TWI679984B - A method for preparing osmanthus fragrans extracts - Google Patents

Abstract

The invention provides a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is acteoside. Specifically, this type of colchicoside has anti-oxidant, skin maintenance, anti-microbial and anti-inflammatory effects.

Description

Preparation method of osmanthus flower extract

The invention provides a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is acteoside. Specifically, this type of colchicoside has anti-oxidant, skin-care, anti-microbial, and anti-inflammatory effects.

Osmanthus fragrans (Thunb) Lour. Is an evergreen shrub of the family Osmanthus Osmanthus. It has aromatic flowers and can extract its essential oils. It can be used to produce osmanthus extracts. On the other hand, it has the effect of warming the lungs to drink and dispersing cold and analgesic. In medicine, its root or root bark can be used to treat stomach pain, toothache, rheumatism, numbness, and bone and bone pain; its flowers can be used to reduce phlegm, dissipate blood stasis, treat phlegm, cough and asthma, intestinal wind and blood, pimple, hernia, toothache and bad breath ; And its fruit can be used to warm the stomach, Pinggan, Yishen, scattered cold and cure liver and stomach pain.

Lutein, also known as verbascoside, ergoside or verbascoside, is generally obtained from plants such as Rehmannia, Cistanche tubulosa or Psyllium, and Osmanthus fragrans. Lutein is an effective antimicrobial component and is known to have good antibacterial effects on Staphylococcus aureus (Guillermo et al., 1999, Journal of Ethnopharmacology 66 (1): 75-8.), While lucene is also Has a good anti-inflammatory effect (Speranza et al., 2009, Journal of biological regulators and homeostatic agents 23 (3): 189-95.). And colchicoside also has whitening, anti-wrinkle and anti-ultraviolet effects. In addition, studies have pointed out that colchicoside can be used for liver protection or to treat medical effects such as Alzheimer's disease. It can be seen that a large amount of chloroticin is needed for extraction. However, the steps of the existing extraction method are still cumbersome.

The present invention unexpectedly discovered a novel method for preparing cycosides, which can be extracted from osmanthus in large amounts and efficiently.

The purpose of the present invention is to provide a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is prepared by the following steps: (1) mixing osmanthus with water or a first alcohol solution, and then extracting them by boiling or ultrasonic vibration, respectively; (2) after filtering the crude extract solution obtained in step (1) to remove the precipitate, and then concentrating or freeze-drying under reduced pressure to obtain the osmanthus extract, wherein the crude extract solution can also be directly concentrated or frozen under reduced pressure After drying, the Osmanthus fragrans extract was obtained.

In an embodiment of the present invention, the osmanthus osmanthus extract is prepared by the following steps: (1) mixing osmanthus osmanthus with water or a first alcohol solution for boiling or ultrasonic oscillation, respectively, and then extracting the obtained crude extract solution through filtration After removing the precipitate, it was concentrated under reduced pressure to obtain the crude extract. (2) The crude extract of step (1) was reconstituted with water and passed through a chromatography column, and then washed with water and alcohol in order. The solution is extracted, and the extract is collected and concentrated under reduced pressure or freeze-dried to obtain the Osmanthus fragrans extract.

In one aspect, the present invention provides a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is prepared by the following steps: (1) Mixing Osmanthus fragrans with water or a first alcohol solution, respectively, and then extracting them by boiling or ultrasonic vibration. The obtained crude extract solution is filtered to remove the precipitate, and then concentrated under reduced pressure to obtain the crude extract; 2) The crude extract filtrate of step (1) is extracted with a second alcohol solution. The obtained extract solution is filtered to remove the precipitate, and then concentrated under reduced pressure or freeze-dried to obtain the Osmanthus fragrans extract.

In another aspect, the present invention provides a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is prepared by the following steps: (1) after mixing osmanthus with water or a first alcohol solution for boiling or ultrasonic vibration After extraction, the obtained crude extract solution is filtered to remove the precipitate, and then concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of step (1) is extracted with a second alcohol solution, and the obtained After the extract solution is filtered to remove the precipitate, it is then concentrated under reduced pressure to obtain an extract; (3) the extract of step (2) is reconstituted with water and passed to a chromatography column, and sequentially with water and alcohol The osmanthus osmanthus extract is obtained after the quasi-elution solution is subjected to leaching, and the leaching solution is collected and concentrated under reduced pressure or freeze-dried.

In one aspect, in the method for preparing a sweet-scented osmanthus extract provided by the present invention, the first alcohol solution is a 5-95% ethanol solution. In a specific embodiment, the first alcohol solution is a 30-80% ethanol solution.

