Method for extraction of Chinese herbal medicine using small molecule micro-shear technology

Abstract

A method for extraction of Chinese herbal medicines using a small molecule micro-shear technology, including: pretreating, jet milling, grinding, pulverizing, cell-wall breaking, and extraction of Chinese herbal medicines, so that the raw material can be fully utilized. Herbs are cut into small molecule substances, which is easy to be absorbed by the means of a superfine grinding technology and a cell-wall breaking technology. By means of a supercritical carbon dioxide extraction technology, active ingredients in Chinese herbal medicines can be efficiently and singly extracted, and organic solvent residues in the raw herbs can be removed.

Claims

1. A method for extraction of Chinese herbal medicines using small molecule micro-shear technology, comprising: (1) pretreating 500 g forsythia raw materials removed of mildew and impurity until the moisture content 8.0%; (2) initially pulverizing the Chinese herbal medicinal material until it can pass through a 200 mesh sieve; (3) pulverizing the pulverized medicinal material by a supersonic jet mill, and a gas flow pressure is between 0.1 and 0.8 MPa; (4) adding 2-3 wt % of maltase and 1-2 wt % of 65% ethanol solution of oxalic acid to a pulverized powder, grinding them into a slurry, then filtering and recovering the slurry; (5) treating a mixture obtained in the step (4) by using an ultra-fine lamination ball mill for 10-15 min; (6) putting 120 mL of propylene glycol and materials treated by the ultra-fine lamination ball mill into an extraction kettle of a supercritical fluid extractor, and the supercritical fluid flow rate into the extraction kettle is 40 L/h, the temperature of the extraction kettle is 52 C., and the pressure is 32 MPa, the time of extraction with supercritical fluid is 7 h; (7) taking the fluid from the extraction kettle into middle of a separation column to separate the fluid by a first stage, wherein the separation column has a pressure of 12 MPa and a temperature of 65 C.; (8) taking the fluid passed through the separation column into a stirred first separation kettle to separate it by a second stage, wherein the first separation kettle has a pressure of 5.5 MPa and a temperature of 55 C.; and (9) taking the fluid separated by the first separation kettle enters a stirred second separation kettle, wherein the second separation kettle has a pressure of 5 MPa and a temperature of 45 C.

2. The method for extraction of Chinese herbal medicines using small molecule micro-shear technology of claim 1, wherein the gas flow pressure is 0.2-0.5 MPa.

Description

DESCRIPTION OF THE EMBODIMENTS

Example 1

(1) (1) Pretreating 500 g panax notoginseng raw materials removed of mildew and impurity until the moisture content 8.0%.

(2) (2) Initially pulverizing the Chinese herbal medicines material until it can pass through a 200 mesh sieve.

(3) (3) Pulverizing the pulverized medicinal material by a supersonic jet mill, and the gas flow pressure is between 0.1 and 0.8 MPa.

(4) (4) Adding 2-3 wt % of maltase and 1-2 wt % of 65% ethanol solution of oxalic acid to the pulverized powder, grinding them into a slurry, then filtering and recovering the slurry.

(5) (5) Treating the mixture obtained in the step (4) by using an ultra-fine lamination ball mill for 10-15 min.

(6) (6) Putting 120 mL of propylene glycol and the materials treated by the ultra-fine lamination ball mill into the extraction kettle of the supercritical fluid extractor, and the supercritical fluid flow rate into the extraction kettle is 40 L/h, the temperature of the extraction kettle is 52 C., and the pressure is 32 MPa, the time of extraction with supercritical fluid is 7 h.

(7) (7) Taking the fluid from the extraction kettle into the middle of the separation column to separate the fluid by the first stage. The separation column has a pressure of 12 MPa and a temperature of 65 C.

(8) (8) Taking the fluid passed through the separation column into a stirred first separation kettle to separate it by the second stage. The first separation kettle has a pressure of 5.5 MPa and a temperature of 55 C.

