CN103980291B - Method for extracting moringa from Moringa root - Google Patents

Abstract

The method of pterygospermim lai is extracted from Moringa root, the present invention relates to a kind of method that subcritical technology extracts the pterygospermim lai in Moringa, 1) Moringa root is pulverized, load filter basket, drop in subcritical abstraction still, airtight extraction kettle, adds organic extractant, is warming up to extraction liquid in subcritical abstraction still and is in subcritical state; After extraction extraction terminates, be decompressed to vacuum tightness 0.01 ~ 0.1Mpa recycling design, obtain brown color leach liquor.2) in brown color leach liquor, to add etc. the sorbent material of quality, absorption pterygospermim lai, uses eluent sorbent material, and eluent is removed in decompression, obtains yellow medicinal extract.3) silicagel column on medicinal extract, with ethanol-dichloromethane, the ascending gradient elution of methanol dichloromethane elutriant polarity, collects the cut that pterygospermim lai content is greater than 97%, obtains the pterygospermim lai of pterygospermim lai content more than 98% with ethyl alcohol recrystallization.Product foreign matter content is few and biological activity is high, and extraction efficiency is high, the operational cycle is short, energy-and time-economizing, the extraction agent rate of recovery are high.

Description

Method for extracting moringa from Moringa root

technical field

The invention belongs to the separation and purification of natural products, in particular to a method for extracting active substance moringa in moringa.

Background technique

Moringa (moringaoleifera) is native to India and Africa, also known as the drumstick tree, is a plant of the genus Moringa in the Moringaceae family, and has the reputation of "diamonds in plants". The whole plant of Moringa oleifera has different effects. Currently known medical effects include regulating blood pressure, lowering cholesterol, anti-cancer, enhancing immune defense, hypoglycemic effect, regulating thyroid hormone, antioxidant activity, antibacterial effect, contraception and abortion, etc. Wait. In addition, it is rich in protein, vitamins and amino acids, and its nutritional value is equivalent to that of spirulina, which is called "the miniature treasure house of human nutrition" by modern nutritionists. Wood has extremely high economic value.

The effect of the biologically active substance moringa in the root of Moringa is also quite amazing. It can be confirmed that the moringa contained in moringa has obvious bactericidal effect, and can be developed into natural cleaners and biopesticides, while the discarded residue can be used as soil improver and organic fertilizer. The alkaloids and moringa contained in the water extract of seeds and roots can effectively inhibit Pseudomonas, Staphylococcus aureus and Escherichia coli. In addition, moringa seed oil can be applied to small wounds due to its moringa content to prevent inflammation and prevent infection from suppurating. The most important thing is that the root bark contains moringaine, zeatin, quercetin (flavin), β-sitosterol, chlorogenic acid, Indian moringa and kaempferol, etc., which have anti-tumor and promote sex hormone secretion. Effective for diabetics and thyroid disease. Moringa seeds have been proven in traditional medicine to treat fevers and abdominal tumors. In addition, the alkaloids and moringanin in the root of the Moringa tree are often used to make medicines for paralysis, intermittent fever, chronic rheumatism, and are also used to treat nervous disorders, vertigo, intestinal spasms, hysteria, and flatulence Swelling, as well as contraceptive and hypoglycemic effects.

The molecular formula of Moringa is C ₂₂ H ₁₈ N ₂ S ₂ O ₂ . It is soluble in water-emulsion alcohol and has a melting point of 15 degrees Celsius. The chemical name is: 2,9-dibenzyl-1,8-dioxa-2,9-diaza-dispiro[3.2.3.2]dodeca-5,11-diene-3,10-di Thione, molecular weight is 406.529, its molecular structure is as follows:

Molecular structure of Moringa

Although there are abundant introductions about the effects of moringa in the literature of various countries, there are few methods for the separation and purification of moringa. The invention provides a simple and effective method for extracting moringan from the root of Moringa oleifera. The method is as follows: dry and pulverize the root of Moringa oleifera oleifera, use subcritical extraction to obtain the extract, use an adsorbent to adsorb the moringanin, then use an eluent to elute the adsorbent, pass the obtained crude product through a silica gel column, and then use The organic liquid is recrystallized, and finally the finished product of moringa with high purity is obtained.

