CN207198107U - A kind of cascade Coupled columns mass spectrometer system based on valve - Google Patents

A kind of cascade Coupled columns mass spectrometer system based on valve Download PDF

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Publication number
CN207198107U
CN207198107U CN201721208326.9U CN201721208326U CN207198107U CN 207198107 U CN207198107 U CN 207198107U CN 201721208326 U CN201721208326 U CN 201721208326U CN 207198107 U CN207198107 U CN 207198107U
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way valves
positions
double
valve
output end
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韩彬
韦术敏
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Institute of Botany of CAS
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Institute of Botany of CAS
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Abstract

A kind of cascade Coupled columns mass spectrometer system based on valve is the utility model is related to, the tandem mass spectrum system includes double two-position four-way valves and two six-way valves;No. 1 position of double two-position four-way valves connects No. 8 positions, No. 2 positions of double two-position four-way valves connect 2 ' numbers positions of two six-way valves, the input of No. 3 positions connection binary pump of double two-position four-way valves, the output end of No. 4 positions connection reversed-phase column of double two-position four-way valves, No. 5 positions of the double two-position four-way valves of input connection of reversed-phase column, first import of No. 6 positions connection triple valve of double two-position four-way valves, second import of triple valve connects the output end of isocratic pump, the input of the hydrophilic post of outlet c connections of triple valve, the output end of hydrophilic post connects 6 ' numbers positions of two six-way valves, No. 7 positions connection injector output end of double two-position four-way valves, injector input connects quaternary pump output terminal, two six-way valves, 1 ' number position connection mass detector, two six-way valves, 3 ' numbers positions and 5 ' numbers positions connect waste liquid pool respectively.

