阅读说明：本技术 一种穿琥宁雾化剂原料的提纯工艺 (Purification process of potassium dehydroandrographolide succinate atomizing agent raw material ) 是由 蒋达博 范伟川 张庆坤 李永东 胡平 吴照军 梁星 岳苗闯 张安玲 陈熙英 于 2020-12-25 设计创作，主要内容包括：本发明公开了一种穿琥宁雾化剂原料的提纯工艺,解决了现有的穿琥宁药品因为其原料不纯导致纯度不高,不利于用药,甚至产生副作用的技术问题。本发明包括如下步骤：将穿心莲草颗粒采用提取溶剂进行动态提取得到提取液,再将提取液进行脱色、浓缩和结晶纯化,得到精制的穿心莲内脂,所述脱色和浓缩工序之间还设置有PP微孔过滤处理。本发明具有穿心莲内脂的纯度高、产率高等优点。(The invention discloses a purification process of potassium dehydroandrographolide succinate aerosol raw materials, which solves the technical problems that the conventional potassium dehydroandrographolide succinate medicine is not high in purity due to impure raw materials, is not beneficial to medication and even generates side effects. The invention comprises the following steps: dynamically extracting herba Andrographitis granule with extraction solvent to obtain extractive solution, decolorizing, concentrating, crystallizing, and purifying to obtain refined andrographolide, wherein PP microporous filtration treatment is provided between decolorizing and concentrating processes. The method has the advantages of high purity, high yield and the like of andrographolide.)

1. A purification process of potassium dehydroandrographolide succinate atomizing agent raw materials is characterized by comprising the following steps: dynamically extracting herba Andrographitis granule with extraction solvent to obtain extractive solution, decolorizing, concentrating, crystallizing, and purifying to obtain refined andrographolide, wherein PP microporous filtration treatment is provided between decolorizing and concentrating processes.

2. The process for purifying a potassium dehydroandrographolide succinate aerosol raw material as claimed in claim 1, wherein the step of dynamically extracting specifically comprises:

step 1: firstly, starting an air draft device to blow air so that the soft bag body (6) is bulged;

step 2: adding an extraction solvent into the outer cylinder (1), and adding herba andrographitis particles into the inner frame (2);

and step 3: starting an air draft device to suck air;

and 4, step 4: the motor (4) is started to rotate to drive the inner frame (2) to rotate;

and 5: extracting for 2-4 hours;

step 6: collecting the extractive solution.

3. The process for purifying potassium dehydroandrographolide succinate aerosol raw material according to claim 1 or 2, wherein the size of the andrographis paniculata particles is 2-3 cm.

4. The purification process of potassium dehydroandrographolide succinate atomizing agent raw material as claimed in claim 2, wherein a plurality of through holes are formed in the inner frame (2), and the diameter of each through hole is 0.8-1 mm.

5. The process for purifying potassium dehydroandrographolide succinate atomizing agent raw material as claimed in claim 1 or 2, wherein the process between step 4 and step 5 further comprises the following steps: the air draft device is opened at intervals to blow and suck air.

6. A purification process of potassium dehydroandrographolide succinate raw material as claimed in claim 5, wherein the time of blowing and air suction is 10-30S.

7. The purification process of potassium dehydroandrographolide succinate aerosol raw material as claimed in claim 1 or 2, wherein the pore size of the PP microfiltration membrane subjected to PP microfiltration treatment is 0.22-0.45 mm.

8. The purification process of potassium dehydroandrographolide succinate aerosol raw material as claimed in claim 1 or 2, wherein the extraction solvent is methanol or ethanol.

9. The purification process of potassium dehydroandrographolide succinate aerosol raw material as claimed in claim 1 or 2, wherein the extraction temperature of the extraction solvent is 60-70 ℃.

10. The process for purifying potassium dehydroandrographolide succinate aerosol raw material as claimed in claim 2, wherein the treatment steps of the extracting solution are as follows:

s1: decolorization of

Adding the extracting solution into an activated carbon column for decoloring to obtain a decoloring solution;

s2: PP microporous filtration treatment

Filtering the decolorized solution in the S1 through PP micropores to obtain a filtrate;

s3: concentrating

Distilling and concentrating the filtrate to obtain a concentrated solution;

s4: crystallization of

Adding low-melting-point solvent into the concentrated solution in S3, stirring, and crystallizing at low temperature to obtain refined andrographolide.

