the processing vessel 102 performs a clockwise movement, a rotary movement, and the like. In addition, a stirring blade (not shown) for stirring the raw material may be provided in the processing container 102. When the focused ultrasound is irradiated to the raw material 103 in the processing container 102, the temperature of the raw material 103 may rise to generate gas. A gas outlet (not shown) may be formed in the coupling part 104 to discharge the gas. When the ultrasonic wave generating module 110 generates focused ultrasound for a long time, the temperature of the ultrasonic medium 113 is increased, and thus, a cooling mechanism for cooling the ultrasonic medium 113 is required. The medium cooling mechanism is inserted into the cartridge housing 112 into a metal plate 120 in contact with the ultrasonic medium 113 and a heat sink 122 for dissipating heat transferred through the metal plate 120 into the air. It is composed. Peltier elements may be used in place of the heat sink 122. Raw material containers 130, 132, 134 may be further provided. The raw material containers 130 and 132 store raw materials before ultrasonication. The raw material container 134 stores raw materials after ultrasonication. The raw material container 130 is connected to the raw material inlet 137 of the processing container 102 through the transfer pipe 136, and the raw material transfer through the transfer pipe 136 is controlled through the opening / closing valve 144. The raw material container 132 is connected to the raw material inlet 139 of the processing container 102 through the transfer pipe 138, and the raw material transfer through the transfer pipe 138 is controlled through the opening / closing valve 146. The raw material container 134 is connected to the raw material outlet 141 of the processing container 102 through the transfer pipe 140, and the raw material transfer through the transfer pipe 140 is controlled through the opening / closing valve 148. The raw material container 130 and the raw material container 134 are connected through the transfer pipe 142, and the raw material transfer through the transfer pipe 142 is controlled through the opening / closing valve 150. The raw materials stored in the raw material containers 130 and 132 are transferred into the processing container 102 through a pump (not shown) with the open / close valves 144 and 146 open for ultrasonic processing. The raw material ultrasonicated in the processing container 102 is transferred to the raw material container 134 by opening and closing the valve 148. If it is not necessary to perform the ultrasonic treatment repeatedly, once the ultrasonic treatment is not sufficient, the opening and closing valve 150 is opened so that the raw material stored in the raw material container 134 after the ultrasonic treatment to the transfer pipe 142 Transfer to the raw material container 130 through. The raw material transferred to the raw material container 130 is transferred to the processing container 102 through the transfer pipe 136 and ultrasonicated again. That is, the raw material is circulated in the order of the raw material container 134, the transfer pipe 142, the raw material container 130, the processing container 102. In the present embodiment, since the ultrasonic transducer 116 does not directly contact the raw material in the processing container 102, it is possible to suppress generation of harmful components during ultrasonic processing. The focused ultrasound can be uniformly irradiated to the raw material stably stored in the processing container 102 through the moving mechanism 118.

