CN203772816U - Two-dimensional liquid chromatography-mass spectrometer for detecting strong polar compounds - Google Patents

Two-dimensional liquid chromatography-mass spectrometer for detecting strong polar compounds Download PDF

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Publication number
CN203772816U
CN203772816U CN201420103127.1U CN201420103127U CN203772816U CN 203772816 U CN203772816 U CN 203772816U CN 201420103127 U CN201420103127 U CN 201420103127U CN 203772816 U CN203772816 U CN 203772816U
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China
Prior art keywords
dimensional liquid
interface
chromatographic column
dimensional
way valve
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Expired - Fee Related
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CN201420103127.1U
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Chinese (zh)
Inventor
李淑静
宓捷波
陈其勇
王飞
许泓
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Tianjin Entry Exit Inspection and Quarantine Bureau of Animals Plants and Food Inspection Center
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Tianjin Entry Exit Inspection and Quarantine Bureau of Animals Plants and Food Inspection Center
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Abstract

The utility model discloses a two-dimensional liquid chromatography-mass spectrometer for detecting strong polar compounds. The two-dimensional liquid chromatography-mass spectrometer comprises a one-dimensional liquid chromatographic column, a two-dimensional liquid chromatographic column, a mass spectrum, a one-dimensional pump, a two-dimensional pump and a dilution pump, wherein a six-way valve is connected between the one-dimensional liquid chromatographic column and the two-dimensional liquid chromatographic column; the one-dimensional liquid chromatographic column is connected to the first interface of the six-way valve; the two-dimensional liquid chromatographic column is connected to the fourth interface of the six-way valve; the dilution pump is connected to the fifth interface of the six-way valve; a vacuum pump is connected to the second interface of the six-way valve; a pipeline is connected between the third interface and the sixth interface of the six-way valve; heating wires for heating the pipeline are arranged on the pipeline; the mass spectrum is connected to the two-dimensional liquid chromatographic column; the one-dimensional pump is connected to the one-dimensional liquid chromatographic column; and the two-dimensional pump is connected to the two-dimensional liquid chromatographic column. An organic phase flowing out of a one-dimensional liquid chromatogram can be evaporated through a vacuum solvent evaporation unit consisting of the six-way valve, the heating wires and the vacuum pump, so that the adjusting range of the ratio of a flowing phase entering the two-dimensional liquid chromatographic column is expanded, and the problem of diffusion of strong polar compounds in a two-dimensional chromatograph due to insufficient focusing is solved.