Technical Field

The invention relates to the technical field of purification of potassium dehydroandrographolide succinate raw materials, and discloses a purification process of potassium dehydroandrographolide succinate aerosol raw materials.

Background

The potassium dehydroandrographolide succinate is white to light yellow solid, is used by immune system, has strong antipyretic effect on rabbits with fever caused by bacterial endotoxin, can promote the regression of fever, and can be used for treating diseases such as viral pneumonia and viral upper respiratory tract infection.

The potassium dehydroandrographolide succinate can be injected in the using process, can be used for treating respiratory tract infection through aerosol inhalation of the respiratory tract, and is easy to cause respiratory tract infection along with serious environmental pollution, so the potassium dehydroandrographolide succinate is used as an aerosol increasingly, but if the purity is not enough, adverse reactions are easy to cause.

Andrographolide is prepared by reacting andrographolide with potassium succinate anhydride, and andrographolide is extracted from herba Andrographitis, but the purity of andrographolide is not high due to impure raw materials and poor control of preparation process.

Therefore, in order to improve the purity of the potassium dehydroandrographolide succinate, improvement on raw materials and preparation processes is needed.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: the existing potassium dehydroandrographolide succinate medicine is not high in purity due to impure raw materials, is not beneficial to administration, and even has side effects.

The invention can be realized by the following technical scheme:

a purification process of potassium dehydroandrographolide succinate atomizing agent raw materials comprises the following steps: dynamically extracting herba Andrographitis granule with extraction solvent to obtain extractive solution, decolorizing, concentrating, crystallizing, and purifying to obtain refined andrographolide, wherein PP microporous filtration treatment is provided between decolorizing and concentrating processes.

According to the invention, impurities are removed by adopting PP microporous filtration between the decolorization and crystallization processes, and refined andrographolide can be obtained by crystallization, so that the crystallization load can be reduced.

The invention preferably discloses a purification process of potassium dehydroandrographolide succinate atomizing agent raw materials, and the dynamic extraction step specifically comprises the following steps:

step 1: firstly, starting an air draft device to blow air so as to enable the soft capsule body to swell;

step 2: adding the extraction solvent into the outer cylinder, and adding the andrographis paniculata particles into the inner frame;

and step 3: starting an air draft device to suck air;

and 4, step 4: starting a motor to rotate to drive the inner frame to rotate;

and 5: extracting for 2-4 hours;

step 6: collecting the extractive solution.

The invention preferably relates to a purification process of a potassium dehydroandrographolide succinate aerosol raw material, wherein the size of andrographis paniculata particles is 2-3 cm.

The invention preferably discloses a purification process of a potassium dehydroandrographolide succinate atomizing agent raw material, wherein a plurality of through holes are formed in the inner frame, and the diameter of each through hole is 0.8-1 mm.

The extraction process is carried out in special equipment, firstly the soft capsule body is swelled, then corresponding materials are added into the outer barrel and the inner frame, the extraction solvent in the outer barrel can move towards the inner frame, but the movement of the extraction solvent can be blocked due to the small size of the through holes in the inner frame, so that the air suction device is controlled to suck air, the volume of the soft capsule body can be shrunk and reduced, the extraction solvent in the outer barrel can more easily enter the inner frame under the pressure difference, then the inner frame is rotated, the inner frame moves relative to the extraction solvent, namely the extraction solvent is pressurized and enters the inner frame, further, the contact between the extraction solvent and the andrographis paniculata particles in the inner frame is improved, and the extraction of the andrographis paniculata lactone is better realized.

The invention preferably discloses a purification process of potassium dehydroandrographolide succinate atomizing agent raw material, which further comprises the following steps between the step 4 and the step 5: the air draft device is opened at intervals to blow and suck air.