2 is another example of a focused ultrasound device. As illustrated in FIG. 2, the ultrasonic processing apparatus 200 includes a processing container 202 in which raw materials to be ultrasonicated are stored, and an ultrasonic wave generating module for irradiating focused ultrasound having a focus on a specific position of the processing container 202 ( 210. The ultrasonic processing apparatus 200 is different from the ultrasonic processing apparatus 100 shown in FIG. 1 in that the ultrasonic generating module 210 is located below the processing container 202. The ultrasonic wave generating module 210 includes an ultrasonic transducer 216, a cartridge housing 212, an ultrasonic medium 213, and the like. The ultrasonic transducer 216 includes an ellipsoidal oscillator 217 to generate focused ultrasound. An ultrasonic transducer 216 is installed inside the cartridge housing 212, and an opening is formed at an upper portion thereof, and a cartridge window 214 is attached to the opening. The ultrasonic medium 213 fills the interior of the cartridge housing 212 and delivers the ultrasonic waves generated by the ultrasonic transducer 216 to the cartridge window 214. A moving mechanism 218 for moving the ultrasonic transducer 216 is installed in the ultrasonic wave generation module 210 or the raw material in the processing container 202 so that the focused ultrasound can be evenly irradiated to the raw material stored in the processing container 202. A raw material flow device (not shown) that transmits and shakes vibrations is installed in the processing container 202. A coupling part 204 is formed to detachably mount the processing container 202 to the ultrasonic wave generating module 210. The bottom surface of the processing container 202 is provided with a container window 206 through which ultrasonic waves pass. Since the ultrasonic wave generating module 210 is installed to face upward, sag may occur in the cartridge window 214, and a gap may be formed between the cartridge window 214 and the container window 206. When a gap is formed between the windows 206 and 214, ultrasonic waves cannot be delivered in the air and a large loss occurs. To prevent this phenomenon, a medium capable of transmitting ultrasonic waves is filled between the windows 206 and 214. Alternatively, the container window 206 is formed of a film material in which sagging occurs due to the load of the raw material filled in the processing container 202 and is in close contact with the cartridge window 214. That is, the container window 206 is formed by the film material to be in close contact with the cartridge window 214 where the deflection is similar, so that no empty space is formed between the windows 206 and 214. Since the ultrasonic generation module 210 cannot be completely filled with the ultrasonic medium, the cartridge housing 212 may be configured such that the cartridge window 214 is positioned lower than the normal water surface of the ultrasonic medium 213 in the cartridge housing 212. There is a need. To this end, the cartridge housing 212 forms an air pocket 226 such that the upper periphery 225 has a step compared to the cartridge window 214. The moving mechanism 218 moves the ultrasonic transducer 216 so that the focused ultrasound generated by the ultrasonic transducer 216 is evenly irradiated to the raw material in the storage container 202. In this embodiment, the moving mechanism 218 moves in the X-axis direction, the X-axis moving part 218a for moving the ultrasonic transducer 216 in the X-axis direction, the Y-axis moving part 218b for moving in the Y-axis direction, and moving in the Z-axis direction. It consists of the Z-axis moving part 218c. A raw material flow device (not shown) may be provided to shake the raw material in the processing container 202 so that the focused ultrasound can be evenly irradiated onto the raw material. The raw material flow device may be configured such that the processing vessel 202 performs a clockwise movement, a rotational movement, and the like. In addition, a stirring blade (not shown) for stirring the raw material may be provided inside the processing container 202. When focused ultrasound is irradiated to the raw material in the processing container 202, the temperature of the raw material may rise and gas may be generated. A gas discharge port 252 may be formed in the upper portion of the processing container 202 to discharge the gas. In addition, the gas outlet 252 may be provided with a check valve 254 that opens at a pressure of a predetermined size or more. When the ultrasonic wave generating module 210 generates focused ultrasound for a long time, the temperature of the ultrasonic medium 213 is increased, and thus a cooling mechanism for cooling the ultrasonic medium 213 is required. In this embodiment, the medium cooling mechanism is a metal plate 220 inserted into the cartridge housing 112 and in contact with the ultrasonic medium 113, and a heat sink 222 for dissipating heat transferred through the metal plate 220 into the air. It is composed. A Peltier element may be used instead of the heat sink 222. Raw material containers 230, 232, and 234 may be further provided. The raw material containers 230 and 232 store raw materials before ultrasonication. The raw material container 234 stores raw materials after ultrasonication. The raw material container 230 is connected to the raw material inlet 237 of the processing container 202 through the transfer pipe 236, and the raw material transfer through the transfer pipe 236 is controlled through the opening / closing valve 244. The raw material container 232 is connected to the raw material inlet 239 of the processing container 202 through the transfer pipe 238, and the raw material transfer through the transfer pipe 238 is controlled through the open / close valve 246. The raw material container 234 is connected to the raw material outlet 241 of the processing container 202 through the transfer pipe 240, and the raw material transfer through the transfer pipe 240 is controlled through the open / close valve 248. The raw material container 230 and the raw material container 234 are connected through the transfer pipe 242, and the raw material transfer through the transfer pipe 242 is controlled through the opening / closing valve 250. In this embodiment, since the ultrasonic transducer 216 is not in direct contact with the raw material in the processing container 202, it is possible to suppress the generation of harmful components during the ultrasonic processing. In addition, since it is easy to separate the ultrasonic wave generating module 210 from the processing container 202, it is easy to replace the ultrasonic transducer 216. In addition, in the present embodiment, the focused ultrasonic waves may be uniformly irradiated to the raw material stably stored in the processing container 202 through the moving mechanism 218.