Description

A kind of two-dimensional liquid chromatography-mass spectrometer that detects strong polar compound
Technical field
The utility model relates to two-dimensional liquid chromatography-mass spectrum, specifically, is a kind of two-dimensional liquid chromatography-mass spectrometer of the strong polar compound of detection of mobile phase ratio range of adjustment expansion.
Background technology
In separating substances field, compartment analysis when cannot accomplishing multiclass component for not volatile sample, as: the detection of the multiclass Residual Veterinary Medicines in animal derived food etc.Application two-dimensional liquid chromatography (LC+LC) can improve separation efficiency greatly, can also be by analyte according to the chemical property compartment analysis that divides into groups.
Two-dimensional liquid chromatography adopts the pillar analytic sample of two kinds of different separating mechanisms conventionally, utilize the different qualities of compound that complex mixture is divided into one-component, these characteristics comprise acting force between molecular dimension, isoelectric point, water wettability, electric charge, particular molecule (affine) etc., the component that can not separate completely in one dimension piece-rate system, can in two-dimentional system, better be separated, therefore separating power, resolution are greatly improved.The first root chromatogram column of LC+LC is just equivalent to a pre-separation post, it can be analyzed the measured object second dimension LC post of sending into a group by a group, by setting clipping time, different component is sent in the second dimension chromatographic column and carried out compartment analysis, can obtain so the more detailed information of components of interest.
As shown in Figure 1, in the two-dimensional liquid chromatography of prior art, comprise one dimension liquid-phase chromatographic column 11, two-dimensional liquid chromatography post 12, mass spectrum 13, one dimension pump 14, dilution pumps 15, two-dimentional pump 16, dilution pumps 15 is connected between one dimension liquid-phase chromatographic column 11 and two-dimensional liquid chromatography post 12 by a three-way interface 17, by regulating the flow velocity of one dimension mobile phase and the flow velocity of the mobile phase that dilution pumps 15 promotes to regulate trapping process to enter the ratio of the organic phase of two-dimensional liquid chromatography post.
But the two-dimensional liquid chromatography of prior art, owing to being subject to the restriction of system pressure and flow velocity, two-dimensional liquid chromatography post trapping process enters two-dimensional liquid chromatography post organic phase and can not infinitely reduce, therefore can not well realize the trapping effect of two-dimensional liquid chromatography post for the stronger compound of polarity, thereby while causing two-dimension analysis, there will be the phenomenon of chromatographic peak diffusion.
Utility model content
Technical problem to be solved in the utility model is to provide a kind of two-dimensional liquid chromatography-mass spectrometer of the strong polar compound of detection of mobile phase ratio range of adjustment simple in structure, easy to use expansion.
In order to solve the problems of the technologies described above, the technical solution adopted in the utility model is: a kind of two-dimensional liquid chromatography-mass spectrometer that detects strong polar compound, comprise one dimension liquid-phase chromatographic column, two-dimensional liquid chromatography post, mass spectrum, one dimension pump, two dimension pump, dilution pumps, between one dimension liquid-phase chromatographic column and two-dimensional liquid chromatography post, be connected with six-way valve, one dimension liquid-phase chromatographic column is connected on the first interface of six-way valve, two-dimensional liquid chromatography post is connected on the 4th interface of six-way valve, dilution pumps is connected on the 5th interface of six-way valve, on the second interface of six-way valve, be connected with vacuum pump, between the 3rd interface of six-way valve and the 6th interface, be connected with pipeline, the heater strip of promising pipeline heating is set on pipeline, mass spectrum is connected on two-dimensional liquid chromatography post, on one dimension liquid-phase chromatographic column, be connected with one dimension pump, on two-dimensional liquid chromatography post, be connected with two-dimentional pump.
The heating-up temperature of described heater strip is 50-80 DEG C.
The beneficial effects of the utility model are: the vacuum solvent evaporation element being made up of six-way valve, heater strip and vacuum pump can regulate the mobile phase ratio from one dimension liquid-phase chromatographic column, realize and there is good two-dimension focusing for the stronger compound of polarity, solved the diffusion in two-dimentional chromatogram of the strong polar compound that brought by two-dimension focusing weak effect.
Brief description of the drawings
Fig. 1 is the two-dimensional liquid chromatography-mass spectrographic schematic diagram of prior art.
Fig. 2 is the two-dimensional liquid chromatography-mass spectrographic pre-separation schematic diagram of the strong polar compound of detection of the present utility model.
Fig. 3 is the two-dimensional liquid chromatography-mass spectrographic organic phase evaporation schematic diagram of the strong polar compound of detection of the present utility model.
Fig. 4 is the two-dimensional liquid chromatography-mass spectrographic trapping process schematic diagram of the strong polar compound of detection of the present utility model.
Fig. 5 is the two-dimensional liquid chromatography-mass spectrographic analytic process schematic diagram of the strong polar compound of detection of the present utility model.
Embodiment
Below in conjunction with the drawings and specific embodiments, the utility model is described in further detail:
The principle of work of two-dimensional liquid chromatography of the present utility model is identical with prior art, can be with reference to prior art, so no longer narration, the difference of the utility model and prior art is to be flowed out and flowed into organic phase ratio range of adjustment in the mobile phase of two-dimensional liquid chromatography post by one dimension liquid-phase chromatographic column to expand, and is described in detail below:
As shown in Figure 2, two-dimensional liquid chromatography-the mass spectrometer of the strong polar compound of detection of the present utility model, comprise one dimension liquid-phase chromatographic column 1, two-dimensional liquid chromatography post 2, mass spectrum 3, one dimension pump 4, two dimension pump 6, dilution pumps 5, between one dimension liquid-phase chromatographic column 1 and two-dimensional liquid chromatography post 2, be connected with six-way valve 7, one dimension liquid-phase chromatographic column 1 is connected on the first interface of six-way valve 7, two-dimensional liquid chromatography post 2 is connected on the 4th interface of six-way valve 7, dilution pumps 5 is connected on the 5th interface of six-way valve 7, on the second interface of six-way valve 7, be connected with vacuum pump 9, between the 3rd interface of six-way valve 7 and the 6th interface, be connected with pipeline, the heater strip 8 of promising pipeline heating is set on pipeline, mass spectrum 3 is connected on two-dimensional liquid chromatography post 2, on one dimension liquid-phase chromatographic column 1, be connected with one dimension pump 4, on two-dimensional liquid chromatography post 2, be connected with two-dimentional pump 6.
The heating-up temperature of described heater strip 8 is 50-80 DEG C.
6 interfaces of six-way valve 7 are followed successively by first interface, the second interface, the 3rd interface, the 4th interface, the 5th interface and the 6th interface, by two grades of conversions of valve, first interface and the 6th interface, the 4th interface and the 5th interface, the second interface and the 3rd interface are connected respectively, or first interface and the second interface, the 3rd interface and the 4th interface, the 5th interface and the 6th interface are connected respectively.
The utility model can evaporate organic phase in the mobile phase being flowed out by one dimension chromatographic column, flows out organic phase ratio in component thereby reduce one dimension.
Principle of the present utility model is as follows:
As shown in Figure 2, first step pre-separation: first object carries out pre-separation via one dimension liquid-phase chromatographic column, the mobile phase that now one dimension pump promotes to contain object carries out pre-separation by one dimension liquid-phase chromatographic column, and now in mobile phase, organic phase ratio is higher.
As shown in Figure 3, second step organic phase evaporation: heater strip will be arranged in the organic phase evaporation of pipeline by heating, and under the effect of vacuum pump, organic phase is pulled out to system, thereby reduces the ratio of organic phase.
As shown in Figure 4, the 3rd step object trapping: stream promotes to enter two-dimensional liquid chromatography post by dilution pumps and carries out the trapping of object, and dilution stream is mainly water.
As shown in Figure 5, the 4th step analytic process: stream promotes to carry out two-dimentional wash-out and analytic process by two-dimentional pump.
Above-described embodiment is only for illustrating technological thought of the present utility model and feature, its object is to make those skilled in the art can understand content of the present utility model and implement according to this, can not only limit the scope of the claims of the present utility model with the present embodiment, be equal variation or the modification that spirit that all the utility model disclose is done, still drop in the scope of the claims of the present utility model.

