CN108484627B - Method for extracting low-lead eurycomanone from eurycoma longifolia - Google Patents
Method for extracting low-lead eurycomanone from eurycoma longifolia Download PDFInfo
- Publication number
- CN108484627B CN108484627B CN201810388422.9A CN201810388422A CN108484627B CN 108484627 B CN108484627 B CN 108484627B CN 201810388422 A CN201810388422 A CN 201810388422A CN 108484627 B CN108484627 B CN 108484627B
- Authority
- CN
- China
- Prior art keywords
- lead
- filtering
- extracting
- solution
- eurycoma longifolia
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/10—Spiro-condensed systems
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for extracting low-lead eurycomanone from Eurycoma longifolia, which comprises the following steps: a. pulverizing raw materials, namely pulverizing the raw materials of Eurycoma longifolia into fine powder; b. extracting the fine powder with methanol solution, filtering the extractive solution with plate-frame filter, and mixing; c. rough filtering, combining extracting solutions, filtering by using a Chinese ceramic membrane, d, fine filtering, filtering the rough filtering solution by using a roll-type membrane, e, removing lead, adsorbing the fine filtering solution by using a series-connected resin chromatographic column, f, purifying, adsorbing the lead-removed material liquid to saturation by using a macroporous adsorption resin chromatographic column, washing off adsorbed saccharides and pigment impurities by using pure water, eluting by using an ethanol solution, g, concentrating the eluent in vacuum, h, drying, and drying the concentrated solution to obtain faint yellow fine powder. The method has the advantages of low extraction cost, simple extraction method, convenient operation and suitability for industrial production, and the extract has high content of the eurysanone and the content of heavy metal lead is controlled below the national standard, thereby avoiding the harm to the health of eaters.
Description
Technical Field
The invention relates to the technical field of extraction of plant active ingredients, in particular to a method for extracting low-lead eurysanone from Eurycoma longifolia Robusta.
Background
Eurycoma longifolia Jack is a wild shrub plant growing in moist sandy soil in primitive rainforests near the equator in southeast Asia, Eurycoma longifolia has been used as a traditional medicine for hundreds of years, Eurycoma longifolia has the name of Ma ginseng in Malaysia, Eurycoma longifolia has the effects of resisting cancer and malaria, improving male sexual dysfunction and the like, and also can improve human body functions, resist anxiety, osteoporosis, pain and inflammation, resist bacteria, parasites, regulate immunity, resist angiogenesis and treat diabetes. The active component of Eurycoma longifolia is a biterpene of a lignin, and also contains alkaloid, lignanoid, triterpene and other components, and the eurycoma longifolia is the main active component of Eurycoma longifolia.
In recent years, inspection and quarantine departments once sample and detect Eurycoma longifolia, and the situation that the content of heavy metal lead is too high is found, and the health of consumers can be harmed after the products are eaten. The harm of lead poisoning is mainly manifested in the final damage to nervous system, blood system, cardiovascular system, skeletal system, etc., and lead poisoning often occurs: fatigue, emotional depression, heart failure, abdominal pain, kidney deficiency, hypertension, arthralgia, reproductive disorders, anemia, etc.
Disclosure of Invention
The invention aims to provide a method for extracting low-lead eurycomanone from eurycoma longifolia, which is used for improving the content of eurycomanone in an extract and controlling the content of heavy metal lead below a national standard. In order to achieve the purpose, the invention adopts the following technical scheme:
a method for extracting low-lead eurycomanone from Eurycoma longifolia, which comprises the following steps:
a. pulverizing raw materials, namely pulverizing the raw materials of Eurycoma longifolia into fine powder;
b. extracting the raw material fine powder for several times by using a methanol solution with the volume fraction of 30-50% at the temperature of 65-70 ℃, filtering the extracting solution by using a plate-and-frame filter, and combining to obtain a combined extracting solution;
c. coarsely filtering, combining the extractive solutions, supplementing pure water for dilution, and filtering with Chinese ceramic membrane to obtain coarse filtrate;
d. fine filtering, diluting the coarse filtrate with pure water, and filtering with roll membrane to obtain fine filtrate
e. Removing lead, adsorbing the fine filtrate with several serially connected resin chromatographic columns, and collecting lead-removed liquid;
f. purifying, namely adsorbing the lead-removed feed liquid to saturation by using a macroporous adsorption resin chromatographic column, washing adsorbed saccharides and pigment impurities by using pure water, eluting by using an ethanol solution with the volume concentration of 50-60%, and collecting an eluent;
g. concentrating, controlling the temperature to be 70-80 ℃, and concentrating the eluent in vacuum until no alcohol smell exists to obtain a concentrated solution;
h. drying, and drying the concentrated solution to obtain fine yellowish powder.
