CN216062121U - High-efficient column chromatography system - Google Patents
High-efficient column chromatography system Download PDFInfo
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- CN216062121U CN216062121U CN202122764203.6U CN202122764203U CN216062121U CN 216062121 U CN216062121 U CN 216062121U CN 202122764203 U CN202122764203 U CN 202122764203U CN 216062121 U CN216062121 U CN 216062121U
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Abstract
The utility model discloses a high-efficiency column chromatography system, and belongs to the field of medical equipment. Mainly constitute by chromatography column (3), deacidification post (4), stock solution unit (10), temporary storage unit (20) and collection unit (30), stock solution unit (10), first high pressure constant current pump (1), chromatography column (3), first on-line measuring ware (5), temporary storage unit (20), second high pressure constant current pump (2), deacidification post (4), second on-line measuring ware (6) and collection unit (30) are through communicating pipe intercommunication. The utility model has scientific structure, convenient operation and wide application range, can realize automatic sample loading, elution and multi-step dynamic continuous operation, greatly improves the chromatographic efficiency and the yield and purity of target products, saves labor and materials, and has wide popularization and application prospect.
Description
Technical Field
The utility model relates to a high-efficiency column chromatography system, which is suitable for separating and purifying effective components of traditional Chinese medicines and natural medicines, belongs to the field of medical equipment,
background
Column chromatography is a separation and purification technology widely applied in the fields of biology, medicine, food and the like at present, and is a technical means for separating a mixture according to different partition coefficients of each component in the mixture in a stationary phase and a mobile phase. According to different column chromatography mechanisms, the method also comprises various forms such as adsorption chromatography, distribution chromatography, ion exchange chromatography, gel filtration chromatography and the like. However, the problems of low utilization efficiency, poor stability, low yield and the like of the chromatographic column generally exist in the prior column chromatography application process, and the large-scale application of the chromatographic technology in industrialization is severely restricted.
The ginkgo leaf extract is one of the most representative medicinal plant extracts, and the total flavone content is more than 24%, the lactone content is not less than 6% and the ginkgoic acid content is less than 5mg/kg according to the specific regulation of 2020 edition of Chinese pharmacopoeia. The ginkgo leaf extract which meets the pharmacopoeia standards has excellent effects of promoting blood circulation, removing blood stasis and dredging collaterals, and the main active ingredients of the ginkgo leaf extract, namely flavonoid compounds and terpene lactones, have the functions of improving cerebral vascular circulation, expanding coronary arteries, improving the immunity of the organism and the like, are widely applied to the fields of medicines, health-care products, food additives, functional beverages, cosmetics and the like, and have wide development prospect and higher economic and social values. However, the existing column chromatography equipment for purifying the ginkgo biloba extract only uses the gravity flow of eluent to separate and purify the crude ginkgo biloba extract, which takes long time; the chromatography process needs personnel to observe and change the elution solvent at any time, so that the chromatography efficiency is low and the labor cost is high; the flow rate of the eluent and the like needs to be adjusted manually and continuously, time and labor are wasted, and the difference between batches of the obtained products is large; in the subsequent deacidification process, the chromatographic column needs to be replaced manually, and the dynamic continuous operation of the purification, separation and deacidification process of the extract is difficult to perform.
Aiming at the defects of the existing chromatographic equipment, the column chromatographic equipment needs to be optimized and upgraded urgently, a high-efficiency column chromatography system is innovatively designed, the steps of automatic sample loading, elution, collection, detection and the like are realized, the operating efficiency of a chromatographic column is improved, the time consumed by chromatography is shortened, the purity of a target product is improved, and the batch stability of the target product is improved.
SUMMERY OF THE UTILITY MODEL
Aiming at the common technical problems that the existing column chromatography equipment can not realize automatic operation, and has long time consumption, low yield, poor stability, low purity of the obtained product and the like, the utility model provides an efficient column chromatography system for automatic sampling and elution.
The inventor carries out function integration and pipeline optimization on each unit of the existing column chromatography system, electromagnetic valves are arranged on the liquid storage unit 10, the temporary storage unit 20 and the collection unit 30 respectively, a first high-pressure constant-flow pump 1, a second high-pressure constant-flow pump 2, a first online detector 5 and a second online detector 6 are arranged on node communication pipes, and the automatic operation of operation links such as sample loading, impurity removal, elution and collection is realized by combining a digital control technology, so that the chromatography efficiency is greatly improved, and the batch stability of target products is improved.
