CN110960602A - Method for extracting and nanocrystallizing insoluble components in plant - Google Patents
Method for extracting and nanocrystallizing insoluble components in plant Download PDFInfo
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- CN110960602A CN110960602A CN201911326913.1A CN201911326913A CN110960602A CN 110960602 A CN110960602 A CN 110960602A CN 201911326913 A CN201911326913 A CN 201911326913A CN 110960602 A CN110960602 A CN 110960602A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/87—Vitaceae or Ampelidaceae (Vine or Grape family), e.g. wine grapes, muscadine or peppervine
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/82—Theaceae (Tea family), e.g. camellia
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The traditional extraction process of insoluble components in plants is complicated in steps, complex in process and long in time consumption. Aiming at the defects of the prior art, the invention aims to provide a method for extracting and nanocrystallizing insoluble components in plants, which can effectively improve or enhance the (water) solubility of the insoluble components by converting the insoluble drugs into nano-scale particles with the particle size of 1-l00nm, thereby enhancing the bioavailability and the drug effect of insoluble matters. The advantages are that: (1) the micro powder prepared by the invention contains a large amount of insoluble components in the plant body, and the water solubility of the micro powder is greatly improved after processing. (2) The invention has simple preparation process, easy control of reaction, good stability, industrialization and wide popularization prospect in the field of plant purification and nanocrystallization.
Description
Technical Field
The invention relates to a method for extracting and nanocrystallizing insoluble components in a plant body, in particular to a method for preparing plant nanoparticles by a high-pressure homogenization method.
Background
The obtaining of insoluble components in plants usually involves extraction and purification steps. The extraction is mainly determined by the physicochemical properties (acidity or alkalinity, thermal stability, solubility, etc.) of the target compound, and the aim is to stably extract the target compound in the maximum yield. The extraction method generally comprises water decoction, organic solvent thermal reflux, ultrasonic extraction, etc., and the thermally unstable compounds can only be extracted at low temperature, such as cold soaking, ultralow temperature critical extraction, etc. The extraction solvent is selected according to the polarity and acidity or alkalinity of the compound, such as alkaloids, and since the compound is alkaline, most of the alkaloids are salified by an acid extraction method, are easily dissolved in water, and then are extracted, and then are alkalized to restore the original structure, or the alkaloids are dissociated by an alkaline solution and then are extracted by a polar solvent. For example, polysaccharides are usually soluble in water and insoluble in alcohol, and are generally extracted with water or precipitated with alcohol. In addition, purification is generally performed by extracting according to different polarities, roughly dividing the extract into several polar sections, and then separating by methods such as silica gel column, macroporous resin, high-speed countercurrent extraction and the like, wherein the principle is that separation is performed according to the polarity, molecular weight, affinity with resin, and distribution coefficient difference among different solvents. A small number of compounds may be obtained by recrystallization.
The traditional process has the disadvantages of complicated steps, complex process and long time consumption. In recent years, the high-pressure homogenization technology is widely applied, and is used in the industries of biology, medicine, food, chemical engineering and the like to carry out cell disruption, drink homogenization, fine chemical engineering and prepare products such as liposome, fat emulsion, nano suspension, micro emulsion, lipid microsphere, emulsion, dairy product and the like. However, the application of high pressure homogenization techniques to the extraction of insoluble components from plants has not been reported.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for extracting and nanocrystallizing insoluble components in plants, which can effectively improve or enhance the (water) solubility of the insoluble components by converting the insoluble drugs into nano-scale particles with the particle size of 1-l00nm, thereby enhancing the bioavailability and the drug effect of insoluble matters.
The specific scheme of the invention comprises:
(1) the plant body is pre-dispersed by a low-temperature traditional Chinese medicine ultrafine pulverizer, so that the particle size of the plant powder is less than 10 microns.
(2) One or more solvents are selected, and the plant powder which is difficult to dissolve in the superfine powder is prepared into dispersion (mass fraction is more than 30%). containing surfactant (1-20 wt%) and cosurfactant (1-10 wt%) is slowly dropped (or sprayed) into the dispersion (1/2-1/5 volume of the dispersion) under the condition of stirring and ultrasonic vibration to form suspension of plant particles.
(3) Treating the suspension of the plant particles by a high-pressure homogenizer with a standard rated maximum working pressure of 200-1600bar, circularly reciprocating for 3-5 times, and collecting the homogenized liquid.
(4) A salting-out method is adopted to filter a large amount of water, and then a spray drying method is selected to obtain micro powder of insoluble components in the plant body.
The solvent can be selected from water, alcohols, esters, ketones, liquid acids or bases, or other solvents. Wherein the alcohol is selected from monohydric alcohol or polyhydric alcohol, such as ethanol, propanol, butanol, ethylene glycol, propylene glycol, glycerol, etc.; examples of the esters include ethyl lactate, butyl lactate, ethyl acetate, butyl acetate, and Y-butyrolactone; examples of the ketones include acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, and methyl pentanone; examples of the acid or base include acetic acid, hydrochloric acid, and sodium hydroxide; examples of other solvents are pyridine, tetrahydrofuran, etc.