It involves sub-critical fluid extraction technology, a new type of extraction and separation technology. It uses sub-critical fluid as an extraction agent, and in a closed, oxygen-free, low-pressure pressure vessel, according to the principle of similar solubility of organic matter, through extraction The molecular diffusion process of the material and the extractant during the soaking process makes the fat-soluble components in the solid material transfer to the liquid extractant, and then the extractant is separated from the target product through the process of vacuum evaporation, and finally the target product is obtained.

Compared with other traditional separation methods, subcritical subcritical fluid extraction has many advantages: high extraction efficiency, non-toxic and harmless, low extraction temperature, it is also applicable to the extraction of heat-sensitive substances and can retain the active components of the extract without damage or oxidation, The operation cost is low, the production continuity is good, and it is convenient for large-scale industrial production. Because of the above advantages, subcritical extraction technology has been applied to the extraction of many active ingredients of natural products.

Chinese patent No. 200910094239.9 discloses a method for extracting lam protein from Moringa oleifera seeds. The method is as follows: mix Moringa oleifera seed powder with water, add enzyme, and bathe in water for 12-48 hours to balance the pH After the pH = 7 to 9, centrifuge and take the supernatant; adjust the supernatant to pH = 10 to 12 again, discard the supernatant and remove the precipitate. Moringa protein is dried. The method is simple and easy to operate. But do not relate to the extraction of moringa in Moringa.

Contents of the invention

The purpose of the present invention is to provide a method for extracting and separating from Moringa oleifera and obtaining high-purity large moringa. The method is simple, easy to scale up production, can extract high-purity and high-quality moringa, and can be used for large-scale industrial production.

Above-mentioned purpose of the present invention can be realized by following technical scheme:

The method for extracting moringan from the root of Moringa oleifera, the steps are as follows:

1) Crush the root of Moringa oleifera, put it into a filter basket, put it into a subcritical extraction kettle, seal the extraction kettle, add an organic extractant, adjust the solid-liquid ratio to 1:5-1:20 (g:ml), and adjust the vacuum in the container The temperature is 0.06～0.1Mpa, and the temperature is raised until the extract in the subcritical extraction kettle is in a subcritical state; extraction is performed 2 to 3 times, and the extraction time is 1 to 5 hours each time. After the extraction is completed, the extracted solution is put into the solvent recovery kettle , depressurize to a vacuum of 0.01-0.1Mpa to recover the solvent, and obtain a brown-yellow leachate;

2) Add an equal mass of adsorbent to the brown-yellow leaching solution to absorb moringa, elute the adsorbent with an eluent that is 5 times the mass of the adsorbent, remove the eluent, and depressurize to a vacuum degree of 0.01-0.1Mpa Remove the eluent to obtain a yellow extract;

3) Put the medium yellow extract in 2) on a silica gel column, elute with a gradient from small to large polarity of the eluent, detect, collect fractions with a moringan content greater than 97%, concentrate to dry powder, and then recrystallize with ethanol 2 ~4 times to obtain a moringan product with a moringan content of more than 98%.

The organic extractant is aqueous methanol (v:v=7:3-10:0) or aqueous ethanol (v:v=7:3-10:0).

The adsorbent is bamboo-based activated carbon or coal-based activated carbon.

The eluent is diethyl ether or petroleum ether.

The silica gel is 200-300 mesh, dissolved in twice the volume of the eluent, and ultrasonically debubbled.

The gradient elution rate is 0.2-3 mL/min.

The eluent is ethanol-dichloromethane or methanol-dichloromethane with a volume ratio of 50:50 to 99.9:1.

In the step 1) the temperature of the closed subcritical extraction kettle is raised to 80-200°C, and the pressure is 108kPa-4048kPa.

The subcritical extraction equipment is a subcritical extraction complete set of equipment.

Advantages of using this method to extract moringa and the beneficial effects produced:

1. The present invention relates to the extraction and fine separation of Moringa, more targeted extraction and utilization of biologically active substances in Moringa.