In the invention, when the inner frame rotates in the outer cylinder, the andrographis paniculata granules are not fully mixed in the extraction solvent possibly due to the action of centrifugal force, are easy to stick to the wall of the inner frame or gather to the bottom of the inner frame due to gravity, and the soft capsule body can expand and contract in the inner frame through the air blowing and air suction of the air draft device, so that the surge phenomenon can be formed on the andrographis paniculata granules and the extraction solvent in the inner frame, the mixing effect is realized, and the extraction effect of andrographis paniculata lactone is more favorably improved.

The invention preferably relates to a purification process of potassium dehydroandrographolide succinate atomizing agent raw material, and the air blowing time and the air suction time are both 10-30S.

The interval time is short, the surge phenomenon is more obvious, and the mixing effect is better.

The invention preferably relates to a purification process of a potassium dehydroandrographolide succinate atomizing agent raw material, wherein the pore diameter of a PP microporous filtering membrane subjected to PP microporous filtering treatment is 0.22-0.45 mm.

According to the method, the andrographolide is decolored by activated carbon and simultaneously absorbs some impurities, then the impurities in the andrographolide can be further removed by a filter membrane with a small pore diameter, and finally crystallization is carried out for three times of purification, so that the andrographolide with a good purification effect is obtained.

The invention preferably relates to a purification process of a potassium dehydroandrographolide succinate atomizing agent raw material, and the extraction solvent is methanol or ethanol.

The invention preferably selects a purification process of the potassium dehydroandrographolide succinate atomizing agent raw material, and the extraction temperature of the extraction solvent is 60-70 ℃.

The invention preferably discloses a purification process of a potassium dehydroandrographolide succinate atomizing agent raw material, and the treatment steps of the extracting solution are as follows:

s1: decolorization of

Adding the extracting solution into an activated carbon column for decoloring to obtain a decoloring solution;

s2: PP microporous filtration treatment

Filtering the decolorized solution in the S1 through PP micropores to obtain a filtrate;

s3: concentrating

Distilling and concentrating the filtrate to obtain a concentrated solution;

s4: crystallization of

Adding low-melting-point solvent into the concentrated solution in S3, stirring, and crystallizing at low temperature to obtain refined andrographolide.

The extraction device used in the purification process comprises an outer barrel and an inner frame, wherein the inner frame is positioned in the outer barrel, a rotating shaft is arranged at the bottom of the inner frame, one end of the rotating shaft extends out of the outer barrel and is connected with a rotating motor, a soft bag body is arranged in the inner frame, a vent pipe is connected onto the soft bag, an air draft device is connected onto the vent pipe, and a controller is arranged on the air draft device and is used for controlling the air draft device to blow air and suck air.

Compared with the prior art, the invention has the following advantages and beneficial effects:

1. the invention increases the purity of andrographolide by adding PP microporous filtration between decolorization and crystallization.

2. According to the invention, in the extraction process of the andrographis paniculata particles, pressure difference is realized through structure improvement and process adjustment, and the mixing of the andrographis paniculata lactone particles and an extraction solvent is realized through inner frame rotation, so that the extraction rate of andrographis paniculata lactone is improved.

3. According to the invention, the air blowing and air suction of the air draft device are controlled at intervals, so that the stirring effect of andrographolide grass particles in the inner frame in the extraction solvent is realized, and the extraction rate of andrographolide is improved.

4. The invention realizes high extraction rate and high purity of andrographolide by improving the steps of extracting and purifying andrographolide.

Drawings

The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:

FIG. 1 is a schematic view of the structure of the extraction apparatus of the present invention.

Part names in the drawings:

1-outer cylinder, 2-inner frame, 3-rotating shaft, 4-motor, 5-vent pipe, 6-soft capsule, 7-solvent inlet, 8-extract outlet.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.

Example 1

A purification process of potassium dehydroandrographolide succinate atomizing agent raw materials comprises the following steps:

(1) preparation of herba Andrographitis granule

Crushing 11kg of herba Andrographitis raw material to obtain 10kg of herba Andrographitis granule with size of 2-3 cm, or purchasing herba Andrographitis granule with size of the above size.

(2) Preparation of andrographolide extract

Step 1: the air extracting device is started to blow air, so that the soft bag body 6 is inflated.