The surfactant and cosurfactant comprise: anionic surfactants such as sodium lauryl sulfate, sodium dodecylbenzenesulfonate and the like; nonionic surfactants such as octadecyl polyoxyethylene, fatty acid sorbitan polyoxyethylene, polysorbate, and the like; amphoteric surfactants such as amine carboxylates and quaternary ammonium carboxylates; cationic surfactants such as cetyltrimethylammonium bromide and the like; cosurfactants such as alcohols with medium carbon chain lengths, e.g., dodecanol, hexadecanol, etc.
The invention has the advantages that:
(1) the micro powder prepared by the invention contains a large amount of insoluble components in the plant body, and the water solubility of the micro powder is greatly improved after processing.
(2) The invention has simple preparation process, easy control of reaction, good stability, industrialization and wide popularization prospect in the field of plant purification and nanocrystallization.
Detailed Description
The technical solution of the present invention is further described below by specific examples. The following examples are further illustrative of the present invention and do not limit the scope of the present invention.
Example 1
Pre-dispersing Anji white tea by a low-temperature traditional Chinese medicine ultrafine pulverizer, wherein the particle size of D90 of the powder reaches 5.8 microns.
Preparing water, ethanol and ethyl acetate into a mixed solvent according to the volume ratio of 1:1:1, preparing the superfine tea powder into a dispersion liquid with the mass fraction of 35%, and slowly dripping aqueous solution containing 20% of polysorbate and 5% of hexadecanol into the dispersion liquid (1/3 of the dispersion liquid in volume) under the combined action of stirring and ultrasonic vibration to form a suspension of the superfine tea powder.
Treating the suspension of plant particles with a high-pressure homogenizer at a standard rated maximum working pressure of 1600bar, circulating for 5 times, and collecting homogenized liquid.
A salting-out method is adopted to filter a large amount of water, and then a spray drying method is selected to obtain micro powder containing insoluble components in the tea leaves.
The particle size of the product is as follows: d90 ═ 1.35 microns.
Example 2
The Orthosiphon aristatus is pre-dispersed by a low-temperature traditional Chinese medicine ultrafine pulverizer, and the particle size of D90 of the powder reaches 7.9 microns.
Preparing water, butanol and acetone into a mixed solvent according to the volume ratio of 2:1:0.5, preparing the superfine Chinese alpine rush into a dispersion liquid with the mass fraction of 40%, and slowly dripping aqueous solution containing 10% of sodium dodecyl sulfate and 10% of hexadecanol into the dispersion liquid (the volume of 1/3 of the dispersion liquid) under the combined action of stirring and ultrasonic vibration to form the suspension of the superfine Chinese alpine rush.
Treating the suspension of plant particles with a high-pressure homogenizer at a standard rated maximum working pressure of 800bar, circulating for 5 times, and collecting homogenized liquid.
A salting-out method is adopted to filter a large amount of water, and then a spray drying method is selected to obtain micro powder containing insoluble components in the Chinese alpine rush.
The particle size of the product is as follows: d90 ═ 3.58 μm.
Example 3
The radix tetrastigme is pre-dispersed by a low-temperature traditional Chinese medicine ultrafine pulverizer, and the particle size of D90 of the powder reaches 4.9 microns.
Preparing water, propylene glycol and butyl lactate into a mixed solvent according to the volume ratio of 2:2:1, preparing the superfine herba clerodendri bungei into a dispersion liquid with the mass fraction of 40%, and slowly dripping aqueous solution containing 10% of hexadecyl trimethyl ammonium bromide and 5% of dodecanol into the dispersion liquid (the volume of 1/5 of the dispersion liquid) under the combined action of stirring and ultrasonic vibration to form the suspension of the superfine radix tetrastigme.
Treating the suspension of plant particles with a high-pressure homogenizer at standard rated maximum working pressure of 1000bar, repeating for 3 times, and collecting homogenized liquid.
A salting-out method is adopted to filter a large amount of water, and then a spray drying method is selected to obtain micro powder containing insoluble components in the radix tetrastigme.
The particle size of the product is as follows: d90 ═ 4,15 microns.
Claims (3)
1. A method for extracting and nanocrystallizing insoluble components in a plant body is characterized by comprising the following steps:
(1) the plant body is pre-dispersed by a low-temperature traditional Chinese medicine ultrafine pulverizer, so that the particle size of the plant powder is less than 10 microns.
(2) One or more solvents are selected, and the plant powder which is difficult to dissolve in the superfine powder is prepared into dispersion (mass fraction is more than 30%). containing surfactant (1-20 wt%) and cosurfactant (1-10 wt%) is slowly dropped (or sprayed) into the dispersion (1/2-1/5 volume of the dispersion) under the condition of stirring and ultrasonic vibration to form suspension of plant particles.