3 is another example of a focused ultrasound device. As illustrated in FIG. 3, the ultrasonic processing apparatus 300 includes an ultrasonic wave generating module for irradiating focused ultrasonic waves having a focus on a processing container 202 and a specific position of the processing container 302 in which the raw material to be ultrasonicated is stored ( 310). The ultrasonic wave generating module 310 includes an ultrasonic transducer 316, a cartridge housing 312, an ultrasonic medium 313, and the like. The cartridge housing 312 has a cartridge window 314 formed thereon. The ultrasonic medium 313 fills the interior of the cartridge housing 312 and delivers the ultrasonic waves generated by the ultrasonic transducer 316 to the cartridge window 214. The focus of the ultrasonic wave generating module 310 is that the transducer 316 is aligned with the bottom surface of the processing container 302, that is, near the top surface of the container window 306. An isolation chamber 370 is installed at the bottom of the processing container 302. The isolation chamber 370 has a window through which ultrasonic waves pass. In this embodiment, since the ultrasonic wave generating module 310 is located below the processing container 302, a window is formed at the bottom of the isolation chamber. The focal point of the ultrasonic wave generating module 310 is aligned with the interior of the isolation chamber 370. The isolation chamber 370 includes an inlet 372 through which the raw material flows from the processing container 302, and an outlet 374 through which the raw material flows into the processing container 302. The inlet 372 is provided with an inlet door 376 that opens into the isolation chamber 370, and the outlet 374 is provided with an outlet door 378 that opens to the outside of the isolation chamber 370. In the vicinity of the inflow door 376 or the outflow door 378, raw material conveying fans 380 and 382 may be installed to flow the raw material. The raw materials in the processing container 302 are introduced into the isolation chamber 370 through the inlet 372 by the operations of the raw material conveying fans 380 and 382. The raw material introduced into the isolation chamber 370 is processed by the focused ultrasound while being transported along the isolation chamber, and flows out through the outlet 374. When the focused ultrasound is irradiated to the raw material in the processing container 302, the temperature of the raw material may rise and gas may be generated. A gas discharge port 352 may be formed at an upper portion of the processing container 302 to discharge the gas. In addition, the gas outlet 352 may be provided with a check valve 354 that opens at a pressure of a predetermined size or more. In the present embodiment, the isolation chamber 370 is provided, and the raw material 303 in the processing container 302 is transferred to the isolation chamber 370 and subjected to ultrasonic treatment, whereby the ultrasonic wave can be irradiated more uniformly to the raw material 303.