The technical problem solved by the utility model is realized by the following technical scheme:
the utility model provides a high-efficient column chromatography system, mainly comprises chromatographic column 3, deacidification post 4, stock solution unit 10, temporary storage unit 20 and collection unit 30, its characterized in that:
the liquid storage unit 10 is communicated with a first high-pressure constant flow pump 1 through a first high-pressure constant flow pump liquid inlet pipe 101, the first high-pressure constant flow pump 1 is communicated with a chromatographic column 3 through a first high-pressure constant flow pump liquid outlet pipe 102, the chromatographic column 3 is communicated with a first online detector 5 through a first online detector liquid inlet pipe 201, the first online detector 5 is communicated with a temporary storage unit 20 through a first online detector liquid outlet pipe 202, the temporary storage unit 20 is communicated with a second high-pressure constant flow pump 2 through a second high-pressure constant flow pump liquid inlet pipe 203, the second high-pressure constant flow pump 2 is communicated with a deacidification column 4 through a second high-pressure constant flow pump liquid outlet pipe 204, and the deacidification column 4 is communicated with a second online detector 6 through a second online detector liquid inlet pipe 301; second online detector 6 communicates with collection unit 30 via second online detector effluent pipe 302.
In the present invention, the liquid storage unit 10 is formed by a first liquid storage tank 11, a second liquid storage tank 12, a third liquid storage tank 13, a fourth liquid storage tank 14, and a fifth liquid storage tank 15, which are respectively communicated with a six-way valve 7 through a first liquid storage tank communication pipe 111, a second liquid storage tank communication pipe 121, a third liquid storage tank communication pipe 131, a fourth liquid storage tank communication pipe 141, and a fifth liquid storage tank communication pipe 151 in parallel, and the six-way valve 7 is communicated with a first high-pressure constant flow pump 1 through a first high-pressure constant flow pump liquid inlet pipe 101.
The first-tank communication pipe 111, the second-tank communication pipe 121, the third-tank communication pipe 131, the fourth-tank communication pipe 141, and the fifth-tank communication pipe 151 are respectively provided with a first-tank magnetic control valve 112, a second-tank magnetic control valve 122, a third-tank magnetic control valve 132, a fourth-tank magnetic control valve 142, and a fifth-tank magnetic control valve 152.
In the utility model, the temporary storage unit 20 is formed by a first temporary storage tank 21, a second temporary storage tank 22, a third temporary storage tank 23 and a fourth temporary storage tank 24 which are respectively communicated with a five-way valve 8 in a parallel mode through a first temporary storage tank communicating pipe 211, a second temporary storage tank communicating pipe 221, a third temporary storage tank communicating pipe 231 and a fourth temporary storage tank communicating pipe 241, and the five-way valve 8 is communicated with a first online detector 5 through a first online detector liquid outlet pipe 202.
The first, second, third and fourth buffer tank communication pipes 211, 221, 231 and 241 are respectively provided with a first buffer tank magnetic control valve 212, a second buffer tank magnetic control valve 222, a third buffer tank magnetic control valve 232 and a fourth buffer tank magnetic control valve 242.
In the present invention, the collecting unit 30 is connected in parallel to the four-way valve 9 through the first, second, and third collecting tanks 31, 32, and 33 via the first, second, and third collecting tank connection tubes 311, 321, and 331, respectively, and the four-way valve 9 is connected to the second on-line detector 6 through the second on-line detector liquid inlet tube 301.
First, second, and third collection tank communication tubes 311, 321, and 331 are provided with first, second, and third collection tank magnetic control valves 312, 322, and 332, respectively.
In the innovative design and improvement processes of the high-efficiency column chromatography system, the inventor notices that the separation and purification of the existing column chromatography are realized only by the self gravity of the eluent, and the chromatography consumes long time; the chromatography process needs personnel to observe constantly, manually change an elution solvent and adjust the flow rate, the operation efficiency is low, the labor cost is high, the purification effect is unstable, and the difference between product batches is large; when the chromatographic and deacidification process is involved, the chromatographic column needs to be replaced manually, and dynamic continuous operation cannot be realized.
Aiming at the common technical problem of the column chromatography, the inventor optimizes and integrates all units of the existing column chromatography, optimizes and prepares components such as an electromagnetic valve, a high-pressure constant-flow pump, an online detector and the like through systematic pipeline connection, and realizes the continuity, the dynamism and the integration of the chromatography operation by combining with the control of a computer program.
