TW201601739A - A method for preparing Osmanthus fragrans extracts - Google Patents

Abstract

This invention provides a method for preparing Osmanthus fragrans extracts, wherein the Osmanthus fragrans extracts are acteoside. Particularly, the acteoside has the effect of antioxidant, skin care, antibiotic and anti-inflammation.

Description

Method for preparing sweet-scented osmanthus extract

The invention provides a preparation method of an osmanthus extract, wherein the sweet-scented osmanthus extract is acteoside. Specifically, the leaf aglycone has anti-oxidation, skin care, anti-microbial and anti-inflammatory effects.

Osmanthus fragrans (Thunb) Lour. is an evergreen shrub of the Osmanthus family of Oleaceae. It has a floral aroma, extracts essential oils, prepares sweet-scented osmanthus extracts, and can be used in the production of food and cosmetics. On the top, it has the effect of warming the lungs and dispelling cold and relieving pain. In medicinal use, its roots or root bark can be used to treat stomach pain, toothache, rheumatism, numbness and muscle pain; its flower can be used for phlegm, dilated phlegm, phlegm and blood stasis, intestinal wind, blood stasis, phlegm, toothache and bad breath. And its fruit can be used to warm stomach, Pinggan, Yishen, dispel cold and treat liver and stomach pain.

Cinnamole, also known as verbascoside, ergoside or verbascoside, is generally obtained from plants such as the genus Rehmannia, Cistanche or Prunus, and Osmanthus fragrans also contains phylloside. C. sinensis is an effective antimicrobial ingredient and is known to have good antibacterial activity against Staphylococcus aureus (Guillermo et al., 1999, Journal of Ethnopharmacology 66 (1): 75-8.). It has a good anti-inflammatory effect (Speranza et al., 2009, Journal of biological regulators and homeostatic agents 23 (3): 189-95.). The leaf gonadoside also has the effects of whitening, anti-wrinkle and anti-ultraviolet rays. In addition, studies have shown that flavonoids can be used for liver protection or for the treatment of Alzheimer's disease. From this, it is known that a large amount of extraction of the leaf sinensis is required, however, the existing extraction method steps are still cumbersome.

The present invention unanticipated the discovery of a novel method for the preparation of flavonoids, which can extract a large amount and efficiently extract the phylloside from Osmanthus fragrans.

The object of the present invention is to provide a method for preparing an Osmanthus fragrans extract, wherein the Osmanthus fragrans extract is prepared by the following steps: (1) mixing osmanthus with water or a first alcohol solution and then extracting by boiling or ultrasonic wave oscillation respectively (2) The crude extract solution obtained in the step (1) is concentrated and filtered to remove the precipitate, and then concentrated under reduced pressure or freeze-dried to obtain the sweet-scented osmanthus extract, wherein the crude extract solution can also be directly concentrated under reduced pressure. Or lyophilization to obtain the sweet-scented osmanthus extract.

In an embodiment of the present invention, the sweet-scented osmanthus extract is prepared by the following steps: (1) mixing the sweet-scented osmanthus with water or the first alcohol solution, respectively, after boiling or ultrasonically shaking, and extracting the obtained crude extract solution. After concentration and filtration to remove the precipitate, the solution is concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of step (1) is dissolved in water and then passed through a column of chromatography, followed by water and The alcohol extracting solution is subjected to extraction, and the extract is collected and concentrated under reduced pressure or freeze-dried to obtain the sweet-scented osmanthus extract.

In one aspect, the present invention provides a method for preparing an Osmanthus fragrans extract, wherein the Osmanthus fragrans extract is prepared by the following steps: (1) mixing osmanthus with water or the first alcohol solution, respectively, after boiling or ultrasonic wave shaking, and extracting, the obtained crude extract solution is concentrated and filtered to remove the precipitate, and then concentrated under reduced pressure to obtain the crude extract. (2) extracting the crude extract filtrate of step (1) with a second alcohol solution, and extracting the extract solution to remove the precipitate, and then concentrating under reduced pressure or lyophilizing to obtain the sweet-scented osmanthus extract. .

