CN101575337A

CN101575337A - Process for extracting matrine or nicotine

Info

Publication number: CN101575337A
Application number: CNA2009100121518A
Authority: CN
Inventors: 张国林
Original assignee: Individual
Current assignee: Individual
Priority date: 2009-06-18
Filing date: 2009-06-18
Publication date: 2009-11-11
Anticipated expiration: 2029-06-18
Also published as: CN101575337B

Abstract

The invention discloses a process for extracting matrine or nicotine. The method comprises the extraction principle that alkaloid exists in cytoplasm, extraction of the alkaloid at normal pressure is a process of infiltrating and dissolving, so the time is long, and the efficiency is low; after pressure is applied, solvent can be pressed into a cell; when the pressure is reduced, liquid in the cell can be vaporized and expanded, the cell is burst, solute is taken out, and the alkaloid is extracted; when the pH of the alkaloid is between 10 and 12, the alkaloid can be extracted by methyl chloride; and when the pH of the alkaloid is between 1 and 2, the alkaloid can be extracted back by water phase. Compared with the prior extraction method, the process has the characteristics of short extraction time, low cost and high yield.

Description

A kind of technology of extracting matrine or nicotine

Technical field

The invention belongs to the alkaloid technical field of natural drug, particularly a kind of technology of extracting matrine or nicotine.

Background technology

At present, preparing the method for matrine, mainly is extraction separation and purifying from Chinese medicine leguminous plants kuh-seng, Herba Sophorae alopecuroidis and root of subprostrate sophora.Generally have normal pressure alcohol to extract and two kinds of other water extraction, wherein to extract soak time be tens hours to normal pressure alcohol, and the organism quantity discharged is many, the cost height, and poor product quality, yield are not high; Other water extraction need consume a large amount of fuel, contaminate environment, production cost height.Because alkaloid is present in the tenuigenin, and normal pressure extracts alkaloid, be an infiltration dissolved process, so the time is long, efficient is low, and after the pressurization, solvent just can be pressed in the cell, when decompression, intracellular liquid will be vaporized, be expanded, and cell is burst, solute is taken out of, and alkaloid is extracted out.Alkaloid is 10～12 o'clock at PH, can be extracted by methyl chloride, and be can be stripped by water in 1～2 o'clock at PH.

Summary of the invention

The object of the present invention is to provide a kind of technology of extracting matrine or nicotine that a kind of extraction time is short, cost is low, yield is high.

Technical scheme of the present invention is as follows:

A kind of technology of extracting matrine or nicotine, form by following steps:

1,5～30 orders that will pulverize in pressure cylinder contain alkaloidal herbal medicine, as water submergences such as kuh-seng, tobacco, the Radixs Astragali, and be that the water vapor of 0.1～0.4Mpa feeds direct heating in the pressure cylinder with gauge pressure, the pressure in cylinder is identical with the pressure of water vapour, is incubated 5～30 minutes;

2, with the direct spraying cooling in cylinder of 10～35 ℃ cold water, carry out step-down, or directly with gas in the jar emptying step-down, add water vapor after the step-down again and feed direct heating pressurization in the pressure cylinder, pressure in cylinder is identical with the pressure of water vapour, emits 20～40% of the interior liquid of cylinder, and is incubated 5～30 minutes, and then spray into cold water or transformation is next time carried out in emptying, 3～5 times like this;

3, it is 1～2 that the solution of emitting in the cylinder is added acid adjusting PH, static cooling 12 hours, precipitated impurities, extract supernatant liquor, adding NaOH adjusting PH is 10～12,0.02%～0.5% the emulsion splitter that adds the supernatant liquor quality, as Sodium dodecylbenzene sulfonate, sodium laurylsulfonates etc. add extraction agent then, and the ratio of general supernatant liquor and extraction agent is 5～8: 1, reverse extraction 3～5 times, after separating organic phase, add entry, the ratio of general organic phase and water is 5: 1, and add acid and regulate PH and 1～2 carry out back extraction, reverse extraction 2～3 times, after the water phase separated, it is 10～12 that water adds NaOH adjusting PH, use the reverse extraction of extraction agent 3～5 times again, the ratio of general water and extraction agent is 5: 1;

4, separate organic phase, it is 40～60% matrine or nicotine that evaporation obtains purity, for next step purification.

The invention has the advantages that:

1, with normal pressure alcohol extract phase ratio:

A, leaching time were reduced to 2.5～3.5 hours by tens hours production cycles.

B, the discharging of minimizing organism reduce cost, and are example with the matrine, and matrine per ton reduces cost 40～500,000 yuan.