Specifically, when the high-efficiency column chromatography system of the utility model is used for carrying out the chromatography operation of the effective components of traditional Chinese medicines and natural medicines, the column-washing purified water, the sample-loading liquid medicine, the low-concentration elution solvent, the medium-concentration elution solvent and the high-concentration elution solvent are respectively added into a first liquid storage tank 11, a second liquid storage tank 12, a third liquid storage tank 13, a fourth liquid storage tank 14 and a fifth liquid storage tank 15 of a liquid storage unit 10. Then, the opening and closing conditions and the opening and closing sequence of each magnetic control valve in the liquid storage unit 10, the temporary storage unit 20 and the collection unit 30 are respectively controlled through a program set by a central control computer, and the opening and closing conditions and the flow rate of the first high-voltage constant-current pump 1 and the second high-voltage constant-current pump 2 are respectively controlled. Meanwhile, the first online detector 5 and the second online detector 6 are connected through a central control computer, and the switching condition of the magnetic control valve, the switching condition of the high-voltage constant-current pump and the flow rate are adjusted and corrected in real time. Through the arrangement, under the control of a central control computer, a chromatography program is started, automatic operations of column washing, sample loading, impurity removal, elution, collection and detection are carried out, and finally, a target product is obtained by separation and purification from traditional Chinese medicines and natural medicines.
The chromatographic process of the present invention is further detailed below by taking the separation and purification of ginkgo biloba extract as an example:
firstly, purified water, ginkgo leaf extract, a 10% ethanol solution, a 70% ethanol solution and a 95% ethanol solution are respectively added into a first liquid storage tank 11, a second liquid storage tank 12, a third liquid storage tank 13, a fourth liquid storage tank 14 and a fifth liquid storage tank 15 of a liquid storage unit 10. According to the standard process of ginkgo biloba extract purification, the dosage of purified water, ginkgo biloba extract, 10% ethanol solution, 70% ethanol solution and 95% ethanol solution is calculated. The opening and closing of the first liquid storage tank magnetic control valve 112, the second liquid storage tank magnetic control valve 122, the third liquid storage tank magnetic control valve 132, the fourth liquid storage tank magnetic control valve 142 and the fifth liquid storage tank magnetic control valve 152 in the liquid storage unit 10, and the opening and closing and the flow rate of the first high-pressure constant flow pump 1 are respectively controlled by a program set by the central control computer.
Then, starting a preset program of the central control computer, and sequentially opening or closing the first liquid storage tank magnetic control valve 112, the second liquid storage tank magnetic control valve 122, the third liquid storage tank magnetic control valve 132, the fourth liquid storage tank magnetic control valve 142, the fifth liquid storage tank magnetic control valve 152 and the first high-pressure constant flow pump 1 according to the sequence of pure water → ginkgo leaf extract liquid → pure water → 10% ethanol → pure water → 70% ethanol elution → 95% ethanol washing column, and the like, thereby sequentially completing the process steps of pure water washing column → ginkgo leaf extract loading → pure water impurity removal → 10% ethanol impurity removal → pure water impurity removal → 70% ethanol elution → 95% ethanol washing column. The first on-line detector 5 is arranged at the lower end of the chromatographic column 3, detects the liquid flowing out of the chromatographic column 3 in real time, feeds back the detection data to the central control computer, and adjusts and corrects the switching condition of the magnetic control valve, the switching condition of the high-pressure constant flow pump and the flow rate in real time through a program of the central control computer, so that the chromatographic parameter condition is kept stable and accurate, and the chromatographic eluent of the ginkgo leaf target product is completely collected.
Meanwhile, column washing purified water, 70% ethanol eluent and 95% ethanol column washing liquid flowing out of the chromatographic column 3 respectively flow into the first temporary storage tank 21, the third temporary storage tank 23 and the fourth temporary storage tank 24 of the temporary storage unit 20 through setting of a program of a central control computer, and other liquids, such as ginkgo leaf upper column effluent liquid, ginkgo leaf upper column pure water column washing liquid, 10% ethanol impurity removal eluent and the like flow into the second temporary storage tank 22 for temporary storage and discarding.
And continuously operating the central control computer program, and sequentially opening or closing the first temporary storage tank magnetic control valve 212, the second temporary storage tank magnetic control valve 222, the third temporary storage tank magnetic control valve 232, the fourth temporary storage tank magnetic control valve 242 and the second high-pressure constant flow pump 2 according to the sequence of pure water → 70% ethanol eluent → 95% ethanol eluent, so that the process steps of pure water washing column → deacidification of 70% ethanol eluent → 95% ethanol washing column and the like are sequentially completed. The second on-line detector 6 is arranged at the lower end of the deacidification column 4, the liquid flowing out of the deacidification column 4 is detected in real time, the detection data is fed back to the central control computer, and the opening and closing conditions of the magnetic control valve, the opening and closing conditions of the second high-pressure constant flow pump 2 and the flow rate are adjusted and corrected in real time through the program of the central control computer, so that the chromatographic parameter conditions are kept stable and accurate.