Description

A kind of cascade Coupled columns mass spectrometer system based on valve
Technical field
The utility model is on a kind of cascade Coupled columns mass spectrometer system based on valve, is related to biochemical instrument technology neck Domain.
Background technology
The UPLC/6540 Q-TOF of Agilent 1290 are that Anjelen Sci. & Tech. Inc's development and application are led in separation detection The ultrahigh pressure liquid phase chromatographic tandem high resolution mass spectrum detector in domain, it uses packing material size as 1.8 μm of chromatographic column, Neng Gou The separation detection to complex sample is realized in 30min, more conventional liquid chromatograph analysis time shortens more than half, while can 1200bar pressure is resistant to, is imitated especially for the group that complexity is high, number is big with the obvious advantage for product.
At present, existing system single injected sampling can only use a root chromatogram column to carry out separation detection, by taking RPLC chromatographic columns as an example, It can realize that centering polarity, low pole compound efficiently separate, can not realize efficiently separating for highly polar compound, Zhi Nengshi Flowed out altogether within the system dead time.
Utility model content
In view of the above-mentioned problems, the purpose of this utility model is to provide a kind of component that can make opposed polarity in complex sample It is able to efficiently separate by different chromatographic columns respectively and the cascade chromatographic column string based on valve of tandem mass spectrum detection can be completed Join mass spectrometer system.
To achieve the above object, the utility model takes following technical scheme:A kind of cascade Coupled columns based on valve Mass spectrometer system, it is characterised in that the tandem mass spectrum system include double two-position four-way valves, two six-way valves, binary pump, reversed-phase column, Triple valve, isocratic pump, hydrophilic post, quaternary pump, mass detector and waste liquid pool;Double two-position four-way valves include No. 1 position~No. 8 Position, two six-way valves include 1 ' number position~6 ' number position;No. 1 position of double two-position four-way valves connects double two-position four-ways No. 8 double positions of valve, No. 2 positions of double two-position four-way valves connect 2 ' numbers positions of two six-way valves, double two-position four-ways No. 3 positions of valve connect the input of the binary pump, and No. 4 positions of double two-position four-way valves connect the output of the reversed-phase column End, the input of the reversed-phase column connect No. 5 positions of double two-position four-way valves, No. 6 positions connection of double two-position four-way valves First import of the triple valve, the second import of the triple valve connect the output end of the isocratic pump, the triple valve The input of the c connections hydrophilic post is exported, the output end of the hydrophilic post connects 6 ' numbers positions of two six-way valves, described No. 7 positions of double two-position four-way valves connect the output end of the quaternary pump, 1 ' number position of two six-way valves by an injector The mass detector is connected, 3 ' numbers positions and 5 ' numbers positions of two six-way valves connect the waste liquid pool respectively.
Further, by controlling double two-position four-way valves and two six-way valves, the tandem mass spectrum system is divided into loading Position, reversed phase chromatography separation position and hydrophilic chromatographic separation three kinds of position mode of operation.
Further, when the tandem mass spectrum system is loading position mode of operation:The quaternary pump is through the injector and institute No. 7 positions connection of double two-position four-way valves is stated, No. 5 positions of double two-position four-way valves are connected with the input of the reversed-phase column, institute No. 4 positions for stating double two-position four-way valves are connected with the output end of the reversed-phase column, No. 6 positions and described three of double two-position four-way valves The first import connection of port valve, the second import of the triple valve are connected with the isocratic pump, the outlet of the triple valve and institute The input connection of hydrophilic post is stated, 6 ' positions of two six-way valves are connected with the output end of the hydrophilic post, described two six 1 ' number position of port valve connects the mass detector, and each interface unit in above-mentioned link circuit is in running order, other devices Part is closed.
Further, when the tandem mass spectrum system is reversed phase chromatography separation position mode of operation:The output end of the binary pump It is connected with No. 3 positions of double two-position four-way valves, No. 5 positions of double two-position four-way valves connect the input of the reversed-phase column, No. 4 positions of double two-position four-way valves connect the output end of the reversed-phase column, No. 2 positions and described two of double two-position four-way valves 2 ' numbers positions of position six-way valve connect, 1 ' number position connection mass detector of two six-way valves, in above-mentioned link circuit Each interface unit it is in running order, other devices are closed.
Further, when the tandem mass spectrum system is that hydrophilic chromatographic separates position mode of operation:The output end of the quaternary pump It is connected through the injector with No. 7 positions of double two-position four-way valves, No. 1 position of double two-position four-way valves passes through exterior tubing It is connected with No. 8 positions of double two-position four-way valves, No. 6 positions of double two-position four-way valves connect with the first import of the triple valve Connect;Second import of the triple valve is connected with the isocratic pump, the outlet of the triple valve and the input of the hydrophilic post Connection;6 ' numbers positions of two six-way valves are connected with the output end of the hydrophilic post, and 1 ' number position of two six-way valves connects Connect the mass detector, each interface unit in above-mentioned link circuit is in running order, and other devices, which are in, closes shape State.
