CN209927802U - Multi-channel integrated liquid phase chromatographic column device - Google Patents

Multi-channel integrated liquid phase chromatographic column device Download PDF

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Publication number
CN209927802U
CN209927802U CN201920676237.XU CN201920676237U CN209927802U CN 209927802 U CN209927802 U CN 209927802U CN 201920676237 U CN201920676237 U CN 201920676237U CN 209927802 U CN209927802 U CN 209927802U
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China
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liquid
box body
way valve
column
pipe
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Expired - Fee Related
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CN201920676237.XU
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Chinese (zh)
Inventor
满勇
刘洁
巴凯凯
郝伟
张卓琳
郭滢
张铃钰
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Henan University of Technology
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Henan University of Technology
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Abstract

The utility model discloses a multichannel integrated liquid chromatographic column device, which comprises a box body with an opening at the front end, wherein an electric heating pipe is coiled on the rear wall of the box body, a plurality of analysis type high performance liquid chromatographic columns, namely analysis columns, are arranged in the box body at parallel intervals, a box door is hinged on the side wall of the box body at the opening, and the top end of each analysis column is connected with a liquid outlet branch pipe; the bottom ends of the analytical columns are respectively connected with a liquid inlet header pipe through a liquid separating mechanism, and the liquid inlet header pipe extends out of the side wall of the box body and is connected with a conveying pump; the utility model discloses synthesize the effectual advantage that advances the appearance volume with the preparation post of analytical column separation, overcome analytical column appearance volume little and preparation type high performance liquid chromatography post and prepare the relatively poor defect of post separation effect promptly, once separate and be equivalent to former multiple separation, high-efficient and convenient, can once separate out multiple compound of wanting, practice thrift the separation cost of complicated compound.