Through the setting of a program of a central control computer, the column washing purified water, the 70% ethanol eluent deacidification liquid target product and the 95% ethanol column washing liquid flowing out of the deacidification column 4 respectively flow into the first collecting tank 31, the second collecting tank 32 and the third collecting tank 33 of the collecting unit 30. Wherein, the column washing purified water is discarded, the 95 percent ethanol column washing liquid is collected and recycled, the 70 percent ethanol eluent is deacidified, and the product is collected as the target.
According to the utility model, the liquid storage unit 10, the temporary storage unit 20, the collection unit 30, the chromatographic column 3, the deacidification column 4, the constant flow pump, the magnetic control valve and other node components are integrated and optimally distributed, the automation of operations such as column washing, sample loading, impurity removal, elution and collection is realized by the connection of pipelines and the arrangement of an online detection unit and the combination of a digital control technology, the labor cost is greatly saved, the chromatographic efficiency is improved, and the purity and the batch stability of a target product are improved.
The utility model has the advantages of exquisite structure, scientific and reasonable design, convenient operation, environmental protection and obvious generated technical effect, and compared with the prior conventional column chromatography equipment, the utility model has the following substantive characteristics and progresses:
1. the utility model has ingenious conception, organically combines column chromatography, a deacidification column, a high-pressure constant flow pump, a magnetic control valve and an online detector, realizes automatic sample loading, elution and dynamic continuous operation by optimizing layout and communication of pipelines, saves labor cost and time cost, greatly improves chromatography efficiency and makes large-scale production of chromatography operation possible.
2. According to the utility model, the sample to be separated and various elution solutions are pumped into the column chromatography and deacidification column by the high-pressure constant flow pump, so that the defects of low efficiency caused by the fact that the existing column chromatography system is eluted only by gravity flow of the eluent are overcome, the sample to be separated can enter the column chromatography unit at a constant speed to be fully diffused, adsorbed and separated, and the purification efficiency is greatly improved.
3. The utility model realizes the integrated operation of chromatography and deacidification, avoids the defect of manual replacement of a chromatography column, completes the separation, purification and deacidification processes of the active ingredients of the traditional Chinese medicine or natural medicine at one time, is convenient and quick, is stable and efficient, and has wide popularization and application prospects.
Drawings
In order to facilitate understanding and mastering of the technical solution of the present invention, the drawings will be briefly introduced below. It should be understood that the following drawings are not to be considered limiting of the described scope of the technical solution, and that other relevant drawings can be derived from the following drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural diagram of a high-efficiency column chromatography system
The scores in the figures are as follows:
1-a first high-pressure constant flow pump; 2-a second high-pressure constant flow pump; 3-a chromatographic column; 4-deacidifying column; 5-a first online detector; 6-a second in-line detector; 7-a six-way valve; 8-a five-way valve; a 9-four-way valve;
10-a liquid storage unit;
11-a first reservoir; 12-a second reservoir; 13-a third liquid storage tank; 14-a fourth reservoir; 15-a fifth liquid storage tank;
111-a first reservoir communication tube; 121-a second liquid storage tank communicating pipe; 131-a third liquid storage tank communicating pipe; 141-a fourth tank communication pipe; 151-fifth liquid storage tank communicating pipe;
112-a first reservoir magnetic control valve; 122-a second liquid storage tank magnetic control valve; 132-a third liquid storage tank magnetic control valve; 142-a fourth reservoir magnetic control valve; 152-fifth liquid storage tank magnetic control valve;
101-a first high-pressure constant-flow pump liquid inlet pipe; 102-a first high-pressure constant-flow pump liquid outlet pipe;
20-a temporary storage unit;
21-a first temporary storage tank; 22-a second holding tank; 23-a third temporary storage tank; 24-a fourth holding tank;
211-a first holding tank communicating tube; 221-a second holding tank communicating pipe; 231-a third holding tank communicating pipe; 241-a fourth holding tank communicating pipe;
212-a first temporary storage tank magnetic control valve; 222-a second temporary storage tank magnetic control valve; 232-a third temporary storage tank magnetic control valve; 242-fourth temporary storage tank magnetic control valve;
201-a first on-line detector liquid inlet pipe; 202-a first online detector drain;
203-a second high-pressure constant-flow pump liquid inlet pipe; 204-a second high-pressure constant-flow pump liquid outlet pipe;
30-a collection unit;
31-a first collection tank; 32-a second collection tank; 33-a third collection tank;
311-a first collection tank communication tube; 321-a second collection tank communication tube; 331-third collection tank communication tube;
312-first collection tank magnetic control valve; 322-second collection tank magnetic control valve; 332-third holding tank magnetic control valve;
301-a second on-line detector liquid inlet pipe; 302-second in-line detector drain.