Claims (2)

1. one kind is detected the two-dimensional liquid chromatography-mass spectrometer of strong polar compound, comprise one dimension liquid-phase chromatographic column (1), two-dimensional liquid chromatography post (2), mass spectrum (3), one dimension pump (4), two dimension pump (6), dilution pumps (5), it is characterized in that, between one dimension liquid-phase chromatographic column (1) and two-dimensional liquid chromatography post (2), be connected with six-way valve (7), one dimension liquid-phase chromatographic column (1) is connected on the first interface of six-way valve (7), two-dimensional liquid chromatography post (2) is connected on the 4th interface of six-way valve (7), dilution pumps (5) is connected on the 5th interface of six-way valve (7), on the second interface of six-way valve (7), be connected with vacuum pump (9), between the 3rd interface of six-way valve (7) and the 6th interface, be connected with pipeline, the heater strip (8) of promising pipeline heating is set on pipeline, mass spectrum (3) is connected on two-dimensional liquid chromatography post (2), on one dimension liquid-phase chromatographic column (1), be connected with one dimension pump (4), on two-dimensional liquid chromatography post (2), be connected with two-dimentional pump (6).
2. two-dimensional liquid chromatography-the mass spectrometer of the strong polar compound of detection according to claim 1, is characterized in that, the heating-up temperature of described heater strip (8) is 50-80 DEG C.
CN201420103127.1U 2014-03-07 2014-03-07 Two-dimensional liquid chromatography-mass spectrometer for detecting strong polar compounds Expired - Fee Related CN203772816U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105403645A (en) * 2015-12-22 2016-03-16 云南中烟工业有限责任公司 On-line concentration device and application thereof to liquid phase-gas phase
CN105717243A (en) * 2014-12-03 2016-06-29 中国科学院大连化学物理研究所 Interface for two-dimensional liquid chromatography
CN107607661A (en) * 2017-09-05 2018-01-19 湖南师范大学 Multi-dimensional chromatograph system
CN109932464A (en) * 2019-04-10 2019-06-25 湖南师范大学 Multi-dimensional chromatograph system and multi-dimensional chromatograph separation method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105717243A (en) * 2014-12-03 2016-06-29 中国科学院大连化学物理研究所 Interface for two-dimensional liquid chromatography
CN105403645A (en) * 2015-12-22 2016-03-16 云南中烟工业有限责任公司 On-line concentration device and application thereof to liquid phase-gas phase
CN107607661A (en) * 2017-09-05 2018-01-19 湖南师范大学 Multi-dimensional chromatograph system
CN109932464A (en) * 2019-04-10 2019-06-25 湖南师范大学 Multi-dimensional chromatograph system and multi-dimensional chromatograph separation method
CN109932464B (en) * 2019-04-10 2020-05-19 湖南师范大学 Multidimensional chromatography system and multidimensional chromatography separation method

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