Preferably, the ratio of the material fine powder to the methanol solution in the step b is 1 (10-15) kg/L.
Preferably, the extraction mode in the step b is cooking extraction or ultrasonic extraction.
Preferably, the extraction times in the step b are 2 times, and the time is 1-3 hours and 1-2 hours respectively.
Preferably, the mesh number of the filter cloth of the plate-frame filter in the step b is 100-300 meshes, the pore diameter of the Chinese ceramic membrane in the step c is 8-50 nm, and the molecular weight of the roll-type membrane in the step d is 5000-15000.
Preferably, pure water with the volume of 1-2 times of that of the solution is replenished in the steps c and d.
Preferably, the fine filtrate in step e flows through the resin chromatographic column at a flow rate of 4 times the column volume per hour, the lead-removing feed liquid in step f flows through the macroporous adsorption resin chromatographic column at a flow rate of 2 times the column volume per hour, and the ethanol solution flows through the macroporous adsorption resin chromatographic column at a flow rate of 1 time the column volume per hour.
Preferably, the detection of the lead content in the effluent in the step e to be less than 0.1ppm is finished, and the detection of the broad-leaved ketone content in the effluent in the step f to be more than 0.01mg/mL is finished.
Preferably, the amount of the pure water in the step f is 1-3 times of the column volume, and the amount of the ethanol solution is 4-6 times of the column volume.
Preferably, the drying mode in the step h is spray drying, the air inlet temperature is 185 ℃, the air outlet temperature is 90 ℃, and the rotation speed of the atomizer is 380 r/s.
After the technical scheme is adopted, the invention has the following beneficial effects:
1. the extraction cost is low, the extraction method is simple, the operation is convenient, and the method is suitable for industrial production;
2. the content of the eurysanone in the extract is high;
3. the content of heavy metal lead is controlled below the national standard, so that the harm to the health of eaters is avoided.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the present invention is further described in detail with reference to the specific embodiments below.
Example one
The embodiment discloses a method for extracting low-lead eurycomanone from Eurycoma longifolia, which comprises the following steps:
1. crushing the raw materials, namely taking 10 kg of Eurycoma longifolia as the raw material, slicing and crushing to 8-20 meshes.
2. Extracting the fine powder with 120L of 35% methanol solution at 65 deg.C for 3 hr and 2 hr respectively under ultrasonic extraction for 2 times, filtering the extractive solutions with 200 mesh plate-and-frame filter, and mixing to obtain 235L of mixed extractive solutions.
3. Coarsely filtering, mixing extractive solutions, adding 2 times of pure water, diluting, and filtering with Chinese ceramic membrane with aperture of 20 nm to obtain coarse filtrate.
4. Fine filtering, diluting the coarse filtrate with 2 times of pure water, and filtering with a roll membrane with molecular weight of 10000 to obtain fine filtrate.
5. Removing lead, adsorbing lead with 3 series-connected resin chromatographic columns with the column volume of 8L, flowing the fine filtrate through the resin chromatographic columns at the flow rate of 32L/h, detecting the lead content in the effluent liquid to be less than 0.1ppm, and collecting 290L of lead-removing feed liquid.