Detailed Description
The following describes in further detail embodiments of the present invention with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present application clearer and clearer, the technical solutions in the embodiments will be described in detail and fully with reference to the accompanying drawings. It should be apparent that the following examples are part, but not all, of the examples of the present application. In general, the components and connections shown and described in the drawings and this embodiment may be arranged and configured in other ways, not to mention here, due to space limitations.
Therefore, the following detailed description of the embodiments does not limit the scope of the claims of the present application, and equivalents and modifications made by those skilled in the art without inventive faculty are intended to be included in the scope of the present invention.
Example 1 high-efficiency column chromatography system structure and operation mode
As shown in the attached figure 1, the high-efficiency column chromatography system mainly comprises a chromatographic column 3, a deacidification column 4, a liquid storage unit 10, a temporary storage unit 20 and a collection unit 30, the liquid storage unit 10 is communicated with a first high-pressure constant flow pump 1 through a first high-pressure constant flow pump liquid inlet pipe 101, the first high-pressure constant flow pump 1 is communicated with a chromatographic column 3 through a first high-pressure constant flow pump liquid outlet pipe 102, the chromatographic column 3 is communicated with a first online detector 5 through a first online detector liquid inlet pipe 201, the first online detector 5 is communicated with a temporary storage unit 20 through a first online detector liquid outlet pipe 202, the temporary storage unit 20 is communicated with a second high-pressure constant flow pump 2 through a second high-pressure constant flow pump liquid inlet pipe 203, the second high-pressure constant flow pump 2 is communicated with a deacidification column 4 through a second high-pressure constant flow pump liquid outlet pipe 204, and the deacidification column 4 is communicated with a second online detector 6 through a second online detector liquid inlet pipe 301; second online detector 6 communicates with collection unit 30 via second online detector effluent pipe 302.
When the high-efficiency column chromatography system is used for separating and purifying the effective components of traditional Chinese medicines and natural medicines, column-washing purified water, a sample-loading liquid medicine, a low-concentration elution solvent, a medium-concentration elution solvent and a high-concentration elution solvent are respectively added into a first liquid storage tank 11, a second liquid storage tank 12, a third liquid storage tank 13, a fourth liquid storage tank 14 and a fifth liquid storage tank 15 of a liquid storage unit 10. Then, setting programs by a central control computer, respectively controlling the switching conditions and the switching sequences of the magnetic control valves in the liquid storage unit 10, the temporary storage unit 20 and the collection unit 30, and respectively controlling the switching conditions and the flow rates of the first high-voltage constant-current pump 1 and the second high-voltage constant-current pump 2. Meanwhile, the first online detector 5 and the second online detector 6 are connected through a central control computer, and the switching condition of the magnetic control valve, the switching condition of the high-voltage constant-current pump and the flow rate are adjusted and corrected in real time. Through the setting of the parameter conditions, under the control of a central control computer, a program is started, the automatic operation of column washing, sample loading, impurity removal, elution, collection and detection is carried out, and finally, the target product is obtained by separation and purification from the traditional Chinese medicine and the natural medicine.
Taking separation and purification of ginkgo biloba extract as an example, the chromatographic operation process of the utility model is further detailed:
firstly, purified water, ginkgo leaf extract, a 10% ethanol solution, a 70% ethanol solution and a 95% ethanol solution are respectively added into a first liquid storage tank 11, a second liquid storage tank 12, a third liquid storage tank 13, a fourth liquid storage tank 14 and a fifth liquid storage tank 15 of a liquid storage unit 10. According to the purification process of the ginkgo biloba extract, the dosage of purified water, the ginkgo biloba extract, a 10% ethanol solution, a 70% ethanol solution and a 95% ethanol solution is calculated. The opening and closing of the first liquid storage tank magnetic control valve 112, the second liquid storage tank magnetic control valve 122, the third liquid storage tank magnetic control valve 132, the fourth liquid storage tank magnetic control valve 142 and the fifth liquid storage tank magnetic control valve 152 in the liquid storage unit 10, and the opening and closing and the flow rate of the first high-pressure constant flow pump 1 are respectively controlled by a program set by the central control computer.