4 is another example of a focused ultrasound device. As shown in FIG. 4, the ultrasonic processing apparatus 400 includes a processing container 402 in which raw materials to be ultrasonicated are stored, and an ultrasonic wave generating module for irradiating focused ultrasound having a focus on a specific position of the processing container 202 ( 410. The ultrasonic wave generation module 410 includes ultrasonic transducers 416a, 416b, and 416c, an ultrasonic medium 413, and a main housing 411. The ultrasonic medium 413 fills the interior of the main housing 412 and delivers the ultrasonic waves generated by the ultrasonic transducers 416a, 416b, 416c. A moving mechanism 418 for moving the ultrasonic transducers 416a, 416b, and 416c is installed in the ultrasonic wave generating module 410 so that the focused ultrasonic waves can be evenly irradiated to the raw material stored in the processing container 402. An opening is formed in an upper surface of the main housing 412. One end of the inclination adjustment columns 464a and 464b supports the bottom surface of the processing container 402. The inclination adjustment parts 462a and 462b can adjust the inclination of the bottom surface of the processing container 402 with respect to the ground by adjusting the heights of the inclination adjustment columns 464a and 464b. As shown in FIG. 4, when the left side of the bottom surface of the processing container 402 is higher than the right side, the raw material moves from left to right along the bottom surface, so that the raw material is transferred in the processing container 402. There is no need to provide a separate mechanism. The bottom of the processing container 402 is provided with a container window 406 through which ultrasonic waves pass. The processing vessel 402 is installed in the opening of the main housing 412 and the vessel window 406 is immersed in the ultrasonic medium 413. If the bottom surface of the processing vessel 402 is inclined with respect to the ground, the raw material does not accumulate on the bottom surface of the processing vessel 402 and flows along the inclined surface, so the focus of the ultrasonic transducers 416a, 416b, and 416c is located directly above the inclined surface. It is desirable to. The plurality of ultrasonic transducers 416a, 416b, and 416c may be disposed along the inclined surface such that the same raw material is irradiated to the ultrasonic wave several times. Raw material containers 430, 432, and 434 may be further provided. The raw material containers 430 and 432 store raw materials before ultrasonication. The raw material container 434 stores raw materials after ultrasonication. The raw material container 430 is connected to the raw material inlet 437 of the processing container 402 through the transfer pipe 436, and the raw material transfer through the transfer pipe 436 is controlled through the opening / closing valve 444. The raw material container 432 is connected to the raw material inlet 439 of the processing container 402 through the transfer pipe 438, and the raw material transfer through the transfer pipe 438 is controlled through the opening / closing valve 446. The raw material container 434 is connected to the raw material outlet 441 of the processing container 402 through the transfer pipe 440, and the raw material transfer through the transfer pipe 440 is controlled through the opening / closing valve 448. The raw material container 430 and the raw material container 434 are connected through the transfer pipe 442, and the raw material transfer through the transfer pipe 442 is controlled through the opening / closing valve 450. With respect to the delivery tube 436, the delivery tube 438 is connected to the same side of the processing vessel 402 and the delivery tube 440 is connected to the opposite side. That is, the raw material inlets 470 and 472 are formed on the same side of the processing container 402, and the raw material outlet 474 is formed on the opposite side. The guide member 474 is further provided so that the raw material injected through the raw material injection holes 470 and 472 flows down the wall instead of directly falling to the bottom surface of the processing container 402.

FIG. 5 is another example of the focused ultrasound apparatus, and FIG. 5A is a configuration diagram of the ultrasonic processing apparatus 500, and FIG. 5B is a configuration diagram of the ultrasonic generation module 504 used in the ultrasonic processing apparatus 500. As illustrated in FIG. 5A, the ultrasonic processing apparatus 500 includes a processing container 502 in which raw materials to be ultrasonicated are stored, and an ultrasonic wave generating module for irradiating focused ultrasound having a focus on a specific position of the processing container 502 ( 504 and an ultrasonic reflection member 510. The ultrasonic reflective member 510 includes an ultrasonic transducer 516, a cartridge housing 512, an ultrasonic medium 513, and the like. The cartridge housing 512 has a cartridge window 514 formed at the bottom thereof, and an ultrasonic transducer 516 is installed therein. The ultrasonic medium 513 fills the interior of the cartridge housing 512 and delivers the ultrasonic waves generated by the ultrasonic transducer 516 to the cartridge window 514. A moving mechanism 506 is provided to move the ultrasonic wave generation module 504 so that the focused ultrasound can be evenly irradiated to the raw material stored in the processing container 502. In the ultrasonic processing apparatus 500, at least a part of the ultrasonic wave generating module 504 is moved by the moving mechanism 506 in a state of being immersed in the raw material inside the processing container 502. The ultrasonic reflection member 510 is connected to and installed in the ultrasonic generation module 504. The ultrasonic reflection member 510 moves together with the ultrasonic wave generation module 504 and is located in the ultrasonic irradiation direction of the ultrasonic wave generation module 504 to reflect the ultrasonic waves past the focus of the focused ultrasonic wave in the opposite direction. The ultrasonic reflection member 510 may be formed in a “c” shape. The ultrasonic reflection member 510 is installed so that one surface thereof faces in the irradiation direction of the ultrasonic waves to reflect the ultrasonic waves. The ultrasonic reflection member 510 allows the ultrasonic waves to be more uniformly irradiated into the raw material. The stirring unit 508 is installed outside the ultrasonic wave generating module 504. The stirring unit 508 mixes the raw materials when the ultrasonic wave generating module 504 is moved by the moving mechanism 506 so that ultrasonic waves are uniformly irradiated onto the raw materials. As shown in FIG. 5B, the ultrasonic wave generating module 504 is connected by the moving mechanism 506 through the moving shaft 518, and the stirring unit 508 is installed to protrude outside the ultrasonic wave generating module 504. do. The stirring parts 508a, 508b, 508c, and 508d are radially symmetrically installed with respect to the ultrasonic wave generating module 504, and may have different directions of a spoon-shaped end portion. In this embodiment, since the ultrasonic generating module 504 is moved by the moving mechanism 506 while a part of the ultrasonic generating module 504 is locked to the raw material inside the processing container 502, the ultrasonic generating module 504 is the processing container. A function of stirring the raw material in 502 is performed. Therefore, the ultrasonic processing apparatus 500 can uniformly irradiate ultrasonic waves to a raw material with a simple structure.