Step 2: adding 95% ethanol into the outer barrel 1, wherein the adding height is 80% of that of the outer barrel 1, adding the andrographis paniculata granules into the inner frame 2, and the adding height is as follows: when the capsule body is completely swelled, the added andrographis paniculata particles are positioned at the position of the extension line of the short axis of the elliptic soft capsule body 6.

And step 3: starting an air draft device to suck air;

after the air suction, the space of the inner frame 2 is enlarged, the pressure is reduced, and then the ethanol in the outer cylinder 1 can enter the inner frame 2 more easily under a certain pressure.

And 4, step 4: starting a motor 4 to rotate, driving an inner frame 2 to rotate, starting an air draft device at intervals to blow air and suck air, wherein the air blowing time and the air suction time are both 15S, and starting heating to keep the temperature of an extraction solvent at 65 ℃;

the inner frame 2 rotates, the speed that the ethanol in the outer barrel 1 enters the inner frame 2 can be improved, the contact force between common andrographis herb particles and the ethanol is increased due to the rotation of the inner frame 2, common andrographis herb lactone in the common andrographis herb particles can be extracted, air blowing and air suction through the air suction device can enable the soft capsule body 6 to expand and contract in the inner frame 2, surge phenomena can be formed on the common andrographis herb particles and the extraction solvent in the inner frame 2, mixing effect is achieved, and the extraction effect of the common andrographis herb lactone is improved.

And 5: extracting for 3 hours;

step 6: collecting the extracting solution,

opening the valve at the bottom of the outer cylinder 1 to discharge the andrographolide extracting solution.

Adding the extraction solvent again, performing secondary extraction, discharging the andrographolide extract obtained in the secondary extraction, and combining the andrographolide extract obtained in the first extraction and the andrographolide extract obtained in the second extraction to obtain the final andrographolide extract.

(3) Decolorization of

Adding the andrographolide extracting solution into an activated carbon column, wherein the volume ratio of the andrographolide extracting solution to the activated carbon is 3:1, and obtaining a destaining solution.

(4) PP microporous filtration

And (3) filtering the decolorized solution through a PP (polypropylene) microporous filter membrane to obtain a filtrate, wherein the pore diameter of the PP microporous filter membrane is 250 microns.

(5) Concentrating

And (3) carrying out reduced pressure distillation on the filtrate under the conditions of: the temperature is 65 ℃, the vacuum degree is 0.05MPa,

to obtain 1.82kg of a concentrated solution.

(6) Crystallization of

95% ethanol solution was added to the concentrated solution, and after stirring, low-temperature crystallization was performed to obtain 312g of refined andrographolide.

Example 2

This example differs from example 1 in that a conventional extraction screw extractor was used, and the resulting concentrate was 1.64kg, and 293g of andrographolide after final crystallization was obtained.

The content was checked by HPLC and the yield was calculated as shown in Table 1 below.

As can be seen from the above Table 1, the present invention improves the extraction apparatus, the extraction method and the purification method to obtain andrographolide with high yield and purity.

As shown in fig. 1, the extraction device used in the purification process of the present invention comprises an outer cylinder 1 and an inner frame 2, wherein the inner frame 2 is located in the outer cylinder 1, a rotating shaft 3 is arranged at the bottom of the inner frame 2, one end of the rotating shaft 3 extends out of the outer cylinder 1 and is connected with a rotating motor 4, a soft bag body 6 is arranged in the inner frame 2, the soft bag is connected with a vent pipe 5, the vent pipe 5 is connected with an air draft device, and the air draft device is provided with a controller for controlling the air draft device to blow and suck air.

The outer barrel 1 is provided with a solvent inlet 7 and an extracting solution outlet 8, and heating elements are arranged around the outer barrel 1 and used for heating the extracting solvent.

In addition, in order to facilitate sealing and disassembly, a detachable first cover body is arranged at the bottom of the outer barrel 1, a detachable second cover body is arranged at the top of the inner frame 2, and a ventilation pipe 5 connected in a rotating and sealing manner is connected to the first cover body.

The soft bag body 6 is made of soft silica gel, and the thickness of the soft silica gel is 2-3 mm.

The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.