6. Purifying, adsorbing the lead-removing feed liquid to saturation by using a macroporous adsorption resin chromatographic column with the column volume of 20L, allowing the lead-removing feed liquid to flow through the resin chromatographic column at the flow rate of 40L/h, detecting that the content of the eurycosan in the effluent liquid is more than 0.01mg/mL, washing off adsorbed saccharides and pigment impurities by using 40L of pure water, eluting by using 80L of ethanol solution with the volume concentration of 55%, allowing the ethanol solution to flow through the macroporous adsorption resin chromatographic column at the flow rate of 20L/h, and collecting 75L of eluate.
7. Concentrating, controlling temperature at 75 deg.C, and vacuum concentrating the eluate until no alcohol smell exists to obtain 5L concentrated solution.
8. Drying, spray drying the concentrated solution, wherein the air inlet temperature is 185 ℃, the air outlet temperature is 90 ℃, and the rotation speed of an atomizer is 380r/s, so that 710 g of faint yellow fine powder is obtained.
The content of the broad-leaved ketone in the yellowish fine powder obtained in the embodiment is 2.01% by high performance liquid detection, and the content of lead is less than 0.05 ppm by inductively coupled plasma mass spectrometry detection.
Example two
The embodiment discloses a method for extracting low-lead eurycomanone from Eurycoma longifolia, which comprises the following steps:
1. crushing the raw materials, namely taking 10 kg of Eurycoma longifolia as the raw material, slicing and crushing to 8-20 meshes.
2. Extracting the fine powder with 100L 50% methanol solution at 70 deg.C for 2 times (1 hr and 1 hr respectively), filtering the extractive solutions with 300 mesh plate-and-frame filter, and mixing to obtain 190L mixed extractive solutions.
3. Coarsely filtering, mixing extractive solutions, adding 1 time of pure water, diluting, and filtering with 50nm Chinese ceramic membrane to obtain coarse filtrate.
4. Fine filtering, diluting the coarse filtrate with 1 time of pure water, and filtering with a roll-type membrane with molecular weight of 15000 to obtain fine filtrate.
5. Removing lead, adsorbing lead with 3 series-connected resin chromatographic columns with the column volume of 8L, flowing the fine filtrate through the resin chromatographic columns at the flow rate of 32L/h, detecting the lead content in the effluent liquid to be less than 0.1ppm, and collecting 205L of lead-removing feed liquid.
6. Purifying, adsorbing the lead-removing feed liquid to saturation by using a macroporous adsorption resin chromatographic column with the column volume of 20L, allowing the lead-removing feed liquid to flow through the resin chromatographic column at the flow rate of 40L/h, detecting that the content of the eurycor in the effluent liquid is more than 0.01mg/mL, washing off adsorbed saccharides and pigment impurities by using 60L of pure water, eluting by using 120L of ethanol solution with the volume concentration of 50%, allowing the ethanol solution to flow through the macroporous adsorption resin chromatographic column at the flow rate of 20L/h, and collecting 120L of eluate.
7. Concentrating, controlling temperature at 80 deg.C, and vacuum concentrating the eluate until no alcohol smell exists to obtain 4L concentrated solution.
8. Drying, spray drying the concentrated solution, wherein the air inlet temperature is 185 ℃, the air outlet temperature is 90 ℃, and the rotation speed of an atomizer is 380r/s, so that 680 g of faint yellow fine powder is obtained.
The content of the broad-leaved ketone in the yellowish fine powder obtained in the embodiment is 2.08% by high performance liquid detection, and the content of lead is less than 0.05 ppm by inductively coupled plasma mass spectrometry detection.
EXAMPLE III
The embodiment discloses a method for extracting low-lead eurycomanone from Eurycoma longifolia, which comprises the following steps:
1. crushing the raw materials, namely taking 10 kg of Eurycoma longifolia as the raw material, slicing and crushing to 8-20 meshes.
2. Extracting the fine powder with 150L 30% methanol solution at 70 deg.C for 2 times (2 h and 1 h), filtering the extractive solution with 100 mesh plate-and-frame filter, and mixing to obtain 295L mixed extractive solution.
3. Coarsely filtering, combining extractive solutions, adding 1 time of pure water, diluting, and filtering with Chinese ceramic membrane with aperture of 8 nm to obtain coarse filtrate.