In one aspect, in the method for preparing a sweet-scented osmanthus extract provided by the present invention, the alcohol extraction solution is a 10-95% ethanol solution. In a specific embodiment, the alcohol extraction solution is a 20-50% ethanol solution. In another specific embodiment, the alcohol-eluted solution is a 30% ethanol solution.

In another aspect, in the method for preparing a sweet-scented osmanthus extract provided by the present invention, the second alcohol solution is a methanol or ethanol solution.

In another aspect, in the method for preparing a sweet-scented osmanthus extract provided by the present invention, the chromatography column is packed with a hydrophobic macroporous polymer, wherein the polymer is copolymerized with crosslinked polystyrene or crosslinked styrene and vinylbenzene Composed of things. In a specific embodiment of the present invention, the polymer is Diaion HP-20.

In one aspect, the present invention provides a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is acteoside.

In one aspect, the present invention provides a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is cycoside and the cycoside is used for preparing anti-oxidation, skin care, anti-microbial and anti-inflammatory Use of efficacy composition. Specifically, this type of colchicoside has whitening, anti-wrinkle and anti-ultraviolet effects.

These and other aspects of the present invention can be made clearer by the description and drawings of the following preferred embodiments; even if there may be changes or modifications therein, without departing from the novel concepts disclosed by the present invention Spirit and scope.

The illustration of the preferred embodiment presented in the present invention is for the purpose of illustrating the present invention. It should be understood that the invention is not limited to the preferred embodiments shown.

FIG. 1 shows the preparation process of the Osmanthus fragrans extract. The dried Osmanthus fragrans extract is first extracted with a 60% ethanol solution, filtered and concentrated under reduced pressure, and then subjected to column chromatography to obtain the Osmanthus fragrans extract.

Figure 2 shows the preparation process of the Osmanthus fragrans extract. The dried Osmanthus fragrans extract is first extracted with a 60% ethanol solution, filtered and concentrated under reduced pressure, followed by extraction with methanol or ethanol, and then column Chromatography to obtain the Osmanthus fragrans extract.

Figure 3 shows the preparation process of the osmanthus osmanthus extract. The dried osmanthus osmanthus is first extracted with a 50% ethanol solution, filtered and concentrated under reduced pressure, followed by extraction with methanol or ethanol, and then subjected to column chromatography to obtain the osmanthus Extracts.

FIG. 4 shows a preparation process of the osmanthus osmanthus extract. The dried osmanthus osmanthus extract is extracted with water, filtered and concentrated under reduced pressure, and then extracted with methanol or ethanol to obtain the osmanthus osmanthus extract.

FIG. 5 shows the preparation process of the osmanthus osmanthus extract. After the dried osmanthus osmanthus is extracted with water, it is directly subjected to column chromatography to obtain the osmanthus osmanthus extract.

Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those who have ordinary knowledge in the field of the present invention.

Unless the context clearly indicates otherwise, as used herein, the singular forms "a", "an" and "the" shall include plural forms including "at least one". Thus, for example, reference to "an ingredient" includes a plurality of such ingredients and equivalents known to those having ordinary knowledge in the field.

The present invention provides a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is prepared by the following steps: (1) mixing the sweet-scented osmanthus powder with water or the first alcohol solution, and then extracting them by boiling or ultrasonic vibration; 2) The crude extract solution obtained in step (1) is filtered to remove the precipitate, and then concentrated under reduced pressure or freeze-dried to obtain the Osmanthus fragrans extract. The crude extract solution can also be directly concentrated under reduced pressure or freeze-dried. Then obtain the Osmanthus fragrans extract.

According to an embodiment of the present invention, the osmanthus osmanthus extract is prepared by the following steps: (1) mixing the osmanthus powder with water or the first alcohol solution for boiling or ultrasonic oscillation, respectively, and then extracting the obtained crude extract solution After removing the precipitate by filtration, it was concentrated under reduced pressure to obtain the crude extract. (2) The crude extract of step (1) was reconstituted with water and passed through a chromatography column, followed by water and alcohol in order. The osmanthus osmanthus extract can be obtained after the quasi-elution solution is subjected to leaching, and the leaching solution is collected and concentrated under reduced pressure or freeze-dried.

According to another embodiment of the present invention, the osmanthus osmanthus extract is prepared by the following steps: (1) mixing the osmanthus powder with water or the first alcohol solution to perform extraction after boiling or ultrasonic vibration, respectively, and the obtained crude extract After the product solution is filtered to remove the precipitate, it is concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of step (1) is extracted with a second alcohol solution, and the resulting extract solution is removed by filtration After the precipitate was concentrated under reduced pressure or freeze-dried, the Osmanthus fragrans extract was obtained.

According to a specific embodiment of the present invention, the osmanthus osmanthus extract is prepared by the following steps: (1) mixing the osmanthus powder with water or the first alcohol solution for boiling or ultrasonic oscillation, respectively, and then extracting the obtained crude extract After the solution was filtered to remove the precipitate, it was concentrated under reduced pressure to obtain the crude extract. (2) The crude extract of step (1) was extracted with a second alcohol solution, and the resulting extract solution was filtered to remove the precipitate. After extracting, it was concentrated under reduced pressure to obtain the extract; (3) After the solution of step (2) is reconstituted with water, it is passed through a chromatography column and washed with water and alcohol extraction solution in sequence. Collect these extraction solutions and concentrate them under reduced pressure or The osmanthus flower extract was obtained after freeze-drying.

In one aspect, in the method for preparing a sweet-scented osmanthus extract provided by the present invention, the first alcohol solution is a 5-95% ethanol solution. In a specific embodiment, the first alcohol solution is a 30-80% ethanol solution.

In one aspect, in the method for preparing a sweet-scented osmanthus extract provided by the present invention, the alcohol extraction solution is a 10-95% ethanol solution. In a specific embodiment, the alcohol extraction solution is a 20-50% ethanol solution. In another specific embodiment, the alcohol-eluted solution is a 30% ethanol solution.

In another aspect, in the method for preparing a sweet-scented osmanthus extract provided by the present invention, the second alcohol solution is a methanol or ethanol solution. In a specific embodiment, the second alcohol solution is a methanol solution.

In another aspect, in the method for preparing a sweet-scented osmanthus extract provided by the present invention, the chromatography column is packed with a hydrophobic macroporous polymer, wherein the polymer is copolymerized with crosslinked polystyrene or crosslinked styrene and vinylbenzene Composed of things. In a specific embodiment, the polymer is Diaion HP-20.

In one aspect, the present invention provides a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is acteoside.

In one aspect, the present invention provides a method for preparing a sweet-scented osmanthus extract, wherein the sweet-scented osmanthus extract is cycoside, and the cycoside is used for preparing anti-oxidant, skin maintenance, anti-microbial and anti-inflammatory effects. Uses of the composition. Specifically, this type of colchicoside has whitening, anti-wrinkle and anti-ultraviolet effects.

The invention is illustrated by the above description of the invention and the following examples, but is not intended to limit the scope of the invention.

Example 1: Preparation of Osmanthus fragrans extract (1)

Add 1.0 kg of dried Osmanthus fragrans to 10 times the volume of 60% ethanol solution, and then perform ultrasonic extraction for 40 minutes to obtain a crude extract. After filtering the crude extract and repeating the above extraction steps to obtain a crude extract, Combine twice to obtain a crude extract. After filtration and concentration under reduced pressure, 384.0 g of a crude extract is obtained, wherein the crude extract contains about 30-40% acteoside. The crude extract is then re-dissolved in an aqueous solution, and the crude extract after re-dissolution is passed through a column (Diaion HP-20) filled with a hydrophobic macroporous polymer for chromatography. The column is firstly washed with water, and then sequentially with 30% and 95% ethanol. Among them, the eluate obtained by eluting with a 30% ethanol extracting solution is concentrated under reduced pressure to dry and obtain 77.8 g of citroside and 67.5 g of a mixture containing mannitol and citroside. 60-70% chloroticin. The extraction process is shown in Figure 1.

Example 2: Preparation of Osmanthus fragrans extract (2)

Add 1.0 kg of dried Osmanthus fragrans to 10 times the volume of 60% ethanol solution, and then perform ultrasonic extraction for 40 minutes to obtain a crude extract. After filtering the crude extract and repeating the above extraction steps to obtain a crude extract, Combine twice to obtain a crude extract. After filtration and concentration under reduced pressure, 355.5 g of a crude extract can be obtained, wherein the crude extract contains about 30-40% chloroticin. The crude extract is then extracted with a methanol or ethanol solution, and the methanol or ethanol soluble layer (278.4 g) can be obtained after concentration by filtration. Next, the methanol or ethanol soluble layer was passed through a column (Diaion HP-20) containing a hydrophobic macroporous polymer for chromatography. The column is firstly washed with water, and then sequentially with 30% and 95% ethanol. Among them, the extract obtained by extracting with a 30% ethanol extract solution is concentrated under reduced pressure and dried to obtain 83.5 g of cynoside and 67.5 g of a mixture containing mannitol and cynoside. 60-70% chloroticin. The extraction process is shown in Figure 2.