Then, starting a preset program of the central control computer, and sequentially opening or closing the first liquid storage tank magnetic control valve 112, the second liquid storage tank magnetic control valve 122, the third liquid storage tank magnetic control valve 132, the fourth liquid storage tank magnetic control valve 142, the fifth liquid storage tank magnetic control valve 152 and the first high-pressure constant flow pump 1 according to the sequence of pure water → ginkgo leaf extract liquid → pure water → 10% ethanol → pure water → 70% ethanol elution → 95% ethanol washing column, and the like, thereby sequentially completing the process steps of pure water washing column → ginkgo leaf extract loading → pure water impurity removal → 10% ethanol impurity removal → pure water impurity removal → 70% ethanol elution → 95% ethanol washing column. The first online detector 5 is arranged at the lower end of the chromatographic column 3, detects liquid flowing out of the chromatographic column 3 in real time, feeds detection data back to the central control computer, and adjusts and corrects the switching condition of the magnetic control valve, the switching condition of the high-pressure constant flow pump and the flow rate in real time through a program of the central control computer, so that the chromatographic parameter condition is kept stable and accurate, and chromatographic eluent of a target product of ginkgo leaves is completely collected.
Meanwhile, column-washing purified water, 70% ethanol eluent and 95% ethanol column-washing liquid flowing out of the chromatographic column 3 respectively flow into the first temporary storage tank 21, the third temporary storage tank 23 and the fourth temporary storage tank 24 of the temporary storage unit 20 through program setting of a central control computer, and other liquids, such as ginkgo leaf-feeding column-feeding effluent liquid, ginkgo leaf-feeding column-feeding pure water column-washing liquid, 10% ethanol impurity-removing eluent and the like flow into the second temporary storage tank 22 for temporary storage and discarding.
And continuously operating the central control computer program, and sequentially opening or closing the first temporary storage tank magnetic control valve 212, the second temporary storage tank magnetic control valve 222, the third temporary storage tank magnetic control valve 232, the fourth temporary storage tank magnetic control valve 242 and the second high-pressure constant flow pump 2 according to the sequence of pure water → 70% ethanol eluent → 95% ethanol eluent, so that the process steps of pure water washing column → deacidification of 70% ethanol eluent → 95% ethanol washing column and the like are sequentially completed. The second on-line detector 6 is arranged at the lower end of the deacidification column 4, the liquid flowing out of the deacidification column 4 is detected in real time, the detection data is fed back to the central control computer, and the opening and closing conditions of the magnetic control valve, the opening and closing conditions of the second high-pressure constant flow pump 2 and the flow rate are adjusted and corrected in real time through the program of the central control computer, so that the chromatographic parameter conditions are kept stable and accurate.
Through the setting of a program of a central control computer, the column washing purified water, the 70% ethanol eluent deacidification liquid target product and the 95% ethanol column washing liquid flowing out of the deacidification column 4 respectively flow into the first collecting tank 31, the second collecting tank 32 and the third collecting tank 33 of the collecting unit 30. And removing column washing purified water, collecting and recovering 95% ethanol column washing liquid, and removing acid liquid from 70% ethanol eluate to obtain the target collection product.
Example 2 study of column chromatography integration System for purification of Ginkgo biloba leaf extract
1 Material
Ginkgo biloba extract, available from pharmaceutical research and development center, of the company, qianpu, runan, inc (ginkgo biloba, available from santa robusta, ltd, tanzhou, mountain east); LX-158 and LX-02 macroporous resins (Xian lan Xiao science and technology materials Co., Ltd.); 36X 920mm protein compression column and 200mL microflow reactor pump (Shanghai Satsuka separation technology Co., Ltd.).
2 method
2.1 purification of Ginkgo biloba extract by conventional column chromatography
Column assembling: a clean protein compression column was taken and packed tightly and uniformly into LX-158 macroporous resin (column volume about 540mL) (this step can be omitted for a regenerated chromatography column).
Punching the column: the microflow reactor pump was set at a flow rate of 35mL/min, and the column was washed with pure water (this step can be omitted for a new column).
Loading: setting the pump flow of the microflow reactor to be 25mL/min, and taking a processed ginkgo leaf extract sample to load the chromatographic column in the step I.