2. The present invention adopts subcritical extraction technology. Compared with the traditional extraction method, the utilization rate of the solvent is improved, the solvent is saved, the extraction temperature is reduced, and the sample decomposition caused by long-term high temperature is avoided. The extraction rate is fast and the efficiency is high. Moreover, the structure is simple, the operation is convenient, and at the same time, the advantages of supercritical fluid extraction are retained, the active ingredients are fully extracted, and the waste of material resources is reduced.

3. After the product is obtained, it is subjected to column chromatography to further ensure the purity and product yield of the extracted moringa.

4. Methanol and ethanol are used as extraction agents, and ethanol is recovered and reused for gradient elution and recrystallization, which reduces the amount of impurities introduced, efficiently utilizes extraction agents, and saves resources.

5. Gradient elution of the eluent shortens the analysis period, improves the separation ability, and obtains more pure moringa. At the same time, water and ethanol are non-toxic, and dichloromethane is the least toxic of methane chlorides, which not only reduces the harm to the human body, but also reduces environmental pollution.

Description of drawings

Figure 1: Flowchart of Moringa Extraction Operation.

Figure 2: Schematic diagram of methanol subcritical fluid extraction technology, conventional extraction, and supercritical fluid extraction operation area.

Figure 3: Schematic diagram of ethanol subcritical fluid extraction technology, conventional extraction, and supercritical fluid extraction.

The following are specific embodiments of the present invention, and the examples are to further describe the present invention, but the scope of protection claimed by the present invention is not limited to the following embodiments.

specific embodiment

The technical scheme of the present invention will be further described below in conjunction with specific embodiments:

Rinse the fresh Moringa oleifera roots (taken from the plantation field), dry them in an oven (30° C.) after natural air drying. Pulverize, stir and sieve (preferably 100 mesh sieves), and the gained Moringa oleifera root powder is sealed and preserved.

Example 1

Get 150g of Moringa root powder, put it into a filter basket, put it into a CBE-5L type subcritical extraction kettle, add 1072ml of ethanol with a volume fraction of 70%, adjust the vacuum to 0.06Mpa, heat up to 80°C, and extract twice, each time The time is 10 minutes. Each time the obtained extract is put into a solvent recovery kettle, the pressure is reduced to a vacuum of 0.01Mpa, and the solvent is recovered to obtain a black-green leachate. Then weigh 1g of coal-based activated carbon and place it in a beaker, add 1g of Moringa oleifera root subcritical extract, stir to make it adsorb, then add 5g of petroleum ether eluent to elute the activated carbon to obtain an extract-like substance. Take 1 g of the extract and put it on a silica gel column, and use a dichloromethane-ethanol solution with a volume ratio of 50:50 to 99.9:0.1 for gradient elution from small to large polarity, and the elution rate is 0.2ml/min. When the volume ratio of methane-methanol is appropriate, an off-white solid can be obtained, which can be recrystallized twice with methanol to obtain 1.153 mg of the product with a content of 98.5%.

Example 2

Get Moringa oleifera root powder 150g, put into filter basket, drop into subcritical extraction kettle, add volume fraction and be 80% ethanol 2000ml, adjust vacuum degree to be 0.08Mpa, be warming up to 120 ℃, extract twice, each time is 30min, Each time the obtained extract is put into a solvent recovery kettle, the pressure is reduced to a vacuum of 0.01Mpa, and the solvent is recovered to obtain a black-green leachate. Then take by weighing 20g of bamboo-based activated carbon and place it in a beaker, add in the subcritical extract of 20g of Moringa oleifera root, stir to make it adsorb, then add 100g of ether to elute the activated carbon to obtain an extract-like substance. Take 2 g of the extract and put it on a silica gel column, and use a dichloromethane-ethanol solution with a volume ratio of 50:50 to 99.9:0.1 for gradient elution from small to large polarity, and the elution rate is 2ml/min. - When the volume ratio of methanol is appropriate, an off-white solid is obtained, which is recrystallized three times with methanol to obtain 21.09 mg of the product, with a content of 98.2%.