6 is another example of a focused ultrasound device. As illustrated in FIG. 6, the ultrasonic processing apparatus 600 includes a processing container 602 for storing raw materials to be ultrasonicated, and an ultrasonic wave generating module 604 for generating focused ultrasound. The ultrasonic processing apparatus 600 is provided with the raw material raising / lowering mechanism 606 which moves the processing container 602 up / down. In addition, the ultrasonic processing apparatus 600 further includes a support 608 for supporting the processing container 602 and the ultrasonic wave generating module 604. The support 608 includes a base portion 610 in which the processing container 602 is positioned at an upper portion thereof, and a support portion 612 standing on one side of the base portion 610 to support the ultrasonic wave generating module 604. A moving wheel 614 is installed below the base part 610. The support part 612 is provided with an ultrasonic moving mechanism 616 for moving the ultrasonic wave generating module 604. The ultrasonic wave generating module 604 is installed to the moving mechanism 616 through the support 626. A stirring member 618 is further provided for stirring the raw materials in the processing container 602. The stirring member 618 is rotated by a motor (not shown), has a propeller shape, and a plurality of stirring members 618 may be installed at regular intervals. The stirring member 618 is connected with the ultrasonic wave generating module 604 by the support 624, and moves together when the ultrasonic wave generating module 604 is moved by the moving mechanism 616 to allow the raw materials to be mixed better. The ultrasonic processing apparatus 600 further includes a temperature sensor 620 for sensing the temperature of the raw material in the processing container 602 and a cooling unit 622 for cooling the temperature of the raw material. One example of the cooling unit 622 is installed in the processing vessel 602 to directly cool raw materials stored in the processing vessel 602. The cooling unit 622 may be implemented with, for example, a Peltier element. Another example of the cooling unit 622 is as illustrated in FIG. 1 or 2, while cooling the raw material while transferring the raw material in the processing container 602 to an external storage container through a transfer pipe, and back to the processing container 602. It may consist of injecting.

FIG. 7 is a conceptual diagram of the ultrasonic wave generating module 604 applied to the ultrasonic processing apparatus 600 of FIG. 6. The ultrasonic generating module 604 includes a plurality of ultrasonic transducers 706 in the cartridge housing 702 filled with the ultrasonic medium 704. The plurality of ultrasonic transducers 706 are located at different heights or different radii of curvature of the ultrasonic oscillator have different focal lengths from the cartridge window 708. In addition, the plurality of ultrasonic transducers 706 may generate ultrasonic waves at different intensities. The ultrasonic transducer 706 is located within the cartridge housing 702 and may be installed to irradiate the ultrasonic wave to the upper side or the lower side of the cartridge housing 702. As in the present embodiment, when the ultrasonic transducer 706 irradiates the lower side of the cartridge housing 702, the cartridge window 708 is installed on the lower surface of the cartridge housing 702. When the ultrasonic transducer 706 irradiates ultrasonic waves to the upper side of the cartridge housing 702, the cartridge window is installed on the upper surface of the cartridge housing 702. The ultrasonic wave generation module 604 supplies power to the plurality of ultrasonic transducers 706 through the power line 708 and a control signal from a controller (not shown) through the control line 710. Further comprising a medium circulation line 714 capable of circulating the ultrasonic medium 703 in the cartridge housing 702, the medium circulation line 714 is provided with a temperature sensor 712 for measuring the temperature of the ultrasonic medium. . The medium circulation line 714 may be configured by tying the power line 708 and the control line 710 into one cable form. The medium circulation line 714 receives temperature information from the temperature sensor 712, and when the medium inside the cartridge housing 702 is heated above a predetermined temperature by ultrasonic waves, the medium is circulated to the outside to appropriately adjust the temperature of the medium. Keep at temperature. The ultrasonic generation module 604 is located in the cartridge housing 702 and further includes a check valve 716. The check valve 716 discharges gas generated inside the cartridge housing 702. The ultrasonic medium can be heated by ultrasonic waves to produce a gas. The gas will be present as bubbles inside the cartridge housing 702, thus preventing the transmission of ultrasonic waves.