Further, the binary pump, quaternary pump and isocratic pump use liquid chromatography pump.
Further, 4 ' numbers positions of two six-way valves block, and are blocked using plug during use.
For the utility model due to taking above technical scheme, it has advantages below:1st, the utility model passes through to existing Ultrahigh-pressure liquid chromatograph tandem mass spectrum installs the structures such as double two-position four-way valve, two six-way valves, triple valve, quaternary pump, isocratic pumps additional The cascade Coupled columns mass spectrometer system based on valve is built up, realizes two root chromatogram columns to opposed polarity compound in same sample After ON-LINE SEPARATION, tested and analyzed respectively by tandem mass spectrum.2nd, the utility model introduces property not with the switching mode of valve Same chromatographic column combination (such as chromatographic column with hydrophilic function HILIC and reverse-phase chromatographic column RPLC, C18), it is simultaneously right so as to meet once Opposed polarity compound efficiently separates in sample.3rd, cascade Coupled columns mass spectrometer system of the present utility model is applied to not The separation of same polarity material so that two kinds of chromatographic columns of different nature cascade and can be directed to opposed polarity in a sample Compound separated respectively, pass sequentially through tandem mass spectrum detection, the component of opposed polarity can pass through respectively in complex sample Different chromatographic columns are efficiently separated, and tandem mass spectrum is detected, and are advantageous to find more potential metabolic marker things, from And more comprehensive and accurate result of study is obtained, the system has the characteristics of flux height and high automaticity, and need not appoint What extra Data Post means, can be greatly improved Efficiency.
Brief description of the drawings
Fig. 1 is cascade Coupled columns mass spectrometer system connection diagram of the utility model based on valve;
Fig. 2 is cascade Coupled columns mass spectrometer system connection diagram of the utility model based on valve;
Fig. 3 is separating spectrum of the utility model pseudo-ginseng leachate in single RPLC chromatographic columns;
Fig. 4 is separating spectrum of the utility model pseudo-ginseng leachate in the cascade Coupled columns mass spectrometer system based on valve.
Embodiment
Come to carry out the utility model detailed description below in conjunction with accompanying drawing.It should be appreciated, however, that accompanying drawing is provided only The utility model is more fully understood, they should not be understood paired limitation of the present utility model.
As shown in Fig. 1~2, the cascade Coupled columns mass spectrometer system provided by the utility model based on valve, including double two It is 11, two six-way valves 12 of position four-way valve, binary pump 13, reversed-phase column (RPLC chromatographic columns) 14, triple valve 15, isocratic pump 16, hydrophilic Post (HILIC chromatographic columns) 17, injector 18, quaternary pump 19, mass detector 20 and waste liquid pool 21.
Double two-position four-way valves 11 include No. 1 position, No. 2 positions, No. 3 positions, No. 4 positions, No. 5 positions, No. 6 positions, No. 7 positions and No. 8 positions.Two Position six-way valve 12 includes 1 ' number position, 2 ' numbers positions, 3 ' numbers positions, 4 ' numbers positions, 5 ' numbers positions and 6 ' numbers positions.
No. 1 position of double two-position four-way valves 11 is connected with No. 8 positions of double two-position four-way valves double 11 by exterior tubing, double two No. 2 positions of four-way valve 11 are connected with 2 ' numbers positions of two six-way valves 12, No. 3 positions connection binary pump 13 of double two-position four-way valves 11 Input, the output end of No. 4 positions connection reversed-phase column 14 of double two-position four-way valves 11, double two four of the input connection of reversed-phase column 14 No. 5 positions of port valve 11, the first import a of No. 6 positions connection triple valve 15 of double two-position four-way valves 11, the second import of triple valve 15 The output end of the isocratic pump 16 of b connections, the input of the hydrophilic post 17 of outlet c connections of triple valve 15, the output end of hydrophilic post 17 connect Connect 6 ' numbers positions of two six-way valves 12, the output end of No. 7 positions connection injector 18 of double two-position four-way valves 11, injector 18 it is defeated Enter the output end of end connection quaternary pump 19,1 ' number position connection mass detector 20 of two six-way valves 12, two six-way valves 12 3 ' numbers positions and 5 ' numbers positions connect waste liquid pool 21 respectively, 4 ' numbers positions closure of two six-way valves 12, can be entered using plug during use Row closure.Wherein, binary pump 13, isocratic pump 16 and quaternary pump 19 can use efficient liquid-phase chromatographic pump.
The utility model can by controlling the positions of double two-position four-way valves 11 and two six-way valves 12, realize loading position, Reversed phase chromatography separation position and hydrophilic chromatographic separation three kinds of position mode of operation, the following detailed description of the work of each mode of operation corresponding device Make state:
Loading position mode of operation:The output end of quaternary pump 19 flows through No. 7 positions with double two-position four-way valves 11 after injector 18 Connection, No. 5 positions of double two-position four-way valves 11 are connected with the input of reversed-phase column 14, No. 4 positions of double two-position four-way valves 11 with it is anti-phase The output end connection of post 14, No. 6 positions of double two-position four-way valves 11 are connected with the first import a of triple valve 15, and the of triple valve 15 Two import b are connected with isocratic pump 16, and the outlet c of triple valve 15 is connected with the input of hydrophilic post 17, and the 6 ' of two six-way valves 12 Position is connected with the output end of hydrophilic post 17,1 ' number position connection mass detector 20 of two six-way valves 12, in above-mentioned link circuit Each interface unit it is in running order, other devices are closed.
Reversed phase chromatography separation position mode of operation:The output end of binary pump 13 is connected with No. 3 positions of double two-position four-way valves 11, double The input of No. 5 positions connection reversed-phase column 14 of two-position four-way valve 11, No. 4 positions of double two-position four-way valves 11 connect the defeated of reversed-phase column 14 Go out end, No. 2 positions of double two-position four-way valves 11 are connected with 2 ' numbers positions of two six-way valves 12,1 ' number position connection of two six-way valves 12 Mass detector 20, each interface unit in above-mentioned link circuit is in running order, and other devices are closed.
Hydrophilic chromatographic separates position mode of operation:The output end of quaternary pump 19 through injector 18 with double two-position four-way valves 11 7 The connection of number position, No. 1 position of double two-position four-way valves 11 are connected by exterior tubing with No. 8 positions of pair two-position four-way valves 11, double two No. 6 positions of four-way valve 11 are connected with the first import a of triple valve 15;Second import b of triple valve 15 is connected with isocratic pump 16, and three The outlet c of port valve 15 is connected with the input of hydrophilic post 17;6 ' numbers positions of two six-way valves 12 and the output end of hydrophilic post 16 connect Connect, 1 ' number position connection mass detector 20 of two six-way valves 12, each interface unit in above-mentioned link circuit is in work shape State, other devices are closed.
The utility model makes reversed-phase column 14 be connected with hydrophilic post 17 by double two-position four-way valves 11, and Initial R PLC is low, and ratio has Machine mobile phase runs 4min, middle polarity and low pole compound is retained on reversed-phase column 14;Meanwhile it can not retain highly polar Compound enters triple valve 15, and low ratio organic phase flow is converted into initial organic at high proportion on hydrophilic post in triple valve 15 Mobile phase, highly polar compound is set to be retained on hydrophilic post;Switched by double two-position four-way valves 11 individually makes successively Reversed-phase column 14 and hydrophilic post 17 are connected with mass detector 20, and the component retained in each chromatographic column is effectively separated, detected. Mass Spectrometer Method and impurity when two six-way valves 12 are mainly used in originating 4min and post switching enter the conversion of waste liquid.Root in experiment The mobile phase ratio on reversed-phase column and hydrophilic post and flow velocity can suitably be adjusted according to the actual conditions of sample, to meet colors The needs of post separation are composed, table 1 show the time distribution of the separation mobile phase ratio and flow velocity of actual sample pseudo-ginseng leachate, no Fine setting is had with sample.
Table 1 cascades the time distribution of Coupled columns mass spectrometer system mobile phase ratio and flow velocity
Note:B is organic phase flow acetonitrile (containing 0.1% formic acid), and A is pure water (containing 0.1% formic acid), and B% is running The ratio of (A+B) volume summation shared by middle acetonitrile.
The utility model is using the separation detection of opposed polarity micromolecular compound in pseudo-ginseng methanol leachate as specific implementation Example example describes the workflow of the cascade Coupled columns mass spectrometer system of the present utility model based on valve in detail:
1st, reversed-phase column 14 is connected sample introduction with hydrophilic post 15 by double two-position four-way valves 11, flows RPLC by triple valve 15 Dynamic inversion of phases is HILC mobile phases, and the highly polar component for making not retaining on reversed-phase column 14 is retained on hydrophilic post 15;
2nd, reversed-phase column 14 is individually connected with mass detector 20, makes to be retained in middle polarity and low pole on reversed-phase column 14 Compound carries out separation detection;
3rd, hydrophilic post 15 is individually connected with mass detector 20, enables the highly polar compound retained on hydrophilic post 15 Separation detection.
The chromatogram that the utility model is only separated by reversed-phase column 14 using identical pseudo-ginseng methanol leachate is as a comparison. By test result indicates that, the collection of illustrative plates obtained using the cascade Coupled columns mass spectrometer system of the present utility model based on valve is (such as Shown in Fig. 4) compared with the existing single result (as shown in Figure 3) using anti-phase column system, its chromatogram peak capacity adds 88%, Generation molecular formula compound amounts improve 89%, and database matching compound numbers improve 67%.This cascade chromatographic column ON-LINE SEPARATION mode used in the time by original offline mode 3 hours shorten 1 hour.
The various embodiments described above are merely to illustrate the utility model, wherein the structure of each part, connected mode and manufacture craft Deng can all be varied from, every equivalents carried out on the basis of technical solutions of the utility model and improvement, It should not exclude outside the scope of protection of the utility model.