And (3) elution: after the sample loading is finished, the column is washed by 1500mL of pure water and 1500mL of 10% ethanol (20 ℃) in sequence at the flow rate of 25 mL/min; eluting with 70% ethanol (20 deg.C), and receiving eluate (discarding the first 200mL), stopping elution until the volume of eluate is 1500 mL; finally, the column is washed and regenerated by 95% ethanol (20 ℃) at the flow rate of 35mL/min, after the eluent completely flows out and the adsorbent is dried, LX-158 macroporous resin is poured into a specified container, and the chromatographic column is cleaned and dried.
Column assembling: according to the method of the step I, the column is reloaded by LX-02 macroporous resin.
Deacidifying: and (4) directly loading the eluent in the step (A) to the chromatographic column in the step (B) at the flow rate of 25mL/min, deacidifying and receiving the chromatographic solution.
2.2 purification of Ginkgo biloba extract by high efficiency column chromatography
Preparing equipment: purified water, a ginkgo biloba leaf extract sample, a 10% ethanol solution, 70% ethanol and a 95% solution are respectively added into a first liquid storage tank 11, a second liquid storage tank 12, a third liquid storage tank 13, a fourth liquid storage tank 14 and a fifth liquid storage tank 15 in the liquid storage unit 10, and normal connection among the equipment components is ensured.
Program setting: during the period of opening the first liquid storage tank magnetic control valve 112, the second liquid storage tank magnetic control valve 122, the third liquid storage tank magnetic control valve 132, the fourth liquid storage tank magnetic control valve 142 and the fifth liquid storage tank magnetic control valve 152, the first high-pressure constant flow pump 1 pumps out 1500mL of purified water at a flow rate of 35mL/min, pumps out the treated ginkgo biloba extract with the same amount as 2.1, 1500mL of purified water, 1500mL of 10% ethanol (20 ℃) and 1700mL of 70% ethanol (20 ℃) at a flow rate of 25mL/min, and pumps out 95% ethanol (20 ℃) at a flow rate of 35 mL/min. Meanwhile, when the first online detector 5 is set to detect pure water, impurity-removed pure water, a 10% ethanol solution and a 95% ethanol solution, the first temporary storage tank magnetic control valve 212, the second temporary storage tank magnetic control valve 222 and the fourth temporary storage tank magnetic control valve 242 are respectively opened. When 70% ethanol is detected, the second temporary storage tank magnetic control valve 222 is opened first 8min later, and then the third temporary storage tank magnetic control valve 232 is opened later. And the second high-pressure constant-current pump 2 is set during the opening period of the first temporary storage tank magnetic control valve 212, the second temporary storage tank magnetic control valve 222 and the fourth temporary storage tank magnetic control valve 242, and keeps running at the flow rate of 25 mL/min; when the second online detector 6 detects purified water, 70% ethanol and 95% ethanol, the first collection tank magnetic valve 312, the second collection tank magnetic valve 322 and the third collection tank magnetic valve 332 are respectively opened, and purified water, 70% ethanol eluent deacidification liquid (target product) and 95% ethanol eluent are respectively collected.
2.3 statistical methods data analysis was performed using GraphPad Prism Software version 5(GraphPad Software, USA) with results expressed as mean. + -. standard deviation. P <0.05 was considered statistically different and P <0.01 was considered statistically significantly different.
3 results
As shown in Table 1, the ginkgo biloba extract purified by the conventional column chromatography equipment and the high-efficiency column chromatography system of the utility model has the total flavone content of more than 24 percent, the lactone content of more than 6 percent and the ginkgoic acid content of less than 5mg/kg, and meets the pharmacopoeia standard. Compared with the ginkgo leaf extract purified by the conventional column chromatography equipment, the ginkgo leaf extract purified by the column chromatography integrated system has the advantages that the flavone content (P is less than 0.05), the lactone content (P is less than 0.05) are obviously higher, the ginkgoic acid content (P is less than 0.05) is obviously lower, the purification time consumption (P is less than 0.01) is obviously shorter, and the yield (P is less than 0.05) is obviously higher, so that the purification efficiency is improved, the purity of a target product is improved, and the labor cost and the material cost are saved. In addition, the fluctuation of flavone content, lactone content, time consumption and yield in the experimental result is obviously smaller, which shows that the application of the high-efficiency column chromatography system for purifying the ginkgo leaf extract can improve the batch stability of the target product.
TABLE 1 yield, flavone content, lactone content, ginkgolic acid content and time consuming comparison
Note: compared with the conventional column chromatography equipment, "+" indicates that P <0.05, and "+" indicates that P < 0.01.