The quality and the yield of C, product increase substantially: content brings up to 40～60% by 5～7%, and yield is brought up to about 96% by 85～87%.

2, compare with other water extraction:

A, a large amount of fuel of saving effectively reduce and discharge SO in air ₂, CO ₂Deng.

The quality and the yield of B, product increase substantially: content brings up to 40～60% by 5～7%, and yield is brought up to about 96% by 85～87%.

C, leaching time were reduced to 2.5～3.5 hours by tens hours production cycles.

D, cost reduce significantly.

Embodiment

Below the invention will be further described.

Embodiment 1 contains matrine 1.1% in the 20kg kuh-seng, makes the aqueous solution 220～240kg, as stated above, adds 0.02% emulsion splitter of aqueous solution quality, and the employing methylene dichloride is an extraction agent, and the ratio of the aqueous solution and methylene dichloride is 5: 1, obtains sample.

Sample: weight: 514.7g content: 41.0% is pure: 211.2g

Yield: 211.2/220=96%

Nicotine: 20kg tobacco leaf, tobacco leaf contain nicotine 2.3%, make aqueous solution 260kg, as stated above, add 0.02% emulsion splitter of aqueous solution quality, and the employing methylene dichloride is an extraction agent, and the ratio of the aqueous solution and methylene dichloride is 5: 1, obtains sample.

Sample: weight: 787.8g content: 57.1% is pure: 450g

Yield: 450/460=97.8%

Embodiment 2 contains matrine 1.1% in the 20kg kuh-seng, makes the aqueous solution 220～240kg, as stated above, adds 0.5% emulsion splitter of aqueous solution quality, and the employing trichloromethane is an extraction agent, and the ratio of the aqueous solution and methylene dichloride is 8: 1, obtains sample.

Sample: weight: 514.9g content: 40.8% is pure: 210.1g

Yield: 210.1/220=95%

Nicotine: 20kg tobacco leaf, tobacco leaf contain nicotine 2.3%, make aqueous solution 260kg, as stated above, add 0.02% emulsion splitter of aqueous solution quality, and the employing trichloromethane is an extraction agent, and the ratio of the aqueous solution and methylene dichloride is 8: 1, obtains sample.

Sample: weight: 769.8g content: 57.3% is pure: 441.1g

Yield: 441.1/460=95.9%

In the foregoing description methylene dichloride, trichloromethane also replaceable be tetracol phenixin.

Claims

1, a kind of technology of extracting matrine or nicotine is characterized in that being made up of following steps:

A, 5～30 orders that will pulverize in pressure cylinder contain the submergence of alkaloidal herbal medicine water, and are that the water vapor of 0.1～0.4Mpa feeds direct heating in the pressure cylinder with gauge pressure, and the pressure in cylinder is identical with the pressure of water vapour, is incubated 5～30 minutes;

B, with the direct spraying cooling in cylinder of 10～35 ℃ cold water, carry out step-down, or directly with gas in the jar emptying step-down, add water vapor after the step-down again and feed direct heating pressurization in the pressure cylinder, pressure in cylinder is identical with the pressure of water vapour, emits 20～40% of the interior liquid of cylinder, and is incubated 5～30 minutes, and then spray into cold water or transformation is next time carried out in emptying, 3～5 times like this;

C, it is 1～2 that the solution of emitting in the cylinder is added acid adjusting PH, static cooling 12 hours, precipitated impurities, extract supernatant liquor, adding NaOH, to regulate PH be 10～12, adds 0.02%～0.5% emulsion splitter of supernatant liquor quality, add extraction agent then, the ratio of general supernatant liquor and extraction agent is 5～8: 1, and reverse extraction 3～5 times is after the separation organic phase, add entry, the ratio of general organic phase and water is 5: 1, and adds acid and regulate PH and 1～2 carry out back extraction, reverse extraction 2～3 times, after the water phase separated, it is 10～12 that water adds NaOH adjusting PH, uses the reverse extraction of extraction agent 3～5 times again, and the ratio of general water and extraction agent is 5: 1;

D, separate organic phase, it is 40～60% matrine or nicotine that evaporation obtains purity, for next step purification.

2, a kind of technology of extracting matrine or nicotine according to claim 1, it is characterized in that: described emulsion splitter is Sodium dodecylbenzene sulfonate or sodium laurylsulfonate.

3, a kind of technology of extracting matrine or nicotine according to claim 1, it is characterized in that: described extraction agent is methylene dichloride, trichloromethane or tetracol phenixin.