Description

Multi-channel integrated liquid phase chromatographic column device
Technical Field
The utility model relates to a high performance liquid preparative chromatography technical field.
Background
The method for preparing the liquid chromatogram has become an important separation and analysis technology in the subject fields of chemistry, biochemistry, medicine, industry, agriculture, environmental protection, commodity inspection, legal inspection and the like, and is an essential tool for workers in analytical chemistry, biochemistry and environmental chemistry. Taking medicines as an example, in the pharmacopoeia of the people's republic of China, the quality control of more than about 600 chemical synthetic medicines and more than about 400 traditional Chinese medicines is applied to a liquid chromatography method, but because the contradiction between the sample treatment capacity and the sample separation efficiency of the traditional preparation chromatography is not solved, the sample treatment capacity is inevitably reduced to obtain a better separation and purification effect, so that the separation is complicated, the cost is increased, and the prices of some related medicines prepared by liquid phases in the market are very expensive.
Currently, high performance liquid chromatographs are only equipped with analytical columns (i.e., analytical high performance liquid chromatography columns), semi-preparative columns, or preparative columns. When the preparation column is used for separating some complex compounds, the separation effect cannot reach the expected separation effect. The analytical column can achieve good separation effect, but the sample size is small, so that the preparation time is long, and the number of mobile phases is large, so that the application of the analytical column in preparing liquid phase is limited. It is a general technical realization for those skilled in the art that analytical columns are used for conducting analytical tests, preparative columns are used for liquid phase preparation, analytical columns and preparative columns are not commonly available.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a multichannel integrated liquid chromatography column device both has good separation effect, has the advantage that the volume of advancing is big, preparation ability is high again.
In order to realize the aim, the multichannel integrated liquid phase chromatographic column device comprises a box body with an open front end, and an electric heating pipe is coiled on the rear wall of the box body;
an electric fan is arranged in the box body in front of the electric heating pipe, a plurality of analysis columns are arranged in the box body in front of the electric fan at intervals in parallel, a box door is hinged to the side wall of the box body at an opening, the box door comprises a door frame and double-layer transparent materials embedded in the door frame, and a cavity is formed between the double-layer transparent materials;
the top end of each analysis column is connected with a liquid outlet branch pipe, each liquid outlet branch pipe is collected into a liquid outlet pipe bundle, the liquid outlet pipe bundle is led out of the box body, one liquid outlet branch pipe in the liquid outlet pipe bundle is used for being connected with an external liquid chromatography detector, and other liquid outlet branch pipes in the liquid outlet pipe bundle are led into a collecting container outside the box body;
the bottom end of each analytical column is connected with a liquid inlet header pipe through a liquid separating mechanism, and the liquid inlet header pipe extends out of the side wall of the box body and is connected with a conveying pump for conveying the mobile phase;
electric heating pipe and electric fan all are connected with an electrically controlled device, and electrically controlled device is connected with display screen and temperature sensor, and electrically controlled device and display screen all are located the box outer wall, and temperature sensor is located inside the box.
A metal pore plate is arranged in the box body between the analysis column and the electric fan, a plurality of small holes are uniformly distributed in the metal pore plate, and two metal pore plates are symmetrically arranged up and down.
The analytical columns are arranged side by side at intervals, and the liquid separation mechanism adopts any one of the following two structures:
a. the liquid separating mechanism comprises a multi-way valve, the multi-way valve is provided with a liquid inlet and a plurality of liquid outlets, and the liquid outlets of the multi-way valve are communicated with the analysis columns in a one-to-one correspondence manner; the liquid inlet of the multi-way valve is connected with a liquid inlet header pipe;
b. the liquid separating mechanism comprises a plurality of three-way valves, and each three-way valve comprises a liquid inlet and two liquid outlets; taking the liquid flowing direction as a downstream direction, connecting a liquid inlet of the three-way valve positioned at the most upstream with a liquid inlet header pipe, and correspondingly communicating two liquid outlets of one three-way valve at the relatively upstream with liquid inlets of two three-way valves at the relatively downstream in the three-way valves connected along the upstream and downstream directions; the total number of liquid outlets of all the three-way valves at the most downstream is the same as the number of the analytical columns and is communicated in a one-to-one correspondence manner.
The utility model discloses an integrated liquid chromatographic column device of multichannel is in parallel with a plurality of analytical columns through multi-ported valve isotructure and is in the same place, total sample throughput has been improved, the advantage that analytical column separation effect is good and preparation post sample input volume is big has been synthesized, the defect that analytical column sample input volume is little and preparation post separation effect is relatively poor has been overcome, primary separation can be equivalent to original multiple separation operation, high efficiency and make things convenient for the use of chromatographic column, can once separate out multiple compound of wanting, practice thrift the separation cost of complicated compound, this is to the detection of arriving national department greatly, pharmaceutical preparation (reduce the medicine preparation cost, reduce the medicine price), little to the living environment, all have very big meaning.
An air interlayer is arranged between the double layers of transparent materials, so that the heat insulation performance of the box door is improved, and the operating personnel can observe the working condition of each analysis column through the box door conveniently.
The metal pore plate plays the effect of convenient fixed chromatographic column on the one hand, and the metal pore plate plays even heat dissipation effect again on the one hand, utilizes the good heat conductivility of metal to make everywhere temperature more even in the box, and porous structure is favorable to the circulation of air, and the air current that the electric fan arouses flows through aperture and the space outside two metal pore plates, gives off the heat that electric heating pipe produced to the box space everywhere evenly.
Liquid separating mechanism simple structure, it is even to join in marriage liquid, and the part that uses such as pipeline, multi-way valve and three-way valve are parts commonly used in the laboratory, and it is all very convenient to maintain and change.
Drawings
FIG. 1 is a schematic structural view of a multi-channel integrated liquid chromatography column apparatus of the present invention with the door removed;
FIG. 2 is a schematic left side view of the multi-channel integrated liquid chromatography column assembly with the electronic control unit and display screen removed;
fig. 3 is an electric control schematic diagram of the present invention;
FIG. 4 is a graph showing the effect of separating a triflurouracil nucleotide solution upon preparation;
FIG. 5 is a graph showing the analytical results of the purified products obtained from each analytical column of the multi-channel integrated liquid chromatography column apparatus; in the figure, each wavy line from top to bottom is an analysis effect curve of a purified product obtained by a No. 1-4 analytical column respectively;