In the process according to the invention, in the step a) sulpholic and water are mixed in a weight ratio of 1:10 to 1:20. Preferably, the weight ratio is 1:13 to 1:17. Most preferably, the weight ratio is 1:15, in which the sulfidation is best mixed without being immersed in the solvent, and the focused ultrasound is irradiated to the cell walls of the sulfidation so that the bioactive component is best eluted. .

In the method according to the invention, the ultrasound in step b) is preferably ultrasound ranging from 10 mW / cm ² to 50 W / cm ² . Ultrasound in step b) is believed to play a role in stimulating the cell wall of sulphation, and in subsequent step c), creating an environment in which the bioactive component can be more easily eluted when focused ultrasound is irradiated.

In the method according to the invention, the steps b) and c) are preferably performed at room temperature, respectively. The normal temperature is preferably a temperature of 15 ° C to 40 ° C, more preferably 27 ° C to 36 ° C. Thus, the process according to the invention does not require a special heating process, so that the time and cost of the whole extraction process is economical. In addition, the application of heat to a temperature exceeding room temperature may increase the extraction yield or shorten the extraction process time, but raw materials such as plants or natural products, in particular, bioactive components contained therein generally There is an important problem that it is denatured. Therefore, carrying out the steps b) and c) at room temperature is very advantageous in terms of yield and purity and in terms of the integrity of the bioactive components in the final product compared to other processes requiring heat above room temperature.

In the method according to the present invention, a separate device such as a cooling device may be necessary to perform the steps b) and c) at room temperature. Irradiation with ultrasound or focused ultrasound often raises the temperature of the medium, which must be kept within a certain range.

In the method according to the present invention, step b) may be performed for 3 to 7 hours. In terms of the yield and purity of the bioactive components of the final product and the efficiency and productivity of the entire extraction process, the most preferred time is about 5 hours.

In the method according to the invention, step c) may be performed for 10 to 20 hours. The most preferred time in terms of yield and purity of the bioactive components of the final product and the efficiency and productivity of the overall extraction process is about 15 hours.

According to another aspect of the invention, between the steps b) and c), further comprising the step of aging at low temperatures, respectively. It is preferable that the said low temperature is the temperature of 1 degreeC-5 degreeC. More preferably, the low temperature is 3 ° C to 4 ° C. The additional step may be carried out for 15 to 25 hours each. The most preferred time in terms of yield and purity of the bioactive components of the final product and the efficiency and productivity of the overall extraction process is about 19 hours.

As used herein, the term "maturation" refers to placing at a low temperature after irradiation with ultrasound or focused ultrasound, which increases the yield and purity of the bioactive component in the final product, and increases the integrity of the bioactive component It seems to work.

The preparation method of the sulfonylisation extract according to the present invention significantly increases the yield and purity of the bioactive component of the syringin extract, which is contained in the sulfonylisation extract, which is the final product, compared to other hydrothermal extraction methods, organic solvent extraction methods, and ultrasonic extraction methods.

In particular, since the whole extraction process is not performed at a temperature exceeding room temperature, there is no possibility that the sulfonated extract or its physiologically active component is destroyed or denatured by a temperature or heat exceeding the room temperature, so The integrity of the physiologically active ingredient sirine component is maintained.

Moreover, the solvent used in the whole extraction process is water and excludes the use of an organic solvent, it can easily meet the conditions required as a cosmetic used for human skin. In other words, when an organic solvent other than water is used in some of the extraction processes, it is necessary to confirm whether the organic solvent remains in the final product, and the organic solvent reacts with the bioactive and / or other components of the sulfonated extract. To determine whether by-products or impurities have been produced. If organic solvents, by-products or impurities are included in the final product and are difficult to use as cosmetics or do not meet the criteria, further purification steps are necessary.