Example 3

Get Moringa oleifera root powder 150g, put into filter basket, drop into subcritical extraction kettle, add volume fraction and be 80% ethanol 3000ml, adjust vacuum degree to be 0.08Mpa, be warming up to 150 ℃, extract twice, each time is 40min, Each time the obtained extract is put into a solvent recovery kettle, the pressure is reduced to a vacuum of 0.01Mpa, and the solvent is recovered to obtain a black-green leachate. Then take by weighing 20g of coal-based activated carbon and place it in a beaker, add in the subcritical extract of 20g of Moringa oleifera root, stir to make it adsorb, and then add 100g of petroleum ether to elute the activated carbon to obtain an extract-like substance. Take 1.3 g of the extract and put it on a silica gel column, and use a dichloromethane-ethanol solution with a volume ratio of 50:50 to 99.9:0.1 for gradient elution from small to large polarity, and the elution rate is 2ml/min. When the volume ratio of methane-methanol is appropriate, an off-white solid can be obtained, which can be recrystallized three times with methanol to obtain 12.20 mg of the product with a content of 99.0%.

Example 4

Get Moringa root powder 150g, put into filter basket, drop into subcritical extraction kettle, add volume fraction and be 100% ethanol 3000ml, adjust vacuum degree to be 0.1Mpa, be warming up to 200 ℃, extract three times, each time is 50min, every time The extracted solution obtained for the second time was put into a solvent recovery kettle, and the pressure was reduced to a vacuum degree of 0.1Mpa, and the solvent was recovered to obtain a black-green leaching solution. Then take by weighing 20g of bamboo-based activated carbon and place it in a beaker, add in the subcritical extract of 20g of Moringa oleifera root, stir to make it adsorb, then add 100g of ether to elute the activated carbon to obtain an extract-like substance. Take 1000g of the extract and put it on a silica gel column, and use dichloromethane-ethanol with a volume ratio of 50:50 to 99.9:0.1 for gradient elution from small to large polarity, and the elution rate is 3ml/min. When the methanol volume ratio is appropriate, an off-white solid is obtained, which is recrystallized 4 times with methanol to obtain 10.25 g of the product with a content of 99.1%.

Claims (7)

1. the method for extracting moringan from the root of Moringa oleifera, is characterized in that the steps are as follows: 1) Crush the root of Moringa oleifera, put it into a filter basket, put it into a subcritical extraction kettle, seal the extraction kettle, add an organic extractant, adjust the solid-liquid ratio to 1:5-1:20 (g:ml), and adjust the vacuum in the container The temperature is 0.06～0.1Mpa, and the temperature is raised until the extract in the subcritical extraction kettle is in a subcritical state; extraction is performed 2 to 3 times, and the extraction time is 1 to 5 hours each time. After the extraction is completed, the extracted solution is put into the solvent recovery kettle , depressurize to a vacuum of 0.01-0.1Mpa to recover the solvent, and obtain a brown-yellow leachate; 2) Add an equal mass of adsorbent to the brown-yellow leaching solution to absorb moringa, elute the adsorbent with an eluent that is 5 times the mass of the adsorbent, remove the eluent, and depressurize to a vacuum degree of 0.01-0.1Mpa Remove the eluent to obtain a yellow extract; 3) Put the medium yellow extract in 2) on a silica gel column, elute with a gradient from small to large polarity of the eluent, detect, collect fractions with a moringan content greater than 97%, concentrate to dry powder, and then recrystallize with ethanol 2 ~4 times to obtain a moringan product with a moringan content of more than 98%; The organic extractant is aqueous methanol v:v=7:3-10:0 or aqueous ethanol v:v=7:3-10:0. 2. The method according to claim 1, characterized in that the adsorbent is bamboo-based activated carbon or coal-based activated carbon. 3. The method according to claim 1, characterized in that the eluent is ether or sherwood oil. 4. The method according to claim 1, characterized in that the silica gel is 200-300 mesh, dissolved in twice the volume of the eluent, and ultrasonically debubbled. 5. The method according to claim 1, characterized in that the gradient elution rate is 0.2-3 mL/min. 6. The method according to claim 1, characterized in that the eluent is ethanol-dichloromethane or methanol-dichloromethane with a volume ratio of 50:50 to 99.9:1. 7. The method according to claim 1, characterized in that in step 1) the temperature of the closed subcritical extraction tank is raised to 80-200°C, and the pressure is 108kPa-4048kPa.