Example 3: Preparation of Osmanthus fragrans extract (3)

Add 1.0 kg of dried Osmanthus fragrans to 10 times the volume of 50% ethanol solution, and then perform ultrasonic extraction for 40 minutes to obtain a crude extract. After filtering the crude extract and repeating the above extraction steps to obtain a crude extract, combine them Twice to obtain a crude extract. After filtration and concentration under reduced pressure, 380.7 g of a crude extract can be obtained, wherein the crude extract contains about 30-40% chloroticin. The crude extract is then extracted with a methanol or ethanol solution, and the methanol or ethanol soluble layer (300.4 g) can be obtained after concentration by filtration. Next, the methanol or ethanol soluble layer was passed through a column (Diaion HP-20) containing a hydrophobic macroporous polymer for chromatography. The column is firstly washed with water, and then sequentially with 30% and 95% ethanol. Among them, the extract obtained by extracting with 30% ethanol extract solution was concentrated and dried under reduced pressure to obtain 90.4 g of cycoside and 69.5 g of a mixture containing mannitol and cycoside. 60-70% chloroticin. The extraction process is shown in Figure 3.

Example 4: Preparation of Osmanthus fragrans extract (4)

1.0 kg of dried Osmanthus fragrans was added to 10 times the volume of the aqueous solution, followed by extraction with ultrasonic vibration for 40 minutes to obtain a crude extract. After filtering the crude extract, the above extraction steps were repeated to obtain a crude extract. A crude extract was obtained. After filtering and concentrating under reduced pressure, 302.9 g of a crude extract can be obtained, wherein the crude extract contains about 30-40% chloroticin. The crude extract is then extracted with a methanol or ethanol solution, and the methanol or ethanol soluble layer (176.3 g) can be obtained after filtration and concentration. The extract preparation process is shown in FIG. 4.

Example 5: Preparation of Osmanthus fragrans extract (5)

1.0 kg of dried Osmanthus fragrans was added to 20 times the volume of the aqueous solution, and then the aqueous solution was boiled and maintained for 1 to 3 hours for extraction. The crude extract was filtered and passed through a column containing a hydrophobic macroporous polymer (Diaion HP -20). The column is firstly washed with water, and then sequentially with 30% and 95% ethanol. Among them, the extract obtained by extracting with a 30% ethanol extract solution was concentrated and dried under reduced pressure to obtain 81.3 g of cynoside and 49.8 g of a mixture containing mannitol and cynoside. 60-70% chloroticin. The extraction process is shown in Figure 5.

It can be known from the results of the examples that the method for preparing osmanthus extract provided by the present invention has the excellent effect of obtaining cynoside in a large amount and quickly.

Claims (13)

A method for preparing a osmanthus extract that is rich in cycosides from osmanthus flavus, wherein the osmanthus extract is prepared by the following steps: (1) mixing dried osmanthus with water or ethanol solution and extracting it by ultrasonic vibration Crude extract; (2) filtering the crude extract obtained in step (1) and concentrating it under reduced pressure to obtain a crude extract, adding an ethanol solution for extraction, and filtering and concentrating to obtain an ethanol-soluble layer; Into a chromatographic column, and sequentially with water and an alcoholic extraction solution, and then concentrated and dried under reduced pressure to obtain the osmanthus-rich osmanthus-rich osmanthus extract. The method of claim 1, wherein the ethanol solution is a 5-95% ethanol solution. The method of claim 2, wherein the ethanol solution is a 30-80% ethanol solution. The method according to claim 1, wherein the alcohol extraction solution is a 10-95% ethanol solution. The method as claimed in claim 4, wherein the alcohol extraction solution is a 20-50% ethanol solution. The method as claimed in claim 5, wherein the alcohol extraction solution is a 30% ethanol solution. According to the method of claim 1, the chromatography column is packed with a hydrophobic macroporous polymer, wherein the polymer is composed of a crosslinked polystyrene or a crosslinked styrene and an ethylene-benzene copolymer. The method of claim 7, wherein the polymer is Diaion HP-20. The method according to claim 1, wherein the Osmanthus fragrans extract obtained by the method is rich in cycoside and can be used for preparing a composition having antioxidative effect. The method according to claim 1, wherein the Osmanthus fragrans extract obtained by the method is rich in cycoside, and can be used for preparing a composition having skin care effect. The method of claim 1, wherein the osmanthus extract obtained by the method has the functions of whitening, anti-wrinkle and anti-ultraviolet rays. The method of claim 1, wherein the osmanthus extract obtained by the method has an antimicrobial effect. The method of claim 1, wherein the osmanthus extract obtained by the method has an anti-inflammatory effect.