Claims (7)

1. a kind of cascade Coupled columns mass spectrometer system based on valve, it is characterised in that the tandem mass spectrum system includes double two Four-way valve, two six-way valves, binary pump, reversed-phase column, triple valve, isocratic pump, hydrophilic post, quaternary pump, mass detector and waste liquid Pond;Double two-position four-way valves include No. 1 position~No. 8 position, and two six-way valves include 1 ' number position~6 ' number position;
No. 8 positions of No. 1 position connection double two-position four-way valves pair of double two-position four-way valves, the 2 of double two-position four-way valves Number position connects 2 ' numbers positions of two six-way valves, and No. 3 positions of double two-position four-way valves connect the input of the binary pump, No. 4 positions of double two-position four-way valves connect the output end of the reversed-phase column, the input connection described double two of the reversed-phase column No. 5 positions of position four-way valve, No. 6 positions of double two-position four-way valves connect the first import of the triple valve, the triple valve Second import connects the output end of the isocratic pump, the input of the outlet c connections hydrophilic post of the triple valve, the parent The output end of water column connects 6 ' numbers positions of two six-way valves, and No. 7 positions of double two-position four-way valves are connected by an injector The output end of the quaternary pump is connect, 1 ' number position of two six-way valves connects the mass detector, two six-way valves 3 ' numbers positions and 5 ' numbers positions connect the waste liquid pool respectively.
2. a kind of cascade Coupled columns mass spectrometer system based on valve as claimed in claim 1, it is characterised in that pass through control Double two-position four-way valves and two six-way valves, the tandem mass spectrum system are divided into loading position, reversed phase chromatography separation position and hydrophilic color Spectrum separation three kinds of position mode of operation.
3. a kind of cascade Coupled columns mass spectrometer system based on valve as claimed in claim 2, it is characterised in that when the series connection Mass spectrometer system is loading position mode of operation:The quaternary pump is connected through the injector with No. 7 positions of double two-position four-way valves, No. 5 positions of double two-position four-way valves are connected with the input of the reversed-phase column, No. 4 positions of double two-position four-way valves with it is described The output end connection of reversed-phase column, No. 6 positions of double two-position four-way valves are connected with the first import of the triple valve, the threeway Second import of valve is connected with the isocratic pump, and the outlet of the triple valve is connected with the input of the hydrophilic post, and described two 6 ' positions of position six-way valve are connected with the output end of the hydrophilic post, and 1 ' number position of two six-way valves connects the Mass Spectrometer Method Device, each interface unit in above-mentioned link circuit is in running order, and other devices are closed.
4. a kind of cascade Coupled columns mass spectrometer system based on valve as claimed in claim 2, it is characterised in that when the series connection Mass spectrometer system is reversed phase chromatography separation position mode of operation:The output end of the binary pump and No. 3 positions of double two-position four-way valves Connection, No. 5 positions of double two-position four-way valves connect the input of the reversed-phase column, and No. 4 positions of double two-position four-way valves connect The output end of the reversed-phase column is connect, No. 2 positions of double two-position four-way valves are connected with 2 ' numbers positions of two six-way valves, described 1 ' number position of two six-way valves connects the mass detector, and each interface unit in above-mentioned link circuit is in running order, Other devices are closed.
5. a kind of cascade Coupled columns mass spectrometer system based on valve as claimed in claim 2, it is characterised in that when the series connection Mass spectrometer system is that hydrophilic chromatographic separates position mode of operation:The output end of the quaternary pump is through the injector and described double two four No. 7 positions connection of port valve, No. 1 position of double two-position four-way valves pass through No. 8 positions of exterior tubing and double two-position four-way valves Connection, No. 6 positions of double two-position four-way valves are connected with the first import of the triple valve;Second import of the triple valve with The isocratic pump connection, the outlet of the triple valve is connected with the input of the hydrophilic post;6 ' numbers of two six-way valves Position is connected with the output end of the hydrophilic post, and 1 ' number position of two six-way valves connects the mass detector, above-mentioned connection Each interface unit in loop is in running order, and other devices are closed.
6. a kind of cascade Coupled columns mass spectrometer system based on valve as claimed in claim 1 or 2, it is characterised in that described Binary pump, quaternary pump and isocratic pump use liquid chromatography pump.
7. a kind of cascade Coupled columns mass spectrometer system based on valve as claimed in claim 1 or 2, it is characterised in that described 4 ' numbers positions of two six-way valves block, and are blocked using plug during use.
CN201721208326.9U 2017-09-20 2017-09-20 A kind of cascade Coupled columns mass spectrometer system based on valve Expired - Fee Related CN207198107U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019228157A1 (en) * 2019-01-14 2019-12-05 中国科学院南海海洋研究所 Lc/ms and ms automatic switching high-throughput continuous sample feeding apparatus
CN111870998A (en) * 2020-07-23 2020-11-03 苏州大学 Device for purifying sea cucumber polysaccharide by virtue of tandem lectin affinity column and use method of device
CN114545014A (en) * 2022-04-22 2022-05-27 成都理工大学 Double-channel sample introduction system

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019228157A1 (en) * 2019-01-14 2019-12-05 中国科学院南海海洋研究所 Lc/ms and ms automatic switching high-throughput continuous sample feeding apparatus
CN111870998A (en) * 2020-07-23 2020-11-03 苏州大学 Device for purifying sea cucumber polysaccharide by virtue of tandem lectin affinity column and use method of device
CN114545014A (en) * 2022-04-22 2022-05-27 成都理工大学 Double-channel sample introduction system

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