(3) Treating the suspension of the plant particles by a high-pressure homogenizer with a standard rated maximum working pressure of 200-1600bar, circularly reciprocating for 3-5 times, and collecting the homogenized liquid.
(4) A salting-out method is adopted to filter a large amount of water, and then a spray drying method is selected to obtain micro powder of insoluble components in the plant body.
2. The method according to claim 1, wherein the solvent is selected from water, alcohols, esters, ketones, liquid acids or bases, and other solvents. Wherein the alcohol is selected from monohydric alcohol or polyhydric alcohol, such as ethanol, propanol, butanol, ethylene glycol, propylene glycol, glycerol, etc.; examples of the esters include ethyl lactate, butyl lactate, ethyl acetate, butyl acetate, and Y-butyrolactone; examples of the ketones include acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, and methyl pentanone; examples of the acid or base include acetic acid, hydrochloric acid, and sodium hydroxide; examples of other solvents are pyridine, tetrahydrofuran, etc.
3. The method according to claim 1, wherein the surfactant and co-surfactant comprise: anionic surfactants such as sodium lauryl sulfate, sodium dodecylbenzenesulfonate and the like; nonionic surfactants such as octadecyl polyoxyethylene, fatty acid sorbitan polyoxyethylene, polysorbate, and the like; amphoteric surfactants such as amine carboxylates and quaternary ammonium carboxylates; cationic surfactants such as cetyltrimethylammonium bromide and the like; cosurfactants such as alcohols with medium carbon chain lengths, e.g., dodecanol, hexadecanol, etc.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911326913.1A CN110960602A (en) | 2019-12-20 | 2019-12-20 | Method for extracting and nanocrystallizing insoluble components in plant |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911326913.1A CN110960602A (en) | 2019-12-20 | 2019-12-20 | Method for extracting and nanocrystallizing insoluble components in plant |
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| CN110960602A true CN110960602A (en) | 2020-04-07 |
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| CN201911326913.1A Pending CN110960602A (en) | 2019-12-20 | 2019-12-20 | Method for extracting and nanocrystallizing insoluble components in plant |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111455563A (en) * | 2020-04-20 | 2020-07-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of Chinese herbal medicine nanofiber membrane with potential antiviral effect |
| CN112457921A (en) * | 2020-12-10 | 2021-03-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of grapefruit essential oil with high extraction rate |
| CN113827633A (en) * | 2021-10-25 | 2021-12-24 | 上海健康医学院 | A method for preparing Chinese medicinal nanometer powder |
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| WO2003037359A1 (en) * | 2001-10-29 | 2003-05-08 | Chengdu Somo Namotechnology Co., Ltd. | Nanoparticle of insoluble medicinal components and method to produce thereof |
| CN1586528A (en) * | 2004-08-13 | 2005-03-02 | 武汉理工大学 | Method for nano plant Chinese medicine |
| CN1626065A (en) * | 2003-12-11 | 2005-06-15 | 成都思摩纳米技术有限公司 | Method for preparing Nano granule of volatile oil |
| US20060151899A1 (en) * | 2003-08-06 | 2006-07-13 | Akira Kato | Process for producing drug ultramicroparticle and apparatus therefor |
| KR20090027734A (en) * | 2006-07-27 | 2009-03-17 | (주)아모레퍼시픽 | Process for preparing powder comprising nanoparticles of sparingly soluble drug |
-
2019
- 2019-12-20 CN CN201911326913.1A patent/CN110960602A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003037359A1 (en) * | 2001-10-29 | 2003-05-08 | Chengdu Somo Namotechnology Co., Ltd. | Nanoparticle of insoluble medicinal components and method to produce thereof |
| US20060151899A1 (en) * | 2003-08-06 | 2006-07-13 | Akira Kato | Process for producing drug ultramicroparticle and apparatus therefor |
| CN1626065A (en) * | 2003-12-11 | 2005-06-15 | 成都思摩纳米技术有限公司 | Method for preparing Nano granule of volatile oil |
| CN1586528A (en) * | 2004-08-13 | 2005-03-02 | 武汉理工大学 | Method for nano plant Chinese medicine |
| KR20090027734A (en) * | 2006-07-27 | 2009-03-17 | (주)아모레퍼시픽 | Process for preparing powder comprising nanoparticles of sparingly soluble drug |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111455563A (en) * | 2020-04-20 | 2020-07-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of Chinese herbal medicine nanofiber membrane with potential antiviral effect |
| CN112457921A (en) * | 2020-12-10 | 2021-03-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of grapefruit essential oil with high extraction rate |
| CN113827633A (en) * | 2021-10-25 | 2021-12-24 | 上海健康医学院 | A method for preparing Chinese medicinal nanometer powder |
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