(9) (9) Taking the fluid separated by the first separation kettle enters the stirred second separation kettle. The second separation kettle has a pressure of 5 MPa and a temperature of 45 C.

Example 2

(10) (1) Pretreating 500 g pinellia ternate raw materials removed of mildew and impurity until the moisture content 8.0%.

(11) (2) Initially pulverizing the Chinese medicinal material until it can pass through a 200 mesh sieve.

(12) (3) Pulverizing the pulverized medicinal material by a supersonic jet mill, and the gas flow pressure is between 0.2 and 0.5 MPa.

(13) (4) Adding 2-3 wt % of trypsin and 1-2 wt % of 65% ethanol solution of oxalic acid to the pulverized powder, grinding them into a slurry, then filtering and recovering the slurry.

(14) (5) Treating the mixture obtained in the step (4) by using an ultra-fine lamination ball mill for 10-15 min.

(15) (6) Putting 120 mL of propylene glycol and 250 g materials treated by the ultra-fine lamination ball mill into the extraction kettle of the supercritical fluid extractor, and the supercritical fluid flow rate into the extraction kettle is 40 L/h, the temperature of the extraction kettle is 52 C., and the pressure is 32 MPa, the time of extraction with supercritical fluid is 7 h.

(16) (7) Taking the fluid from the extraction kettle into the middle of the separation column to separate the fluid by the first stage. The separation column has a pressure of 12 MPa and a temperature of 65 C.

(17) (8) Taking the fluid passed through the separation column into a stirred first separation kettle to separate it by the second stage. The first separation kettle has a pressure of 5.5 MPa and a temperature of 55 C.

(18) (9) Taking the fluid separated by the first separation kettle enters the stirred second separation kettle. The second separation kettle has a pressure of 5 MPa and a temperature of 45 C.

(19) Test Example 1

(20) The forsythia was extracted by the method of Example 1 of the present invention and the method of Example 1 of Patent No. 2009101934934 (Control), and the therapeutic effects of both on the swelling of the ear shell skin of the mouse were examined. The experimental steps are as follows:

(21) Experimental principle: Using inflammatory agents to cause swelling of the ear skin, and the weight of the inflamed ear shell of the applied medicine group and the control group was observed and measured, and the difference in swelling rate was compared.

(22) Operation Method:

(23) (1) Male mice of 25 to 30 g were used.

(24) (2) Under anesthesia of ether, about 0.1 mL the mixed pro-inflammatory solution was applied to both sides of the left ear of the mouse (The inflammation solution contains 2% croton oil, 20% pyridine, 5% distilled water and 73% diethyl ether). The right ear is used as a control.

(25) (3) 0.03 mL/kg of test drug was injected intraperitoneally 0.5-1 hour before the inflammation.

(26) (4) After 4 h, the mice were sacrificed, and the ears were cut. The original ear pieces were taken off with a 9 mm diameter puncher on the same part, and weighed with a balance. The weight of the left ear piece per mouse minus the weight of the right ear piece is the degree of swelling. The mean value and standard deviation of the swelling degree of each group were calculated, and the swelling inhibition rate of the administration group was determined according to the formula. The formula is: swelling rate a=(inflamed ear weightuninflamed ear weight)/uninflamed ear weight.

(27) (5) Both the applied drug and the control group were diluted to 1%.

(28) The experimental results are as follows:

(29) TABLE-US-00001 Number of Swelling Drug animals rate Example 1 20 0.67 0.05 Example 2 18 0.73 0.09 Control group 18 1.62 0.12

(30) From the above results, it was found that the swelling rates of the mouse ear pieces prepared by the method of the present invention were all lower than that of the control group. The pulverization and extraction method of the present invention allows the effective ingredients in the Chinese herbal medicines to be completely retained and fully utilized, so that the obtained drug has a remarkable effect.

(31) The detailed description of the present invention is intended to be illustrative of the preferred embodiments of the present invention, and is not intended to limit the scope of the present invention. Equivalent implementation or modification without departing from the invention shall be included in the scope of the technical scheme of the invention.