FIG. 6 is a comparative analysis chart of the purified product obtained from each analytical column and the preparative column of the multi-channel integrated liquid chromatography column apparatus. Four wavy lines from top to bottom in the figure are respectively the analysis effect curves of the purified product obtained by the No. 1-4 analytical column; the bottom (i.e., the fifth line from top to bottom) of the waveform is the curve of the analytical effect of the purified product obtained from the preparative column.
Detailed Description
As shown in fig. 1 to 6, the multichannel integrated liquid chromatography column device of the present invention comprises a box body 1 with an open front end, an electric heating tube 2 is coiled on the rear wall of the box body 1, an electric fan 3 is arranged in the box body 1 in front of the electric heating tube 2, a plurality of analysis columns 4 are arranged in the box body 1 in front of the electric fan 3 at parallel intervals, a box door is hinged on the side wall of the box body 1 at the open position, the box door comprises a door frame 5 and a double-layer transparent material 6 embedded in the door frame 5, and a cavity 7 is arranged between the double-layer; the transparent material is glass, preferably organic glass.
The top end of each analytical column 4 is connected with a liquid outlet branch pipe 8, the liquid outlet branch pipes are collected into a liquid outlet pipe bundle 9, the liquid outlet pipe bundle 9 is led out of the box body, one liquid outlet branch pipe in the liquid outlet pipe bundle 9 is used for being connected with an external liquid chromatography detector, and other liquid outlet branch pipes in the liquid outlet pipe bundle 9 are led into a collecting container 10 outside the box body 1; the collection vessel 10 is preferably a collection bottle and the liquid chromatography detector is a conventional device, not shown.
The bottom end of each analytical column 4 is respectively connected with a liquid inlet main pipe 11 through a liquid separating mechanism, and the liquid inlet main pipe 11 extends out of the side wall of the box body 1 and is connected with a conveying pump for conveying mobile phases; the transfer pump is conventional and not shown.
The electric heating pipe 2 and the electric fan 3 are both connected with an electric control device 12, the electric control device 12 is connected with a display screen 13 and a temperature sensor 14, the electric control device 12 and the display screen 13 are both positioned on the outer wall of the box body 1, and the temperature sensor 14 is positioned inside the box body 1.
The cavity 7 is arranged between the double-layer transparent materials 6, so that the heat insulation performance of the box door is improved, and the operating personnel can observe the working condition of each analysis column 4 through the box door conveniently.
The electric control device 12 is a 86-degree computer or a single chip microcomputer, and a PLC can also be adopted.
A metal orifice plate 15 is arranged in the box body 1 between the analysis column 4 and the electric fan 3, a plurality of small holes 16 are uniformly distributed on the metal orifice plate 15, and two metal orifice plates 15 are symmetrically arranged up and down. The left and right ends of the metal orifice plate 15 are fixedly connected to the side wall of the box body 1. The small holes 16 facilitate fixing screws for fixing the analytical column 4 and facilitate air convection in the box body 1.
A plurality of analysis columns are arranged side by side at intervals, specifically 4 in the embodiment; the liquid separation mechanism adopts any one of the following two structures:
a. the liquid separating mechanism comprises a multi-way valve, the multi-way valve is provided with a liquid inlet and a plurality of liquid outlets, and the liquid outlets of the multi-way valve are communicated with the analysis columns in a one-to-one correspondence manner; the liquid inlet of the multi-way valve is connected with a liquid inlet header pipe;
b. the liquid separating mechanism comprises a plurality of three-way valves, and each three-way valve comprises a liquid inlet and two liquid outlets; taking the liquid flowing direction as a downstream direction, connecting a liquid inlet of the three-way valve positioned at the most upstream with a liquid inlet header pipe, and correspondingly communicating two liquid outlets of one three-way valve at the relatively upstream with liquid inlets of two three-way valves at the relatively downstream in the three-way valves connected along the upstream and downstream directions; the total number of liquid outlets of all the three-way valves at the most downstream is the same as the number of the analytical columns and is communicated in a one-to-one correspondence manner.
In the embodiment, the liquid separating mechanism adopts a second structure and comprises a main three-way valve 17, wherein a liquid inlet of the main three-way valve 17 is connected with a liquid inlet main pipe 11, two liquid outlets of the main three-way valve 17 are respectively connected with a liquid inlet of a liquid distribution three-way valve 18, each liquid distribution three-way valve 18 is provided with two liquid outlets, and four liquid outlets of the two liquid distribution three-way valves 18 are correspondingly communicated with liquid inlets of four analysis columns 4 one by one through liquid inlet branch pipes 19;
the liquid separating mechanism has a simple structure, liquid distribution is uniform, and used components such as pipelines, three-way valves and the like are common parts in laboratories, so that maintenance and replacement are both convenient.
The process for preparing the liquid phase is: the sample uniformly enters each analytical column 4 along with the mobile phase through the liquid inlet header pipe 11 and the liquid separating mechanism, each separated component sequentially flows out of each analytical column 4 along with the mobile phase through the liquid outlet branch pipe 8, finally enters the collecting bottle 10 through the liquid outlet header pipe 9, and the separated components flowing out at different times are collected in different collecting bottles 10 by replacing the collecting bottles 10;
in the process of preparing the liquid phase, the temperature in the box body is controlled in a preset interval by controlling the opening and closing of the electric heating pipe, and the temperature at each position in the box body is more uniform by opening the electric fan 3.
To verify the effectiveness of the multi-channel integrated liquid chromatography column device, the inventors conducted experiments.
The experimental scheme is as follows:
(1) the configuration treats the trifluoro uracil nucleotide solution of separation, uses the utility model discloses a multichannel integrated liquid chromatography column device separates solution, then uses the analytical column right the utility model discloses every analytical column gained purification product separates the effect appraisal.
(2) The same amount of the triflurouracil nucleotide solution was separated using a preparative column, and the separation effect of the preparative solution was evaluated using an analytical column.
The separation effect of the triflurouracil nucleotide solution during the preparation is shown in FIG. 4.
Four analytical columns 4 of the multi-channel integrated liquid chromatographic column device are respectively numbered as No. 1-4 analytical columns. The analytical profiles of analytical columns Nos. 1 to 4 are shown in FIG. 5.
By analyzing the purified product obtained from the multi-channel integrated liquid chromatography column apparatus, we can find that the separation effect of each analytical column 4 is good and substantially uniform (as shown in fig. 5). Through comparing multichannel integrated liquid chromatography column device separation effect and preparation post separation effect, we can discover under the condition of less sample volume, the utility model discloses a method of multichannel integrated liquid chromatography column device constant temperature preparation liquid phase can reach and prepare the same preparation liquid phase effect of post, has explained the feasibility of device on the preparation liquid phase.
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: the present invention may be modified or substituted with equivalents without departing from the spirit and scope of the invention, which should be construed as being limited only by the claims.