In addition, the method according to the invention takes significantly less overall process time and cost than other methods. Therefore, it can be ensured by the method according to the present invention to extract a large amount of snow softened extract containing a high content and high purity of a syringe ingredient as a cosmetic.

As described above, the sulfonylised extract obtained by the method according to the present invention contains a high content and high purity of sirin as a physiologically active ingredient, and thus has excellent utility as a cosmetic.

1 to 7 show examples of focused ultrasound devices that can be used in the method according to the invention.
8 shows the results of HPLC analysis of the snow softened extract prepared in Example 1. FIG.
9 shows the result of HPLC analysis of the sulfonated extract prepared in Comparative Example 1.

Hereinafter, the present invention will be described in more detail with reference to Examples. However, these examples are for illustrative purposes only, and the scope of the present invention is not limited by these examples. It is also to be understood that the terms not specifically defined herein have a meaning commonly used in the technical field to which the present invention belongs.

Example 1

100 g of dried snow softened water was washed with purified water and then pulverized and added to 1.5 L of distilled water. The snow softening used here was specifically the snow softening bud site. The obtained snow softening solution was sonicated at 27 ° C. for 5 hours. Then it was cooled to 4 ° C. and aged for 19 h.

Thereafter, 1800 W / cm ² focused ultrasound generated through the ellipsoidal oscillator provided in the ultrasonic transducer of FIG. 1 was irradiated to the aged snow softening mixture at 27 ° C. for 15 hours. At this time, the sulfidation solution was continuously stirred so that the focused ultrasound was uniformly irradiated over the entire sulfidation solution.

The resulting snow softening solution was filtered and concentrated using a 75 micron (45 × 40 cm) filter (manufacturer: CRAFT BREW HERO) to prepare a snow softening extract having a final concentration of 1 mg / ml.

Comparative Example 1

100 g of dried snow softened water was washed with purified water and then pulverized and added to 1.5 L of distilled water. The obtained snow softening solution was extracted with hot water at 80 to 90 ° C. for 20 hours with occasional stirring.

The resulting snow softening solution was filtered and concentrated using a 75 Micron (45 × 40 cm) filter (manufacturer: CRAFT BREW HERO) to prepare a snow softening extract having a final concentration of 1 mg / ml.

Comparative Example 2

100 g of dried snow softened water was washed with purified water and then pulverized and added to 1.5 L of distilled water. The obtained snow softening solution was sonicated at 27 ° C. for 5 hours. In Comparative Example 2, ultrasonic waves of 500 W / cm ³ to 700 W / cm ³ were used. Then it was cooled to 4 ° C. and aged for 19 h.

The aged snow softening mixture was then sonicated from 500 W / cm ³ to 700 W / cm ³ at 27 ° C. for 15 hours.

The resulting snow softening solution was filtered and concentrated using a 75 micron (45 × 40 cm) filter (manufacturer: CRAFT BREW HERO) to prepare a snow softening extract having a final concentration of 1 mg / ml.

Experimental Example 1

For each of the sulfidated extract samples obtained in Example 1 and Comparative Example 1, it was confirmed whether or not the concentration of the syringe content in the extract. To this end, High Performance Liquid Chromatography (HPLC) was performed according to the following parameters.

Column: C18 (5 μm, 4.6 × 250 mm)

Column temperature: 30 ° C

Mobile phase: solvent A (methanol) / solvent B (aqueous 0.3% formic acid in HPLC grade water)

Sample injection volume: 10 μl

Detector: DAD (diode array detector)

Detection wavelength: 270 nm

When performing HPLC, the bioactive component of the sulfonylised extract of Sirin has a RT (Retention Time) value of about 2.7 to 2.8. Based on this, it is possible to confirm the presence or absence and concentration of the syringe of each sample from the peak which can be confirmed by the same RT value.

As shown in FIG. 8, which shows the result of HPLC analysis of the sample of Example 1, the sample prepared according to the focused ultrasound extraction method of the present inventors was able to confirm the sharp and high peak at an RT value of about 2.8 corresponding to the syringe. On the other hand, in Figure 9 showing the HPLC analysis results for the sample prepared according to the hydrothermal extraction method of Comparative Example 1 was observed only a very small peak at about 2.8 RT value.