4. Fine filtering, diluting the coarse filtrate with 1 time of pure water, and filtering with a rolling membrane with molecular weight of 5000 to obtain fine filtrate.
5. Removing lead, adsorbing lead with 4 series-connected resin chromatographic columns with the column volume of 8L, flowing the fine filtrate through the resin chromatographic columns at the flow rate of 32L/h, detecting the lead content in the effluent liquid to be less than 0.1ppm, and collecting 335L lead-removing feed liquid.
6. Purifying, adsorbing the lead-removing feed liquid to saturation by using a macroporous adsorption resin chromatographic column with the column volume of 20L, allowing the lead-removing feed liquid to flow through the resin chromatographic column at the flow rate of 40L/h, detecting that the content of the eurycor in the effluent liquid is more than 0.01mg/mL, washing off adsorbed saccharides and pigment impurities by using 20L of pure water, eluting by using 100L of ethanol solution with the volume concentration of 50%, allowing the ethanol solution to flow through the macroporous adsorption resin chromatographic column at the flow rate of 20L/h, and collecting 115L of eluate.
7. Concentrating, controlling temperature at 80 deg.C, and vacuum concentrating the eluate until no alcohol smell exists to obtain 6L concentrated solution.
8. Drying, spray drying the concentrated solution, with inlet air temperature of 185 deg.C, outlet air temperature of 90 deg.C, and atomizer rotation speed of 380r/s to obtain yellowish fine powder 695 g.
The content of the broad-leaved ketone in the yellowish fine powder obtained in the embodiment is 2.07 percent through high performance liquid detection, and the content of lead is less than 0.05 ppm through inductively coupled plasma mass spectrometry detection.
Claims (6)
1. A method for extracting low-lead eurycomanone from Eurycoma longifolia, which is characterized by comprising the following steps:
a. crushing the raw materials, namely taking the raw materials of Eurycoma longifolia, and crushing the Eurycoma longifolia into fine powder of 8-20 meshes;
b. extracting, namely ultrasonically extracting the raw material fine powder twice by using a methanol solution with the volume fraction of 30-50% at the temperature of 65-70 ℃, wherein the extraction time is 1-3 hours and 1-2 hours respectively, the material-liquid ratio of the raw material fine powder to the methanol solution is 1 (10-15) kg/L, filtering and combining the extracting solutions by using a plate-and-frame filter to obtain a combined extracting solution, wherein the mesh number of filter cloth of the plate-and-frame filter is 100-300 meshes;
c. coarse filtration, combining the extracting solutions, supplementing pure water for dilution, and filtering with a Chinese ceramic membrane to obtain a coarse filtrate, wherein the aperture of the Chinese ceramic membrane is 8-50 nm;
d. fine filtering, supplementing pure water to the coarse filtering liquid for dilution, and filtering by using a roll-type membrane to obtain fine filtering liquid, wherein the molecular weight of the roll-type membrane is 5000-15000;
e. removing lead, adsorbing the fine filtrate with several serially connected resin chromatographic columns, and collecting lead-removed liquid;
f. purifying, namely adsorbing the lead-removed feed liquid to saturation by using a macroporous adsorption resin chromatographic column, washing adsorbed saccharides and pigment impurities by using pure water, eluting by using an ethanol solution with the volume concentration of 50-60%, and collecting an eluent;
g. concentrating, controlling the temperature to be 70-80 ℃, and concentrating the eluent in vacuum until no alcohol smell exists to obtain a concentrated solution;
h. drying, and drying the concentrated solution to obtain fine yellowish powder.
2. The method for extracting low-lead eurycoy-lanterone from Eurycoma longifolia according to claim 1, wherein the pure water is added in the liquid in the steps c and d by 1-2 times of volume.
3. The method according to claim 1, wherein the fine filtrate in step e flows through the macroporous adsorbent resin chromatographic column at a flow rate of 4 column volumes per hour, the lead-removing feed liquid in step f flows through the macroporous adsorbent resin chromatographic column at a flow rate of 2 column volumes per hour, and the ethanol solution flows through the macroporous adsorbent resin chromatographic column at a flow rate of 1 column volume per hour.