In another aspect, the present invention provides a method for preparing an Osmanthus fragrans extract, wherein the Osmanthus fragrans extract is prepared by the following steps: (1) mixing osmanthus with water or a first alcohol solution, respectively, after boiling or ultrasonically oscillating The extraction is performed, and the obtained crude extract solution is concentrated and filtered to remove the precipitate, and then concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of the step (1) is further extracted with the second alcohol solution. The obtained extract solution is filtered to remove the precipitate, and then concentrated under reduced pressure to obtain an extract; (3) the extract of the step (2) is dissolved in water and then introduced into the column, followed by water. And extracting the alcohol extracting solution, collecting the extracting liquid, and concentrating under reduced pressure or lyophilizing to obtain the sweet-scented osmanthus extract.

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

In one aspect, the method for preparing an osmanthus extract provided by the present invention, wherein the alcohol extracting solution is a 10-95% ethanol solution. In a particular embodiment, the alcohol extracting solution is a 20-50% ethanol solution. In another specific embodiment, wherein the alcohol extracting solution is a 30% ethanol solution.

In another aspect, in the method for preparing an Osmanthus fragrans extract provided by the present invention, the second alcohol solution is a methanol or ethanol solution.

In another aspect, in the method for preparing an Osmanthus fragrans extract provided by the present invention, the chromatography column is filled with a hydrophobic macroporous polymer, wherein the polymer is copolymerized by crosslinked polystyrene or crosslinked styrene and ethylene benzene. Composition of things. In a particular embodiment of the invention, the polymer is Diaion HP-20.

In one aspect, the present invention provides a method for preparing an Osmanthus fragrans extract, wherein the Osmanthus fragrans extract is acteoside.

In one aspect, the present invention provides a method for preparing an Osmanthus fragrans extract, wherein the Osmanthus fragrans extract is a lutein, and the cohoposide is used for preparation of anti-oxidation, skin care, anti-microbial and anti-inflammatory Use of the efficacy composition. Specifically, the flavonoids have the effects of whitening, anti-wrinkle and anti-ultraviolet rays.

The above and other aspects of the present invention will be apparent from the following description of the preferred embodiments of the invention. Spirit and scope.

The preferred embodiment of the invention presented in the present invention is intended to illustrate the invention. It should be understood that the invention is not limited to the preferred embodiments shown.

Fig. 1 shows a preparation process of the sweet-scented osmanthus extract, wherein the dried osmanthus is first extracted with a 60% ethanol solution, filtered and concentrated under reduced pressure, and then subjected to column chromatography to obtain the sweet-scented osmanthus extract.

2 shows the preparation process of the sweet-scented osmanthus extract, wherein the dried sweet-scented osmanthus is first extracted with a 60% ethanol solution, filtered and concentrated under reduced pressure, followed by extraction with methanol or ethanol, and then subjected to column Chromatography was performed to obtain the osmanthus extract.

3 shows the preparation process of the sweet-scented osmanthus extract, wherein the dried sweet-scented 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 sweet-scented osmanthus. Extracts.

Fig. 4 shows a preparation process of the sweet-scented osmanthus extract, wherein the dried sweet-scented osmanthus is extracted with water, and concentrated by filtration and concentration under reduced pressure, followed by extraction with methanol or ethanol to obtain the sweet-scented osmanthus extract.

Fig. 5 shows a preparation process of the sweet-scented osmanthus extract, wherein the dried osmanthus is extracted with water, and directly subjected to column chromatography to obtain the sweet-scented osmanthus extract.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as the ones of ordinary skill in the art.

The singular forms "a", "an", "the" and "the" are used in the plural. Thus, for example, reference to "a component" includes a plurality of such elements and equivalents to those of ordinary skill in the art.

The invention provides a preparation method of an 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 by boiling or ultrasonic wave shaking; 2) The crude extract obtained in the step (1) is concentrated and filtered to remove the precipitate, and then concentrated under reduced pressure or freeze-dried to obtain the sweet-scented osmanthus extract, wherein the crude extract solution can also be directly concentrated or frozen under reduced pressure. The dried osmanthus extract is obtained after drying.

According to an embodiment of the present invention, 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, respectively, after boiling or ultrasonically oscillating, and extracting the obtained crude extract solution. After the precipitate is removed by concentration and filtration, it is concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of step (1) is dissolved in water and then introduced into the column, followed by water. The alcohol extracting solution is extracted, and the extract is collected and concentrated under reduced pressure or freeze-dried to obtain the sweet-scented osmanthus extract.

According to another embodiment of the present invention, 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, respectively, after boiling or ultrasonically shaking, and extracting the obtained crude extract After the solution is concentrated and filtered to remove the precipitate, it is concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of the step (1) is further extracted with the second alcohol solution, and the obtained extract solution is subjected to extraction. After the precipitate is removed by filtration, the osmanthus extract is obtained by concentration under reduced pressure or freeze-drying.

According to an embodiment of the present invention, 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, respectively, after boiling or ultrasonically oscillating, and extracting the obtained crude extract. The solution is concentrated and filtered to remove the precipitate, and then concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of the step (1) is further extracted with a second alcohol solution, and the resulting extract solution is filtered. After removing the precipitate, it is concentrated under reduced pressure to obtain the extract; (3) The extract of the step (2) is dissolved in water and then introduced into the column of the chromatography column, and then washed with water and an alcohol extracting solution, and the extracts are collected and concentrated under reduced pressure or The osmanthus extract is obtained after freeze drying.

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

In one aspect, the method for preparing an osmanthus extract provided by the present invention, wherein the alcohol extracting solution is a 10-95% ethanol solution. In a particular embodiment, the alcohol extracting solution is a 20-50% ethanol solution. In another specific embodiment, wherein the alcohol extracting solution is a 30% ethanol solution.

In another aspect, in the method for preparing an Osmanthus fragrans extract provided by the present invention, the second alcohol solution is a methanol or ethanol solution. In a particular embodiment, the second alcohol solution is a methanol solution.

In another aspect, in the method for preparing an Osmanthus fragrans extract provided by the present invention, the chromatography column is filled with a hydrophobic macroporous polymer, wherein the polymer is copolymerized by crosslinked polystyrene or crosslinked styrene and ethylene benzene. Composition of things. In a particular embodiment, wherein the polymer is Diaion HP-20.

In one aspect, the present invention provides a method for preparing an Osmanthus fragrans extract, wherein the Osmanthus fragrans extract is acteoside.

In one aspect, the present invention provides a method for preparing an Osmanthus fragrans extract, wherein the Osmanthus fragrans extract is a lutein, and the cohoposide is used for preparing anti-oxidation, skin care, anti-microbial and anti-inflammatory effects. The use of the composition. Specifically, the flavonoids have the effects of whitening, anti-wrinkle and anti-ultraviolet rays.

The invention is described in the above description of the invention and the following examples, which are not intended to limit the scope of the invention.

Example 1: Preparation of Osmanthus fragrans Extract (1)

1.0 kg of dried Osmanthus fragrans was added to 10 volumes of 60% ethanol solution, followed by ultrasonic wave shaking for 40 minutes for extraction, and the crude extract was concentrated and filtered, and then the above extraction was repeated in 10 volumes of 60% ethanol solution. step. After filtration and concentration under reduced pressure, 384.0 g of a crude extract was obtained, the crude extracts containing about 30-40% of the acteoside. The crude extract is then reconstituted as an aqueous solution, and the crude extract after re-dissolving is passed through a column (Diaion HP-20) containing a hydrophobic macroporous polymer for chromatography. The column was first washed with water, and then washed with 30% and 95% ethanol. The extract obtained by extracting with 30% ethanol extracting solution is concentrated and dried under reduced pressure to obtain 77.8 g of flavonoids and 67.5 g of a mixture containing mannitol and flavonoids, wherein the mixture contains about 60-70% class of leaf asparagine. The above extraction preparation process is shown in Figure 1.

Example 2: Preparation of Osmanthus fragrans Extract (II)

1.0 kg of dried Osmanthus fragrans was added to 10 volumes of 60% ethanol solution, followed by ultrasonic wave shaking for 40 minutes for extraction, and the crude extract was concentrated and filtered, and then the above extraction was repeated in 10 volumes of 60% ethanol solution. step. After filtration and concentration under reduced pressure, 355.5 g of a crude extract was obtained. The crude extract is then extracted with a methanol or ethanol solution and concentrated by filtration to give the methanol or ethanol soluble layer (278.4 g). Next, the methanol or ethanol soluble layer was passed through a column (Diaion HP-20) containing a hydrophobic macroporous polymer for chromatography. The column was first washed with water, and then washed with 30% and 95% ethanol. The extract obtained by extracting with a 30% ethanol extracting solution is concentrated and dried under reduced pressure to obtain 83.5 g of cohosin and 67.5 g of a mixture containing mannitol and flavonoids, wherein the mixture contains about 60-70% class of leaf asparagine. The above extraction preparation process is shown in Figure 2.

Example 3: Preparation of Osmanthus fragrans Extract (3)

1.0 kg of dried Osmanthus fragrans was added to 10 volumes of 50% ethanol solution, followed by ultrasonic wave shaking for 40 minutes for extraction, and the crude extract was concentrated and filtered, and then the above extraction step was repeated in 10 volumes of 50% ethanol solution. . After filtration and concentration under reduced pressure, a crude extract of 380.7 g was obtained, and the crude extract contained approximately 30-40% of the leaves of aglycone. The crude extract is then extracted with a methanol or ethanol solution and concentrated by filtration to give the methanol or ethanol soluble layer (300.4 g). Next, the methanol or ethanol soluble layer was passed through a column (Diaion HP-20) containing a hydrophobic macroporous polymer for chromatography. The column was first washed with water, and then washed with 30% and 95% ethanol. The extract obtained by extracting with a 30% ethanol extracting solution is concentrated and dried under reduced pressure to obtain 90.4 g of flavonoids and 69.5 g of a mixture containing mannitol and flavonoids, wherein the mixture contains about 60-70% class of leaf asparagine. The above extraction preparation process is shown in FIG.

Example 4: Preparation of Osmanthus fragrans Extract (4)

1.0 kg of dried Osmanthus fragrans was added to 10 volumes of an aqueous solution, followed by ultrasonication for 40 minutes for extraction, and the crude extract was concentrated and filtered, and the above extraction step was repeated with 10 volumes of an aqueous solution. After filtration and concentration under reduced pressure, 302.9 g of a crude extract was obtained, the crude extracts containing about 30-40% of the leaves. The crude extract is then extracted with methanol or ethanol solution and concentrated by filtration to give the methanol or ethanol soluble layer (176.3 g). The above extraction preparation process is shown in FIG.

Example 5: Preparation of Osmanthus fragrans Extract (5)

1.0 kg of dried Osmanthus fragrans was added to a 20-fold aqueous solution, and then the aqueous solution was boiled and maintained for 1-3 hours for extraction. The crude extract was concentrated and filtered and passed through a column containing a hydrophobic macroporous polymer ( Chromatography was carried out in Diaion HP-20). The column was first washed with water, and then washed with 30% and 95% ethanol. The extract obtained by extracting with 30% ethanol extracting solution is concentrated and dried under reduced pressure to obtain 81.3 g of clathoma and 49.8 g of a mixture containing mannitol and flavonoids, wherein the mixture contains about 60-70% class of leaf asparagine. The above extraction preparation process is shown in FIG.

It can be seen from the results of the examples that the preparation method of the sweet-scented osmanthus extract provided by the present invention has the excellent effect of obtaining a large amount and rapidly obtaining the phylloside.