Claims (7)
1. The utility model provides a high-efficient column chromatography system mainly comprises chromatographic column (3), deacidification post (4), stock solution unit (10), temporary storage unit (20) and collection unit (30), its characterized in that:
the liquid storage unit (10) is communicated with a first high-pressure constant flow pump (1) through a first high-pressure constant flow pump liquid inlet pipe (101), the first high-pressure constant flow pump (1) is communicated with a chromatographic column (3) through a first high-pressure constant flow pump liquid outlet pipe (102), the chromatographic column (3) is communicated with a first on-line detector (5) through a first on-line detector liquid inlet pipe (201), the first on-line detector (5) is communicated with a temporary storage unit (20) through a first on-line detector liquid outlet pipe (202), the temporary storage unit (20) is communicated with a second high-pressure constant flow pump (2) through a second high-pressure constant flow pump liquid inlet pipe (203), the second high-pressure constant flow pump (2) is communicated with a deacidification column (4) through a second high-pressure constant flow pump liquid outlet pipe (204), and the deacidification column (4) is communicated with a second on-line detector (6) through a second on-line detector liquid inlet pipe (301); the second on-line detector (6) is communicated with the collecting unit (30) through a second on-line detector liquid outlet pipe (302).
2. The high-efficiency column chromatography system according to claim 1, wherein the liquid storage unit (10) is formed by a first liquid storage tank (11), a second liquid storage tank (12), a third liquid storage tank (13), a fourth liquid storage tank (14) and a fifth liquid storage tank (15) which are respectively communicated with the six-way valve (7) in a parallel mode through a first liquid storage tank communicating pipe (111), a second liquid storage tank communicating pipe (121), a third liquid storage tank communicating pipe (131), a fourth liquid storage tank communicating pipe (141) and a fifth liquid storage tank communicating pipe (151), and the six-way valve (7) is communicated with the first high-pressure constant flow pump (1) through a first high-pressure constant flow pump liquid inlet pipe (101).
3. The high-efficiency column chromatography system of claim 2, wherein the first-tank communicating pipe (111), the second-tank communicating pipe (121), the third-tank communicating pipe (131), the fourth-tank communicating pipe (141) and the fifth-tank communicating pipe (151) are respectively provided with a first-tank magnetic control valve (112), a second-tank magnetic control valve (122), a third-tank magnetic control valve (132), a fourth-tank magnetic control valve (142) and a fifth-tank magnetic control valve (152).
4. The high-efficiency column chromatography system of claim 1, wherein the temporary storage unit (20) is composed of a first temporary storage tank (21), a second temporary storage tank (22), a third temporary storage tank (23) and a fourth temporary storage tank (24) which are respectively communicated with a five-way valve (8) through a first temporary storage tank communicating pipe (211), a second temporary storage tank communicating pipe (221), a third temporary storage tank communicating pipe (231) and a fourth temporary storage tank communicating pipe (241) in a parallel connection manner, and the five-way valve (8) is communicated with the first online detector (5) through a first online detector liquid outlet pipe (202).
5. The high-efficiency column chromatography system according to claim 4, wherein the first temporary storage tank communicating pipe (211), the second temporary storage tank communicating pipe (221), the third temporary storage tank communicating pipe (231) and the fourth temporary storage tank communicating pipe (241) are respectively provided with a first temporary storage tank magnetic control valve (212), a second temporary storage tank magnetic control valve (222), a third temporary storage tank magnetic control valve (232) and a fourth temporary storage tank magnetic control valve (242).
6. The high efficiency column chromatography system according to claim 1, wherein the collection unit (30) is connected in parallel to a four-way valve (9) by a first collection tank (31), a second collection tank (32) and a third collection tank (33) via a first collection tank connection pipe (311), a second collection tank connection pipe (321) and a third collection tank connection pipe (331), respectively, and the four-way valve (9) is connected to the second on-line detector (6) via a second on-line detector liquid inlet pipe (301).
7. The high efficiency column chromatography system of claim 6, wherein the first collection tank connection pipe (311), the second collection tank connection pipe (321) and the third collection tank connection pipe (331) are respectively provided with a first collection tank magnetic control valve (312), a second collection tank magnetic control valve (322) and a third collection tank magnetic control valve (332).
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| CN202122764203.6U CN216062121U (en) | 2021-11-12 | 2021-11-12 | High-efficient column chromatography system |
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| CN202122764203.6U CN216062121U (en) | 2021-11-12 | 2021-11-12 | High-efficient column chromatography system |
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