Claims (3)

1. The multichannel integrated liquid chromatographic column device is characterized in that: comprises a box body with an opening at the front end, and an electric heating pipe is coiled on the rear wall of the box body;
an electric fan is arranged in the box body in front of the electric heating pipe, a plurality of analysis columns are arranged in the box body in front of the electric fan at intervals in parallel, a box door is hinged to the side wall of the box body at an opening, the box door comprises a door frame and double-layer transparent materials embedded in the door frame, and a cavity is formed between the double-layer transparent materials;
the top end of each analysis column is connected with a liquid outlet branch pipe, each liquid outlet branch pipe is collected into a liquid outlet pipe bundle, the liquid outlet pipe bundle is led out of the box body, one liquid outlet branch pipe in the liquid outlet pipe bundle is used for being connected with an external liquid chromatography detector, and other liquid outlet branch pipes in the liquid outlet pipe bundle are led into a collecting container outside the box body;
the bottom end of each analytical column is connected with a liquid inlet header pipe through a liquid separating mechanism, and the liquid inlet header pipe extends out of the side wall of the box body and is connected with a conveying pump for conveying the mobile phase;
electric heating pipe and electric fan all are connected with an electrically controlled device, and electrically controlled device is connected with display screen and temperature sensor, and electrically controlled device and display screen all are located the box outer wall, and temperature sensor is located inside the box.
2. The multi-channel integrated liquid chromatography column device of claim 1, wherein: a metal pore plate is arranged in the box body between the analysis column and the electric fan, a plurality of small holes are uniformly distributed in the metal pore plate, and two metal pore plates are symmetrically arranged up and down.
3. The multi-channel integrated liquid chromatography column device of claim 1, wherein: the analytical columns are arranged side by side at intervals, and the liquid separation mechanism adopts any one of the following two structures:
a. the liquid separating mechanism comprises a multi-way valve, the multi-way valve is provided with a liquid inlet and a plurality of liquid outlets, and the liquid outlets of the multi-way valve are communicated with the analysis columns in a one-to-one correspondence manner; the liquid inlet of the multi-way valve is connected with a liquid inlet header pipe;
b. the liquid separating mechanism comprises a plurality of three-way valves, and each three-way valve comprises a liquid inlet and two liquid outlets; taking the liquid flowing direction as a downstream direction, connecting a liquid inlet of the three-way valve positioned at the most upstream with a liquid inlet header pipe, and correspondingly communicating two liquid outlets of one three-way valve at the relatively upstream with liquid inlets of two three-way valves at the relatively downstream in the three-way valves connected along the upstream and downstream directions; the total number of liquid outlets of all the three-way valves at the most downstream is the same as the number of the analytical columns and is communicated in a one-to-one correspondence manner.
CN201920676237.XU 2019-05-13 2019-05-13 Multi-channel integrated liquid phase chromatographic column device Expired - Fee Related CN209927802U (en)

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Application Number Priority Date Filing Date Title
CN201920676237.XU CN209927802U (en) 2019-05-13 2019-05-13 Multi-channel integrated liquid phase chromatographic column device

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Application Number Priority Date Filing Date Title
CN201920676237.XU CN209927802U (en) 2019-05-13 2019-05-13 Multi-channel integrated liquid phase chromatographic column device

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CN209927802U true CN209927802U (en) 2020-01-10

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110018264A (en) * 2019-05-13 2019-07-16 河南工业大学 The method that multichannel integrates liquid chromatogram column device and carries out liquid phase preparation

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110018264A (en) * 2019-05-13 2019-07-16 河南工业大学 The method that multichannel integrates liquid chromatogram column device and carries out liquid phase preparation

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