Claims (18)

The invention relates to a method for preparing an osmanthus extract, wherein the osmanthus extract is prepared by the following steps: (1) mixing osmanthus with water or a first alcohol solution and then extracting by boiling or ultrasonic wave shaking; (2) stepping (1) The obtained crude extract solution is concentrated and filtered to remove the precipitate, and then concentrated under reduced pressure or freeze-dried to obtain the sweet-scented osmanthus extract, wherein the crude extract solution can also be directly concentrated under reduced pressure or freeze-dried to obtain The osmanthus extract. The invention relates to a method for preparing an osmanthus extract, wherein the osmanthus extract is prepared by the following steps: (1) mixing osmanthus with water or a first alcohol solution, respectively, and then extracting by boiling or ultrasonic wave, and extracting the crude extract solution. After the precipitate is removed by concentration and filtration, it is concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of step (1) is dissolved in water and then introduced into the column, followed by water. And extracting the alcohol extracting solution, collecting the extracting liquid, and concentrating under reduced pressure or lyophilizing to obtain the sweet-scented osmanthus extract. The invention relates to a method for preparing an osmanthus extract, wherein the osmanthus extract is prepared by the following steps: (1) mixing osmanthus with water or a first alcohol solution, respectively, and then extracting by boiling or ultrasonic wave, and extracting the crude extract solution. After the precipitate is removed by concentration and filtration, it is concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of the step (1) is further extracted with the second alcohol solution, and the obtained extract solution is removed by filtration. After the precipitate is precipitated, it is concentrated under reduced pressure or freeze-dried to obtain the sweet-scented osmanthus extract. The invention relates to a method for preparing an osmanthus extract, wherein the osmanthus extract is prepared by the following steps: (1) mixing osmanthus with water or a first alcohol solution, respectively, and then extracting by boiling or ultrasonic wave, and extracting the crude extract solution. After the precipitate is removed by concentration and filtration, it is concentrated under reduced pressure to obtain the crude extract; (2) the crude extract of the step (1) is further extracted with the second alcohol solution, and the obtained extract solution is removed by filtration. After the precipitate is concentrated, it is concentrated under reduced pressure to obtain the extract; (3) the extract of the step (2) is dissolved in water and then introduced into the column, and sequentially washed with water and an alcohol. Rushing, collecting the extracts and then concentrating under reduced pressure or lyophilizing The osmanthus extract. The preparation method of any one of claims 1 to 4, wherein the first alcohol solution is a 5-95% ethanol solution. The preparation method of claim 5, wherein the first alcohol solution is a 30-80% ethanol solution. The preparation method of claim 2 or 4, wherein the alcohol extracting solution is a 10-95% ethanol solution. The preparation method of claim 7, wherein the alcohol extracting solution is a 20-50% ethanol solution. The preparation method of claim 8, wherein the alcohol extracting solution is a 30% ethanol solution. The preparation method of claim 3, wherein the second alcohol solution is a methanol or ethanol solution. The preparation method of claim 2 or 4, wherein the chromatography column is filled with a hydrophobic macroporous polymer, wherein the polymer consists of crosslinked polystyrene or a crosslinked styrene and a vinyl benzene copolymer. The preparation method of claim 11, wherein the polymer is Diaion HP-20. The preparation method of any one of claims 1 to 4, wherein the sweet-scented osmanthus extract is acteoside. A use of a flavonoid for the preparation of a composition having an antioxidant effect, wherein the flavonoid is prepared by the preparation method of any one of claims 1 to 4. A use of a flavonoid for the preparation of a composition having a skin care efficacy, wherein the copula is prepared by the preparation method of any one of claims 1 to 4. The use of the scope of claim 15 wherein the composition has whitening, anti-wrinkle and anti-ultraviolet effects. A use of a flavonoid for the preparation of a composition having an antimicrobial effect, which is prepared by the preparation method of any one of claims 1 to 4. A use of a flavonoid for the preparation of a composition having an anti-inflammatory effect, wherein the copula is prepared by the preparation method of any one of claims 1 to 4.