From the above experimental results, it was proved that the sulfonylised extract prepared by using the focused ultrasound extraction method according to the present invention contained a significant amount of sirin, and also significantly inhibited the destruction of the bioactive component. Proven.

Experimental Example 2

In Example 1, Comparative Example 1 and Comparative Example 2 to the quantitative measurement of the content of the syringe components in the snow softened extract samples are shown in Table 1 below.

sample menstruum Ultrasonic Power (W) Extraction temperature (℃) Content of syringe (%) Example 1 water 1800 27 0.42 ± 0.11 Comparative Example 2 water 500-700 27 0.20 ± 0.06 Comparative Example 1 water - 80-90 0.16 ± 0.02

As can be seen in Table 1, the sulphated extract prepared in Comparative Example 1 according to the hot water extraction method was calculated to contain 0.16 ± 0.02% by weight of the bioactive ingredient sirine.

It was confirmed that the sulfonylisation extract prepared in Comparative Example 2 according to the ultrasonic extraction method contained about 1.25 times more bioactive ingredient sirine than the sulfonylation extract prepared in Comparative Example 1.

According to the method of the present invention using focused ultrasound, the content of the sulphylated extract prepared in Example 1 was about 2.6 times higher than that of Comparative Example 1 using the hydrothermal extraction method. Compared with Comparative Example 2, it was confirmed that the content of the physiologically active ingredient sirine was increased by about 2.1 times. This indicates that the sulphated extract prepared by the focused ultrasound extraction method according to the present invention contains a high content of the physiologically active ingredient serine in comparison with the sulphated extract prepared by the extraction method which has been conventionally used conventionally. In addition, since the focused ultrasonic extraction method according to the present invention uses only water as a solvent without using an organic solvent, it does not need a separate process for removing impurities from the final product, which is advantageous in terms of process productivity and time, and also the final product. The purity of the physiologically active ingredient sirine is high. As described above, the sulfonylised extract prepared by the focused ultrasound extraction method according to the present invention can be used as a component of the cosmetic composition without any special intermediate process, and thus, various applications are possible in the industry. In particular, since the raw material used as a cosmetic is directly subjected to human skin, the necessity of removing impurities such as an organic solvent is very high, and this necessity can be solved by the present invention.

In addition, the focused ultrasonic extraction method according to the present invention, despite the extraction temperature was carried out at a room temperature of 27 ℃ high destruction of physiologically active components appearing due to the high temperature content of the syringe compared to the hot water extraction method performed at a high temperature of 80 to 90 ℃ And very little or no denaturation.

Claims (13)

a) mixing snow softening with a water solvent;
b) sonicating the mixture obtained in step a); And
c) irradiating the high-intensity focused ultrasound of 1,500 W / cm ³ to 2,000 W / cm ³ to the mixture sonicated in step b);
The snow softening extract is a manufacturing method comprising a syringe (syringin) as a bioactive component. The method of claim 1,
The method according to claim 1, further comprising the step of grinding snow softening before step a). The method of claim 1,
C) stir the mixture while irradiating high intensity focused ultrasound of 1,500 W / cm ³ to 2,000 W / cm ³ in step c). The method of claim 1,
In step a) snow softening and water is a manufacturing method, characterized in that mixing in a weight ratio of 1:10 to 1:20. The method of claim 1,
The b) and c) step is characterized in that carried out at a temperature of 15 ℃ to 40 ℃, respectively. The method of claim 1,
The step b) is characterized in that for performing for 3 to 7 hours. The method of claim 1,
The c) step is performed for 10 to 20 hours. The method of claim 1,
And further comprising the step of aging at a temperature of 1 ° C. to 5 ° C. between steps b) and c). The method of claim 8,
The further step of aging at a temperature of 1 ℃ to 5 ℃ is characterized in that carried out for 15 to 25 hours. The method of claim 1,
And further comprising a filtering step after step c). A sulphated extract, prepared according to the method of claim 1, comprising a syringe as a physiologically active ingredient. A cosmetic composition comprising the sulphated extract of claim 11. delete

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