4. The method as claimed in claim 1, wherein the step e for detecting that the content of lead in the effluent is less than 0.1ppm and the step f for detecting that the content of broad-leaved ketone in the effluent is more than 0.01 mg/mL.
5. The method for extracting low-lead eurycoy-lactone from eurycoma longifolia according to claim 1, wherein the amount of pure water is 1-3 times of the column volume and the amount of ethanol solution is 4-6 times of the column volume in step f.
6. The method for extracting low-lead eurycoy-lanugo ketone from Eurycoma longifolia according to claim 1, wherein the drying in step h is spray drying, the air inlet temperature is 185 ℃, the air outlet temperature is 90 ℃, and the rotation speed of the atomizer is 380 r/s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810388422.9A CN108484627B (en) | 2018-04-26 | 2018-04-26 | Method for extracting low-lead eurycomanone from eurycoma longifolia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810388422.9A CN108484627B (en) | 2018-04-26 | 2018-04-26 | Method for extracting low-lead eurycomanone from eurycoma longifolia |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108484627A CN108484627A (en) | 2018-09-04 |
| CN108484627B true CN108484627B (en) | 2022-04-19 |
Family
ID=63314156
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810388422.9A Active CN108484627B (en) | 2018-04-26 | 2018-04-26 | Method for extracting low-lead eurycomanone from eurycoma longifolia |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108484627B (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353296B (en) * | 2017-07-06 | 2019-03-29 | 湖南华诚生物资源股份有限公司 | A method of extracting activated protein and eurycomanone from Tongkat Ali |
-
2018
- 2018-04-26 CN CN201810388422.9A patent/CN108484627B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN108484627A (en) | 2018-09-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1974527B (en) | Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf | |
| CN101723996A (en) | Method for separating high-purity anthocyanin monomers from black rice | |
| CN101973984B (en) | Method for extracting general flavones from bamboo leaves | |
| CN102106931B (en) | Method for producing diverse extracts of berry tea | |
| CN101274953A (en) | Method for extracting corosolic acid from plant | |
| CN107793456A (en) | Anthocyanidin of extraction purification and preparation method thereof from perilla leaf | |
| CN101348474A (en) | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem | |
| CN109593110B (en) | Method for preparing naringin by using pummelo peel | |
| CN108276271B (en) | Method for simultaneously preparing high-purity carnosol and carnosic acid from rosemary | |
| CN108218948A (en) | A kind of preparation method of Sodium Aescinate | |
| CN109481478A (en) | A kind of residual ganoderan extract of low agriculture and preparation method thereof | |
| CN108484627B (en) | Method for extracting low-lead eurycomanone from eurycoma longifolia | |
| CN109320569A (en) | A method of extracting high-purity baicalin from radix scutellariae | |
| CN111440184B (en) | Method for preparing high-purity carnosol | |
| CN101658598B (en) | Method for extracting and enriching alisma total triterpenic ketone alcohol components from alisma | |
| CN104945450A (en) | Method for extracting stibene glucoside from vines of multiflower knotweeds | |
| CN108997359A (en) | A method of chlorophyll is extracted from stevioside production waste residue | |
| CN111035622B (en) | Angelica keiskei chalcone microcapsule and preparation method thereof | |
| CN114917265A (en) | Method for extracting ginsenoside | |
| CN101696381B (en) | Novel process for preparing highland barley flavone extract and application thereof in health wine | |
| CN102329346A (en) | Method for extracting echinacoside from cistanche deserticola | |
| CN109553654B (en) | The method of glycyrrhizin, licoflavone and licorice polysaccharide is extracted from Radix Glycyrrhizae | |
| CN104262448B (en) | Method for extracting glycyrrhizic acid for licorice | |
| CN106749487A (en) | A kind of method that separating ursolic acid is extracted from seabuckthorn fruit peel | |
| CN111848705A (en) | Preparation and separation method of glucoside combined-state aroma precursor substance in tea |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |