CN110455970A - Sample introduction fraction collector and system - Google Patents

Sample introduction fraction collector and system Download PDF

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Publication number
CN110455970A
CN110455970A CN201910772089.6A CN201910772089A CN110455970A CN 110455970 A CN110455970 A CN 110455970A CN 201910772089 A CN201910772089 A CN 201910772089A CN 110455970 A CN110455970 A CN 110455970A
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China
Prior art keywords
sample
valve opening
sample introduction
needle
pipeline
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CN201910772089.6A
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CN110455970B (en
Inventor
李乃杰
韩雪
杨三东
王丰琳
于德秀
唐涛
李彤
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YILITE ANALYSIS INSTRUMENT CO Ltd DALIAN
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YILITE ANALYSIS INSTRUMENT CO Ltd DALIAN
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • G01N2030/201Injection using a sampling valve multiport valves, i.e. having more than two ports

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The present invention provides a kind of sample introduction fraction collector and systems, are related to chromatography column feed materials equipment technical field, which includes switching valve group and multiple sample introduction mechanisms;Each sample introduction mechanism respectively includes sample needle and sample introduction pipeline, sample needle and sample introduction pipeline are connect with switching valve group respectively, the sample needle of each sample introduction mechanism can be connected to or disconnect under the control of switching valve group with sample introduction pipeline, switching valve group is used to multiple sample introduction pipelines selecting one and be connected to the chromatographic column of chromatogram arrangement, to realize multiple sample introduction mechanisms in turn to the chromatographic column sample introduction of chromatogram arrangement;Wherein at least one sample needle, which can export with the detector of chromatogram arrangement and switch valve group, select one and changeable be connected to.The present invention has had both the function of the fast automatic sample introduction of spininess and sample introduction fraction, can meet diversified experiment demand by an equipment, reduces the cost investment of equipment, also, the form of relatively existing two equipment, also saves space occupied.

Description

Sample introduction fraction collector and system
Technical field
The present invention relates to chromatography column feed materials equipment technical fields, more particularly, to a kind of sample introduction fraction collector and system.
Background technique
Liquid chromatograph is current mankind's grasp to one of the important means of complex mixture separation.As a kind of precision High, fireballing analysis and separating tool, liquid chromatogram in terms of the production of medical industry, biochemical technology and fine chemicals As more and more important separation preparation means.The autosampler of traditional technology only has a sample needle, in order to guarantee to analyze Repeatability, cleaning of the sample needle before and after sample introduction is essential, and which has limited sample introduction speed to improve.What is developed later is double Needle sample injector can be very good to solve this problem, and two sample needles are worked alternatively, sample introduction speed can be doubled.But it passes The structure of the crosspointer autosampler of system is the two sets of independent sampling systems built using two high pressures, two six-way valves, and high Pressing two six-way valves, the price is very expensive, and two high pressures, two six-way valves can almost account for whole instrument manufacturing cost 40% or more, along with components such as two sets of independent motors, lead screw, guide rail, sample needle, Butterworth Hatch, low pressure valves, this is resulted in Crosspointer autosampler holds at high price, and the price of a set of complete crosspointer autosampler of configuration is almost on the market Two times of single needle autosampler.Rotor and stator in two six-way valves of high pressure belong to vulnerable part, need to regularly replace, and replace Price is also very high.The use cost that this has resulted in traditional crosspointer autosampler is also higher.
And traditional automatic sampling fraction collector has both the function of autosampler and fraction collector, inherently one Kind of multiple function apparatus, but presently, there are the problem of it is similar with crosspointer autosampler, be equally two independent high pressures of needs Two six-way valves are high to realize the function of automatic sampling and fraction collection, manufacturing cost.
Also, although existing crosspointer autosampler can be realized fast sample, but and do not have fraction collection work With;Although automatic sampling fraction collector can be carried out fraction collection but its sample introduction efficiency is low.And some realities in actual use It tests and needs quick crosspointer automatic sampling, and some needs carry out fraction collection while automatic sampling, so, it generally requires Crosspointer autosampler and automatic sampling fraction collector are bought respectively.But two equipment are bought, one side higher cost, On the other hand, the occupied space of equipment is also larger.
Summary of the invention
The purpose of the present invention is to provide a kind of sample introduction fraction collectors, and to solve, either crosspointer is automatic in the prior art Sample injector or automatic sampling fraction collector have a single function, and single equipment is difficult to meet different experiments demand, generally require Crosspointer autosampler and automatic sampling fraction collector are bought respectively, cause experimental facilities higher cost, the occupancy of equipment empty Between larger technical problem.
A kind of sample introduction fraction collector provided by the invention, for connect with chromatogram arrangement, including switching valve group with it is more A sample introduction mechanism;
Each sample introduction mechanism respectively includes sample needle and sample introduction pipeline, the sample needle and sample introduction pipeline difference It is connect with the switching valve group, the sample needle and the sample introduction pipeline of each sample introduction mechanism can be in the switching valves It is connected to or disconnects under the control of group, the switching valve group is one with chromatogram arrangement chromatography for selecting multiple sample introduction pipelines Column connection, to realize multiple sample introduction mechanisms in turn to the chromatographic column sample introduction of chromatogram arrangement;
Wherein at least one sample needle can be exported with the detector of chromatogram arrangement and the switching valve group selects one can be switched Connection, and when the sample needle and the detector outlet, which is used to recycle the detector outflow of chromatogram arrangement Fraction substance, other pass through the chromatographic column sample introduction of its sample feeding pipe road direction chromatogram arrangement with sample needles for connect of switching valve group.
Further, the quantity of the sample introduction mechanism is two, respectively the first sample introduction mechanism and the second sample introduction mechanism;
First sample introduction mechanism includes the first sample needle and the first sample introduction pipeline, and second sample introduction mechanism includes second Sample needle and the second sample introduction pipeline, the first sample needle, the first sample introduction pipeline and the second sample introduction pipeline respectively with The switching valve group connection, the second sample needle are used to select with the outlet of the detector of liquid-chromatography apparatus and the switching valve group One and changeable connection;The switching valve group is also used to be connected to the chromatographic column of liquid-chromatography apparatus;
When the second sample needle is connected to the switching valve group, the switching valve group can be acted, to realize described A sample needle is by the first sample introduction pipeline and the second sample needle by the second sample introduction pipeline in turn to the color of liquid-chromatography apparatus Compose column sample introduction;When the second sample needle and the detector outlet, the first sample needle passes through the first sample feeding pipe road direction liquid The chromatographic column sample introduction of phase chromatogram arrangement, the distillations that the second sample needle is flowed out for the detector of reclaim liquid phase chromatogram arrangement Matter.
Further, the sample introduction fraction collector further includes wiper mechanism and sample introduction driving mechanism;
The sample introduction driving mechanism includes sample introduction driving pipeline, and the sample introduction driving pipeline is connect with switching valve group;It is described Wiper mechanism includes detergent line, and the detergent line is connect with the switching valve group;
The switching valve group can act, in first state and the second state transformation, in the second sample needle and institute Switching valve group connection is stated, and when the switching valve group is in first state: the first sample needle and the first sample introduction pipeline Conducting, sample introduction driving pipeline and the first sample introduction pipeline connection, the sample introduction driving mechanism can drive the first sample needle to Sample introduction in first sample introduction pipeline;The second sample needle and the second sample introduction pipeline disconnect, and the second sample introduction pipeline can It is connected to chromatographic column, with to chromatography in-column injection;Second sample needle can be connected to detergent line, for cleaning second sample Needle;
It is connected in the second sample needle with the switching valve group, and when the switching valve group is in the second state: first Sample needle and the first sample introduction pipeline disconnect, and the first sample introduction pipeline can be connected to chromatographic column, with to chromatography in-column injection;Institute Stating detergent line can be connected to the first sample needle, to clean the first sample needle;The second sample needle and described second Sample introduction pipeline conducting, wherein when the second sample needle is connected with the second sample introduction pipeline, the sample introduction drives pipeline and the Two sample introduction pipeline connections, the sample introduction driving mechanism can drive the second sample needle sample introduction into the second sample introduction pipeline;
The second sample needle and detector outlet, and when the switching valve group is in first state, described the A sample needle is connected with the first sample introduction pipeline, and the sample introduction driving pipeline and the first sample introduction pipeline connection, the sample introduction drive Motivation structure can drive the first sample needle sample introduction into the first sample introduction pipeline;
The second sample needle and detector outlet, and when the switching valve group is in the second state: the first sample Needle and the first sample introduction pipeline disconnect, and the first sample introduction pipeline can be connected to chromatographic column, with to chromatography in-column injection;It is described clear Washing pipeline can be connected to the first sample needle, to clean the first sample needle.
Further, the switching valve group includes two ten-way valves, 10 valve openings of two ten-way valves be respectively according to The first valve opening, the second valve opening, third valve opening, the 4th valve opening, the 5th valve opening, the 6th valve opening, the 7th valve opening, the 8th valve of secondary setting Hole, the 9th valve opening and the tenth valve opening;
First valve opening with the infusion pump of chromatogram arrangement for connecting, and first valve opening is used for and the tenth valve Hole is selected one with second valve opening and is connected to, and the tenth valve opening is connected to by the second sample introduction pipeline with the 4th valve opening, Second valve opening is connected to by the first sample introduction pipeline with the 6th valve opening;5th valve opening is connected to chromatographic column, and institute The 5th valve opening is stated for selecting one with the 4th valve opening and the 6th valve opening and being connected to;The third valve opening and the sample introduction drive Pipeline connection, and the third valve opening with the 4th valve opening and second valve opening for selecting one and being connected to;7th valve opening Be connected to the first sample needle, the 9th valve opening can be connected to the second sample needle, the 8th valve opening with it is described Detergent line connection, and the 8th valve opening can select one and be connected to the 7th valve opening and the 9th valve opening;
Wherein, when two ten-way valves are in first state: first valve opening is connected to the tenth valve opening, described 4th valve opening is connected to the 5th valve opening, to realize the chromatographic column sample introduction of the second sample feeding pipe road direction chromatogram arrangement;Described second Valve opening is connected to the third valve opening, and the 6th valve opening is connected to the 7th valve opening, to realize the sample introduction driving mechanism The first sample needle sample introduction into the first sample introduction pipeline can be driven;8th valve opening and the 9th valve opening connect It is logical, when the second sample needle is connected to the 9th valve opening, to realize the cleaning of the second sample needle;
When two ten-way valves are in the second state, first valve opening is connected to second valve opening, and the described 5th Valve opening is connected to the 6th valve opening, to realize the chromatographic column sample introduction of the first sample feeding pipe road direction chromatogram arrangement;4th valve opening It is connected to the third valve opening, the tenth valve opening is connected to the 9th valve opening, the 9th valve opening and second sample Needle be connected to when, with realize the sample introduction driving mechanism can drive the second sample needle into the second sample introduction pipeline into Sample;8th valve opening is connected to the 7th valve opening, to realize the cleaning of the first sample needle.
Further, 10 valve openings of two ten-way valves are successively uniformly distributed along circularizing clockwise;
The switching valve group further includes switched conductive pipeline, and the quantity of the switched conductive pipeline is 5, described two ten Port valve in first state, 5 switched conductive pipelines be respectively used to the first valve opening be connected to the tenth valve opening, the 4th valve opening with The connection of 5th valve opening, the second valve opening is connected to third valve opening, the 6th valve opening is connected to the 7th valve opening and the 8th valve opening and the 9th Valve opening connection;
When two ten-way valves turn to the second state, 5 switched conductive pipelines be respectively used to the first valve opening with The connection of second valve opening, the 5th valve opening is connected to the 6th valve opening, the 4th valve opening is connected to third valve opening, the tenth valve opening and the 9th valve opening Connection and the 8th valve opening are connected to the 7th valve opening.
Further, the sample introduction fraction collector further includes the first two-position three-way valve, first two-position three-way valve It is mounted between detector outlet and the second sample needle between detergent line and the 8th valve opening for selecting one;
Wherein, when first two-position three-way valve is mounted between detector outlet and the second sample needle, second sample Product needle is used for fraction collection;
When first two-position three-way valve is mounted between the detergent line and the 8th valve opening, the second sample needle energy It is enough cleaned.
Further, the wiper mechanism further includes the first cleaning solution reservoir and the second cleaning solution reservoir, and described When between detergent line described in one two-position three-way valve and the 8th valve opening, three interfaces of first two-position three-way valve respectively with institute State the first cleaning solution reservoir, the second cleaning solution reservoir and the connection of the 8th valve opening.
Further, the sample introduction driving mechanism further includes the second two-position three-way valve and sampling injector;
Three interfaces of second two-position three-way valve respectively with the sampling injector, the third valve opening and waste liquid Storage container connection.
Further, the wiper mechanism further includes the first rinse bath and the second rinse bath, and first rinse bath is used for The the first sample needle that need to be cleaned is placed, second rinse bath is for placing the second sample needle that need to be cleaned;
First rinse bath and the second rinse bath are connect by the first three-way connection with waste liquid storage container.
Further, it is provided on the pipeline between second two-position three-way valve and the waste liquid storage container and is connected to two The second three-way connection of person, the remaining interface of second three-way connection are connected to first three-way connection.
Further, the cleaning pump to the 8th valve opening feed flow is provided in the detergent line.
Further, when first two-position three-way valve is mounted between detector outlet and the second sample needle, described the The remaining interface of one two-position three-way valve is connect with waste liquid storage container.
Further, the first sample feeding pipe road is provided with the first quantitative loop, and the second sample feeding pipe road is provided with Second quantitative loop.
A kind of sample introduction fraction collection system provided by the invention, including liquid-chromatography apparatus and sample introduction provided by the invention Fraction collector;
Wherein, the liquid-chromatography apparatus includes detector, infusion pump, chromatographic column and mobile phase bottle, the detector Import is connect with the chromatographic column, and a connection is selected in the outlet of the detector and waste liquid storage container and the second sample needle;
The infusion pump is for driving the solution of mobile phase bottle that the sample in corresponding sample introduction pipeline is pushed to enter the color Compose column.
Sample introduction fraction collector provided by the invention includes switching valve group and multiple sample introduction mechanisms, multiple sample introduction mechanisms Sample needle and sample introduction pipeline are connect with switching valve group respectively, and multiple sample introduction mechanisms may be implemented in turn to liquid-chromatography apparatus Chromatographic column sample introduction, namely have the function of spininess quickly sample introduction in turn;And wherein at least one sample needle can be with detector Outlet and switching valve group select one it is changeable be connected to, when the sample needle is with the detector outlet, which is used for back The fraction substance of the detector outflow of liquid-chromatography apparatus is received, other sample needles connecting with switching valve group pass through its sample introduction pipeline To the chromatographic column sample introduction of liquid-chromatography apparatus, namely have the function of sample introduction and fraction collection at this time.As it can be seen that sample introduction of the invention Fraction collector has had both the function of the fast automatic sample introduction of spininess and sample introduction fraction, in this way, can be met by an equipment Diversified experiment demand reduces the cost investment of equipment, also, the form of relatively existing two equipment, also saves and account for Ground space.
Sample introduction fraction collection system provided by the invention includes liquid-chromatography apparatus and sample introduction fraction provided by the invention Collection device has beneficial effect same as sample introduction fraction collector provided by the invention, and details are not described herein.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is that sample introduction fraction collector provided in an embodiment of the present invention cooperates liquid-chromatography apparatus in crosspointer automatic sampling The schematic diagram of the sampling of the first sample needle, the second quantitative loop sample introduction state under device mode;
Fig. 2 is that sample introduction fraction collector provided in an embodiment of the present invention cooperates liquid-chromatography apparatus in crosspointer automatic sampling The schematic diagram of the sampling of the second sample needle, the first quantitative loop sample introduction state under device mode;
Fig. 3 is that sample introduction fraction collector provided in an embodiment of the present invention cooperates liquid-chromatography apparatus in automatic sampling fraction Sampling state under collection mode;
Fig. 4 is that sample introduction fraction collector provided in an embodiment of the present invention cooperates liquid-chromatography apparatus in automatic sampling fraction Sample introduction and fraction collection state under collection mode.
Icon: 1- sample introduction fraction collector;2- liquid-chromatography apparatus;3- detector;4- infusion pump;5- chromatographic column;6- Mobile phase bottle;The first two-position three-way valve of 7-;Two ten-way valves of 8-;The second quantitative loop of 9-;The first quantitative loop of 10-;11- the second two Triple valve;12- cleaning pump;13- the second sample needle;The first rinse bath of 14-;15- sampling injector;16- the first sample needle;17- Second rinse bath;The first three-way connection of 18-;The second three-way connection of 19-;20- the first cleaning solution reservoir;The second cleaning solution of 21- Reservoir;22- sample tray;23- sample bottle;24- waste liquid storage container.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with embodiment, it is clear that described reality Applying example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
As shown in Figure 1 to 4, the present embodiment provides a kind of sample introduction fraction collectors 1, comprising: switching valve group and multiple Sample introduction mechanism.
Switching valve group with the chromatographic column 5 of liquid-chromatography apparatus 2 for being connected to;Each sample introduction mechanism respectively include sample needle and Sample introduction pipeline, sample needle and sample introduction pipeline are connect with switching valve group respectively, to realize multiple sample introduction mechanisms in turn to liquid chromatogram The chromatographic column sample introduction of device;Wherein at least one sample needle can export and switch with detector valve group select one it is changeable be connected to, And when the outlet of the sample needle and detector 3, detector 3 of the sample needle for reclaim liquid phase chromatogram arrangement 2 flows out Fraction substance, other pass through with sample needles for connect of switching valve group the chromatographic column 5 of its sample feeding pipe road direction liquid-chromatography apparatus 2 into Sample.
It is understood that wherein at least one sample needle, which can export with detector and switch valve group, selects a changeable company Logical, referring at least one sample needle set, there are two types of work or connection status, and one is the sample needles can be with switching valve group Connection, at this point, the corresponding sample introduction mechanism of sample needle can be by switching chromatographic column sample introduction of the valve group to liquid-chromatography apparatus;It is another Kind is the outlet of the detector of the sample needle and liquid-chromatography apparatus, at this point, the sample needle into sample bottle for conveying The substance that fraction obtains.It should be noted that when needing to carry out fraction, accordingly also should at least one sample for answering Sample introduction mechanism can be used for sample introduction.
Multiple sample introduction mechanisms are that is, at least two, and in two sample introduction mechanisms, one of sample needle can be with detection Device outlet and switching valve group are selected one and changeable are connected to;Naturally, can be 1 either 2 accordingly when sample introduction mechanism is 3 Sample needle can be selected with the outlet of detector 3 and switching valve group one it is changeable be connected to, when sample introduction mechanism is more, as needed Reasonable distribution.It should be noted that when the quantity of sample introduction mechanism is not less than 3, if still had under fraction state The sample introduction needle of multiple sample introduction mechanisms is connect with switching valve group, at this point, these multiple sample introduction mechanisms can be sample introduction in turn, can be Single one sample introduction, for example, the quantity of sample introduction mechanism is 3, one of sample introduction needle can be with the outlet and switching of detector 3 Valve group selects a changeable connection, in the outlet of the sample introduction needle and detector 3, correspondingly, remaining two sample introduction needles can To be sample introduction in turn, it can also be and select a sample introduction.
As shown in Figure 1 to 4, in the preferred one embodiment of the present embodiment, the sample introduction mechanism of sample introduction fraction collector 1 Quantity be two, respectively the first sample introduction mechanism and the second sample introduction mechanism.
Wherein, the first sample introduction mechanism includes the first sample needle 16 and the first sample introduction pipeline, and the second sample introduction mechanism includes second Sample needle 13 and the second sample introduction pipeline, the first sample needle 16, the first sample introduction pipeline and the second sample introduction pipeline respectively with switching valve group Connection, the outlet that the second sample needle is used for the detector 3 with switching valve group and liquid-chromatography apparatus 2 are selected one and are connected to;Switch valve group It is also used to connect with the chromatographic column 5 of liquid-chromatography apparatus 2;
When second sample needle 13 is connected to switching valve group, switching valve group can be acted, to realize that the first sample needle 16 passes through First sample introduction pipeline and the second sample needle 13 by the second sample introduction pipeline in turn to the chromatographic column 5 of liquid-chromatography apparatus 2 into Sample;When the outlet of the second sample needle 13 and detector 3, the first sample needle 16 is filled by the first sample feeding pipe road direction liquid chromatogram Set 25 sample introduction of chromatographic column, the fraction substance that the second sample needle 13 is flowed out for the detector 3 of reclaim liquid phase chromatogram arrangement 2.This The the second sample needle 13 for inventing the sample introduction fraction collector provided is selected one with the outlet of switching valve group and detector 3 and is connected to, the When two sample needles 13 are connected to switching valve group, switching valve group can be acted, to realize that the first sample needle 16 passes through the first sample feeding pipe Road and the second sample needle 13 pass through the second sample introduction pipeline in turn to the chromatographic column sample introduction of liquid-chromatography apparatus, namely have double The quick function of sample introduction in turn of needle;In the outlet of the second sample needle 13 and detector 3, the first sample needle 16 passes through first 5 sample introduction of chromatographic column of sample feeding pipe road direction liquid-chromatography apparatus 2, the second sample needle 13 are used for the detection of reclaim liquid phase chromatogram arrangement 2 The fraction substance that device 3 flows out, namely have the function of sample introduction and fraction collection at this time.As it can be seen that sample introduction fraction collection of the invention Device has had both the function of the fast automatic sample introduction of crosspointer and sample introduction fraction, in this way, can be met by an equipment diversified Experiment demand reduces the cost investment of equipment, also, the form of relatively existing two equipment, also saves space occupied.
With continued reference to shown in FIG. 1 to FIG. 4, specifically, the present embodiment sample introduction fraction collector, further includes wiper mechanism With sample introduction driving mechanism;First sample feeding pipe road is provided with the first quantitative loop 10, and it is quantitative that the second sample feeding pipe road is provided with second Ring 9.
Wherein, the first sample introduction mechanism is appreciated that as main sample introduction mechanism, and corresponding first sample needle 16 is main sample needle, first Quantitative loop 10 is main quantitative loop, and the second sample introduction mechanism can be regarded as secondary sample introduction mechanism, and corresponding second sample needle 13 is duplicate sample product Needle, the second quantitative loop 9 are secondary quantitative loop.
Sample introduction driving mechanism includes sample introduction driving pipeline, and sample introduction drives pipeline to connect with switching valve group;Wiper mechanism includes Detergent line, detergent line are connect with switching valve group.Switching valve group can act, in first state and the second state transformation, Be connected in the second sample needle 13 with switching valve group, and switch valve group when being in first state: the first sample needle 16 and first quantifies Ring 10 is connected, and sample introduction driving pipeline is connected to the first quantitative loop 10, and sample introduction driving mechanism can drive the first sample needle 16 to the Sample introduction in a certain amount of ring 10;Second sample needle 13 and the second sample introduction pipeline disconnect, and the second quantitative loop 9 can be connected to chromatographic column 5, With the sample introduction into chromatographic column 5;Second sample needle 13 can be connected to for cleaning the second sample needle 13 with detergent line.
Be connected in the second sample needle 13 with switching valve group, and switches valve group when being in the second state: the first sample needle 16 and First quantitative loop 10 disconnects, and the first quantitative loop 10 can be connected to chromatographic column 5, with the sample introduction into chromatographic column 5;Detergent line can It is connected to the first sample needle 16, to clean the first sample needle 16;Second sample needle 13 is connected with the second sample introduction pipeline, wherein the When two sample needles 13 and the second quantitative loop 9 are connected, sample introduction driving pipeline is connected to the second quantitative loop 9, and sample introduction driving mechanism can Drive the second sample needle 13 sample introduction into the second quantitative loop 9 of the second sample introduction pipeline.
When the outlet of the second sample needle 13 and detector 3, the first sample needle 16 is in first state in switching valve group When, the first sample needle 16 and the first quantitative loop 10 are connected, and sample introduction driving pipeline is connected to the first quantitative loop 10, sample introduction driving mechanism The first sample needle 16 sample introduction into the first quantitative loop 10 can be driven;Switching valve group is when be in the second state: the first sample needle and First quantitative loop 10 disconnects, and the first quantitative loop 10 can be connected to chromatographic column 5, with to chromatography in-column injection;Detergent line can It is connected to the first sample needle 16, to clean the first sample needle 16.
It is understood that when the second sample needle 13 is connect with switching valve group, it, can by switching the switching of valve group state When realizing the first quantitative loop 10 to 5 sample introduction of chromatographic column, the first sample needle 16 is in cleaning state, and sample introduction driving mechanism is simultaneously Drive the second sample needle 13 sample introduction into the second quantitative loop 9;Or second quantitative loop 9 to 5 sample introduction of chromatographic column when, the second sample needle 13 In cleaning state, and sample introduction driving mechanism drives the first sample needle 16 sample introduction into the first quantitative loop 10, due to the first sample Product needle 16 and the second sample needle 13 are in same time, one of cleaning, another sample introduction, and quantitative loop is synchronous to chromatographic column 5 sample introductions realize the purpose of crosspointer fast sample.In the outlet of the second sample needle 13 and detector 3, the second sample needle 13 can be used for recycling fraction substance, and at this point, the first sample needle 16 can still be met while the function of sample introduction fractionation with sample introduction It can demand.As shown in Figure 1 to 4, as a preferred embodiment of the present invention, switching valve group includes two ten-way valves 8, and two 10 valve openings of ten-way valve 8 are respectively the first valve opening (reference of serial number 1 in FIG. 1 to FIG. 4 on two ten-way valves 8 set gradually Hole), the second valve opening (hole that serial number 2 in FIG. 1 to FIG. 4 on two ten-way valves 8 refers to), third valve opening is (two in FIG. 1 to FIG. 4 The hole that serial number 3 on the ten-way valve 8 of position refers to), the 4th valve opening (hole that serial number 4 in FIG. 1 to FIG. 4 on two ten-way valves 8 refers to), 5th valve opening (hole that the serial number 5 in FIG. 1 to FIG. 4 on two ten-way valves 8 refers to), (two ten lead to the 6th valve opening in FIG. 1 to FIG. 4 The hole that serial number 6 on valve 8 refers to), the 7th valve opening (hole that the serial number 7 in FIG. 1 to FIG. 4 on two ten-way valves 8 refers to), the 8th valve Hole (hole that the serial number 8 in FIG. 1 to FIG. 4 on two ten-way valves 8 refers to), the 9th valve opening are (in FIG. 1 to FIG. 4 on two ten-way valves 8 The hole that serial number 9 refers to) and the tenth valve opening (hole that the serial number 10 in FIG. 1 to FIG. 4 on two ten-way valves 8 refers to).
First valve opening is used to export with the infusion pump 4 of liquid-chromatography apparatus 2 and connect, and, the first valve opening is used for and the tenth valve Hole is selected one with the second valve opening and is connected to, and the tenth valve opening is connected to by the second sample introduction pipeline with the 4th valve opening, and the second valve opening passes through first Sample introduction pipeline is connected to the 6th valve opening;5th valve opening is connected to chromatographic column 5, and the 5th valve opening is used for and the 4th valve opening and the 6th valve Kong Zeyi connection;Third valve opening and sample introduction drive pipeline connection, and third valve opening is used to select one with the 4th valve opening and the second valve opening Connection;7th valve opening is connected to the first sample needle, and the 9th valve opening can be connected to the second sample needle, the 8th valve opening and detergent line Connection, and the 8th valve opening can select one and be connected to the 7th valve opening and the 9th valve opening.
Wherein, when two ten-way valves 8 are in first state: the first valve opening is connected to the tenth valve opening, the 4th valve opening and the 5th Valve opening connection, to realize sample introduction in the second sample feeding pipe road direction chromatographic column 5;Second valve opening is connected to third valve opening, the 6th valve opening with 7th valve opening connection, to realize that sample introduction driving mechanism can drive the first sample needle 16 sample introduction into the first quantitative loop 10;8th Valve opening is connected to the 9th valve opening, when the second sample needle is connected to the 9th valve opening, to realize the cleaning of the second sample needle 13.
When two ten-way valves 8 are in the second state, the first valve opening is connected to the second valve opening, and the 5th valve opening and the 6th valve opening connect It is logical, to realize the first quantitative loop 10 sample introduction into chromatographic column 5;4th valve opening is connected to third valve opening, the tenth valve opening and the 9th valve Hole connection, when the 9th valve opening is connected to the second sample needle, to realize that sample introduction driving mechanism can drive the second sample needle 13 to the Sample introduction in two quantitative loops 9;8th valve opening is connected to the 7th valve opening, in the cleaning to realize the first sample needle 16.
As a concrete implementation form, 10 valve openings of two ten-way valves 8 are successively uniformly distributed along circularizing clockwise.It cuts Changing valve group further includes switched conductive pipeline, and the quantity of switched conductive pipeline is 5, and two-position three-way valve is in first state, such as Fig. 1 It is shown, 5 switched conductive pipelines be respectively used to the first valve opening is connected to the tenth valve opening, the 4th valve opening is connected to the 5th valve opening, Two valve openings are connected to third valve opening, the 6th valve opening is connected to the 7th valve opening and the 8th valve opening is connected to the 9th valve opening.Two ten When port valve turns to the second state by driving assembly, as shown in Fig. 2, 5 switched conductive pipelines be respectively used to the first valve opening with The connection of second valve opening, the 5th valve opening is connected to the 6th valve opening, the 4th valve opening is connected to third valve opening, the tenth valve opening and the 9th valve opening Connection and the 8th valve opening are connected to the 7th valve opening.
Wherein, driving assembly can be the form etc. of motor cooperation lead screw.
It should be noted that the switching valve group of the present embodiment is not limited to the form of two ten-way valves 8, it can be multiple multi-pass Combining form of valve, such as two six-way valves etc., but consider from cost, connection simplicity etc., generally using high pressure Two ten-way valves 8.
With continued reference to shown in FIG. 1 to FIG. 4, the concrete form of a connection, this reality are selected as the second sample needle 13 of the invention Applying a sample introduction fraction collector further includes the first two-position three-way valve 7, and the first two-position three-way valve 7 is mounted on detector for selecting one Between 3 outlet and the second sample needle between detergent line and the 8th valve opening.Wherein, the first two-position three-way valve 7 is mounted on inspection When surveying between device outlet and the second sample needle 13, the second sample needle 13 is for being fractionated;First two-position three-way valve 7 is mounted on cleaning pipe When between eight valve opening of Lu Yu, the second sample needle 13 can be cleaned.
Specifically, wiper mechanism further includes the first cleaning solution reservoir 20 and the second cleaning solution reservoir 21, first liang When position three-way valve 7 is connected between detergent line and the 8th valve opening, three interfaces of the first two-position three-way valve 7 are clear with first respectively Washing lotion reservoir 20, the second cleaning solution reservoir 21 are connected to the 8th valve opening.First two-position three-way valve 7 is mounted on detector 3 When between outlet and the second sample needle 13, the remaining interface of the first two-position three-way valve 7 is connect with waste liquid storage container 24.
Wherein, the first cleaning solution reservoir 20 can be strong reagent washer bottle, and the second cleaning solution reservoir 21 can be weak Reagent washer bottle.
The sample introduction driving mechanism of the sample introduction fraction collector of the present embodiment specifically further includes 11 He of the second two-position three-way valve Sampling injector 15;Three interfaces of the second two-position three-way valve 11 are stored up with sampling injector 15, third valve opening and waste liquid respectively Deposit the connection of container 24.
Wiper mechanism further includes the cleaning pump 12 to the 8th valve opening feed flow, the first rinse bath 14 and the second rinse bath 17, and One rinse bath 14 is for placing the first sample needle 16 that need to be cleaned, and the second rinse bath 17 is for placing the second sample needle that need to be cleaned 13;First rinse bath 14 and the second rinse bath 17 are connect by the first three-way connection 18 with waste liquid storage container 24.
It is also settable on pipeline between second two-position three-way valve 11 and waste liquid storage container 24 to be connected to the 2nd 3 of the two Pass joint 19, the remaining interface of the second three-way connection 19 are connected to the first three-way connection 18.
The present embodiment also provides a kind of sample introduction fraction collection system, including liquid-chromatography apparatus 2 and the present embodiment provides Sample introduction fraction collector 1.Specifically, liquid-chromatography apparatus 2 includes detector 3, infusion pump 4, chromatographic column 5 and mobile phase bottle 6, the import of detector 3 is connect with chromatographic column 5, and the outlet of detector 3 and waste liquid storage container 24 and the second sample needle 13 select one Connection;Infusion pump 4 is for driving the solution of mobile phase bottle 6 that the sample in corresponding quantitative loop is pushed to enter chromatographic column 5.
Wherein, when the outlet of detector 3 is connect with waste liquid storage container 24, it not will do it fraction collection at this time, but it is straight Connecing will test the liquid of device 3 and is transported to waste liquid storage container 24;When the outlet of detector 3 is connect with the second sample needle 13, this When, the second sample needle 13 can carry out the collection of fraction substance, and the substance being collected into is placed into corresponding sample bottle.
When two sample introduction mechanisms provided referring to the present embodiment, switch valve group, wiper mechanism, sample introduction driving mechanism accordingly With the arrangement form of sample introduction mechanism, correspondingly, the form of the sample introduction mechanism for 3 or more, can be closed as needed The setting of reason, details are not described herein.
Illustratively below with reference to FIG. 1 to FIG. 4, in a specific embodiment of the present embodiment, sample introduction fraction collection The course of work of device 1.
Firstly, sample introduction fraction collector 1 is illustrated in conjunction with liquid-chromatography apparatus 2 in the specific embodiment, Middle liquid-chromatography apparatus 2 is mainly used for illustrating the connection and use in liquid chromatographic system of sample introduction fraction collector 1 Method.Liquid-chromatography apparatus 2 includes detector 3, infusion pump 4, chromatographic column 5 and mobile phase bottle 6.Sample introduction fraction collector 1 exists When as under the mode of crosspointer autosampler: two ten-way valves 8 and the first quantitative loop 10, the second quantitative loop 9, the first sample needle 16, the second sample needle 13, cleaning pump 12, the second two-position three-way valve 11 be connected, and simultaneously with the infusion pump in liquid-chromatography apparatus 2 4 and chromatographic column 5 be connected;Second two-position three-way valve 11 is connected with sampling injector 15, and by the second three-way connection 19 and gives up Liquid storage container 24 is connected, while the first rinse bath 14 and the second rinse bath 17 cross the first three-way connection 18 and be connected to the two or three Pass joint 19;The entrance of cleaning pump 12 is connected to the first two-position three-way valve 7, while the first two-position three-way valve 7 and the first cleaning solution Reservoir 20 and the second cleaning solution reservoir 21 are connected;Sample bottle 23 is placed on sample tray 22;The outlet of detector 3 with Waste liquid storage container 24 is connected.Sample introduction fraction collector 1 can be configured to automatic sampling by simply modifying connecting line Fraction collector mode, on the basis of above-mentioned crosspointer autosampler mode, the whole for disconnecting the first two-position three-way valve 7 connects It connects, again connect the first two-position three-way valve 7 with the second sample needle 13, the outlet of detector 3 and waste liquid storage container 24; Two ten-way valves 8 of high pressure are connected with the second cleaning solution reservoir 21.
Above-mentioned two ten-way valves 8, the second two-position three-way valve 11, the first two-position three-way valve 7 can be by circuit control systems Control two kinds of positions of switching and corresponding different flow path, the second two-position three-way valve 11 and the first two-position three-way valve 7 can gate two-way In be connected all the way with primary path, two ten-way valves 8 have ten connecting holes, and flow path therein is drawn in the accompanying drawings.Cleaning pump 12 Start and stop can be controlled by circuit control system, and control revolution.First sample needle 16 can be only with the second sample needle 13 Vertical operation, and the spatial movement mode with the formation multiaxis of sample tray 22, penetrate the first sample needle with the second sample needle In Arbitrary Samples bottle 23 on to sample tray 22, and it can return to respectively in the first rinse bath 14 and the second rinse bath 17.Into Sample syringe 15 can be completed the movement of calibrated shot and imbibition by circuit control.
The course of work of the crosspointer automatic sampling fraction collector of the embodiment of the present invention is as follows:
The state of the first sample needle 16 sampling 9 sample introduction of the second quantitative loop under crosspointer autosampler mode, such as Fig. 1 institute Showing, the first sample needle 16 penetrates in sample bottle 23, while the first sample needle 16 is connected to the 7th valve opening of two ten-way valves 8, Second two-position three-way valve 11 connects the access of the third valve opening of sampling injector 15 and two ten-way valves 8, at this time sampling injector 15 imbibitions generate negative pressure at the first sample needle 16, and the sample in sample bottle 23 is inhaled into the first sample needle 16, and is successively flowed The 7th valve opening and the 6th valve opening, the first quantitative loop 10 through two ten-way valves 8, and rest in the first quantitative loop 10 and complete first The sampling of sample needle 16, waits 10 sample introduction of the first quantitative loop, and subsequent second two-position three-way valve 11 is switched to connection sampling injector 15 and second three-way connection 19 state, sampling injector 15 by its internal waste liquid release via the second two-position three-way valve 11 with Second three-way connection 19, finally flows into waste liquid storage container 24.Also the second sample needle 13 started simultaneously at the above process In the second rinse bath 17, cleaning solution or the second cleaning in the first cleaning solution reservoir 20 is may be selected in the first two-position three-way valve 7 Cleaning solution in liquid reservoir 21 is pumped into the 8th valve opening of two ten-way valves 8 by cleaning pump 12, by the 9th valve opening, from It is flowed out at the needle point of two sample needles 13, cleans the inside and outside wall of the second sample needle 13, and then from the outlet stream of the second rinse bath 17 Out, waste liquid storage container 24 is finally flowed by the first three-way connection 18 and the second three-way connection 19, completed to the second sample needle 13 cleaning.Mobile phase in mobile phase bottle 6 is pumped into two ten-way valves 8 by the infusion pump 4 in liquid-chromatography apparatus 2, warp Push the sample in the second quantitative loop 9 via the 4th valve opening, the 5th valve in two ten-way valves 8 by the first valve opening, the tenth valve opening Hole enters the sample introduction that chromatographic column 5 completes the second quantitative loop 9.The sampling and second of the first sample needle 16 is completed in the process The sample introduction of quantitative loop 9, and the second sample needle 13 is cleaned.
The second sample needle 13 under crosspointer autosampler mode samples 10 sample introduction state of the first quantitative loop, as shown in Fig. 2, Second sample needle 13 penetrates in sample bottle 23, while the second sample needle 13 is connected to the 9th valve opening of two ten-way valves 8, and second The access of two-position three-way valve 11 connection sampling injector 15 and two 8 third valve openings of ten-way valve, 15 imbibition of sampling injector at this time, Negative pressure is generated at the second sample needle 13, the sample in sample bottle 23 is inhaled into the second sample needle 13, and followed by two 9th valve opening of ten-way valve 8 and the tenth valve opening, the second quantitative loop 9, and rest in the second quantitative loop 9 and complete the second sample needle 13 Sampling, wait 9 sample introduction of the second quantitative loop, subsequent second two-position three-way valve 11 be switched to connection sampling injector 15 and the two or three Its internal waste liquid is released and is connected via the second two-position three-way valve 11 with the two or three by the state of pass joint 19, sampling injector 15 First 19, it finally flows into waste liquid storage container 24.Also the first sample needle 16 started simultaneously at the above process is in the first cleaning In slot 14, the cleaning solution or the second cleaning solution reservoir 21 in the first cleaning solution reservoir 20 is may be selected in the first two-position three-way valve 7 In cleaning solution, the 8th valve opening of two ten-way valves 8 is pumped to by cleaning pump 12, by the 7th valve opening from the first sample needle 16 It is flowed out at needle point, cleans the inside and outside wall of the first sample needle 16, then flowed out by the outlet of the first rinse bath 14, by the first threeway Connector 18 and the second three-way connection 19 finally flow into waste liquid storage container 24, complete the cleaning to the first sample needle 16.Liquid phase color Mobile phase in mobile phase bottle 6 is pumped into two ten-way valves 8 by the infusion pump 4 in spectral apparatus 2, via the first valve opening, second Valve opening push the sample in the first quantitative loop 10 via in two ten-way valves 8 the 6th valve opening, that the 5th valve opening enters chromatographic column 5 is complete At the sample introduction of the first quantitative loop 10.Complete in the process the second sample needle 13 sampling and the first quantitative loop 10 into Sample, and the first sample needle 16 is cleaned.
Sampling state under automatic sampling fraction collection mode, as shown in figure 3, under this state, the first sample needle 16 penetrates Into sample bottle 23, while the first sample needle 16 is connected to the 7th valve opening of two ten-way valves 8, the connection of the second two-position three-way valve 11 The access of sampling injector 15 and two 8 third valve openings of ten-way valve, 15 imbibition of sampling injector at this time, at the first sample needle 16 Negative pressure is generated, the sample in sample bottle 23 is inhaled into the first sample needle 16, and followed by the 7th valve opening of two ten-way valves 8 With the 6th valve opening, the first quantitative loop 10, and the sampling for completing the first sample needle 16 is rested in the first quantitative loop 10, waits first 10 sample introduction of quantitative loop, subsequent second two-position three-way valve 11 are switched to the shape of connection sampling injector 15 and the second three-way connection 19 State, sampling injector 15 releases its internal waste liquid via the second two-position three-way valve 11 and the second three-way connection 19, final to flow Enter in waste liquid storage container 24.It is switched to also the first two-position three-way valve 7 that this above process carries out simultaneously and connect the second sample The flow path state that product needle 13 and detector 3 export, cleans the second sample needle 13 using the clean mobile phase before sample introduction, clearly Waste liquid after washing is stored up via the outlet of the second rinse bath 17, the first three-way connection 18, the second three-way connection 19, the final waste liquid that flow to Deposit container 24.The first two-position three-way valve 7 can be switched to the flow path shape that connection waste liquid storage container 24 is exported with detector 3 at any time State terminates the cleaning to the second sample needle 13, will be drained into waste liquid storage container 24 from the mobile phase flowed out in detector 3. The sampling of the first sample needle 16 and the cleaning to the second sample needle 13 are completed in the process.
Sample introduction and fraction collection state under automatic sampling fraction collection mode, as shown in figure 4, infusion pump in this case 4 outlet is connected to the first valve opening of two ten-way valves 8, and mobile phase is pumped by infusion pump 4, via the of two ten-way valves of high pressure One valve opening, the second valve opening enter the first quantitative loop 10 and push the sample in the first quantitative loop 10 via two ten-way valves of high pressure The 6th valve opening, the 5th valve opening complete sample introduction into chromatographic column 5.After completing sample introduction, into fraction collection state, first liang The outlet and waste liquid storage container 24 of 7 communication with detection device 3 of position three-way valve, the second sample needle 13, which penetrates, to be prepared to collect fraction In sample bottle 23, sample introduction fraction collector 1 waits detector 3 to provide signal, passes through when detector 3 is detected to collection of material Commencing signal can be issued when detector 3, sample introduction fraction collector 1 is after receiving commencing signal, according to length of pipe and stream First two-position three-way valve 7 is switched to the second sample needle 13 of connection and detector after delay time by the fast computing relay time The flow path states of 3 outlets, at this time will be by the first two-position three-way valve 7 from the by the fraction to be collected of the outlet of detector 3 discharge The needle point of two sample needles 13 flows out, and enters in sample bottle 23, when detector 3 detects the whole devices after testing of fraction to be collected End signal can be issued when 3, after sample introduction fraction collector 1 receives end signal, switched the first two-position three-way valve 7, made The outlet of detector 3 is connected to waste liquid storage container 24, completes fraction collection.It needs to repeat if needing to collect there are many fraction The step of fraction collection state.
In conclusion sample introduction fraction collector of the embodiment of the present invention is ingenious in design, integrated level is high, high reliablity, configuration Fast and flexible, it not only uses an instrument, realizes the function of two kinds of high end instruments, reduces the wasting of resources;And its cost It will also be lower than a traditional crosspointer autosampler or a traditional automatic sampling fraction collector.Greatly reduce the purchase of user It buys and use cost;Simultaneously also therefore, user only needs the operation for learning this instrument that can cope with complicated experiment condition, simplifies Experimental implementation, reduces learning cost.Its maximum innovative point is to receive crosspointer autosampler and automatic sampling fraction Storage integrates, and can realize the switching of above two high-end instrumental function by simply changing piping connection, And that innovates has used two ten-way valves of a high pressure to replace above-mentioned two instruments in traditional technology to be both needed to use two height Two six-way valve this core components are pressed, instrument manufacturing cost and use cost are significantly reduced.It can be said that this crosspointer Automatic sampling fraction collector has whole function of crosspointer autosampler Yu two kinds of high end instruments of automatic sampling fraction collector Energy and advantage, and it is low in cost, it is particularly suitable for promoting and applying in the art, has a vast market foreground.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into Row equivalent replacement;And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution The range of scheme.

Claims (10)

1. a kind of sample introduction fraction collector, for being connect with chromatogram arrangement, which is characterized in that the sample introduction fraction collector Including switching valve group and multiple sample introduction mechanisms;
Each sample introduction mechanism respectively includes sample needle and sample introduction pipeline, the sample needle and the sample introduction pipeline respectively with institute Switching valve group connection is stated, the sample needle and the sample introduction pipeline of each sample introduction mechanism can be in the switching valve groups The lower connection of control disconnects, and the switching valve group is used to select multiple sample introduction pipelines one and connects with the chromatographic column of chromatogram arrangement It is logical, to realize multiple sample introduction mechanisms in turn to the chromatographic column sample introduction of chromatogram arrangement;
Wherein at least one sample needle can with the detector of chromatogram arrangement export and the switching valve group select one can be switched be connected to, And when the sample needle and the detector outlet, which is used to recycle the fraction of the detector outflow of chromatogram arrangement Substance, other sample needles connecting with switching valve group pass through the chromatographic column sample introduction of its sample feeding pipe road direction chromatogram arrangement.
2. sample introduction fraction collector according to claim 1, which is characterized in that the quantity of the sample introduction mechanism is two It is a, respectively the first sample introduction mechanism and the second sample introduction mechanism;
First sample introduction mechanism includes the first sample needle and the first sample introduction pipeline, and second sample introduction mechanism includes the second sample Needle and the second sample introduction pipeline, the first sample needle, the first sample introduction pipeline and the second sample introduction pipeline respectively with it is described Switch valve group connection, the second sample needle is used to select one with the outlet of the detector of chromatogram arrangement and the switching valve group and can cut Change connection;
When the second sample needle is connected to the switching valve group, the switching valve group can be acted, to realize first sample Product needle by the first sample introduction pipeline and the second sample needle by the second sample introduction pipeline in turn to the chromatographic column of chromatogram arrangement into Sample;When the second sample needle and the detector outlet, the first sample needle passes through the first sample feeding pipe road direction chromatogram arrangement Chromatographic column sample introduction, the second sample needle be used for recycle chromatogram arrangement detector outflow fraction substance.
3. sample introduction fraction collector according to claim 2, which is characterized in that the sample introduction fraction collector also wraps Include wiper mechanism and sample introduction driving mechanism;
The sample introduction driving mechanism includes sample introduction driving pipeline, and the sample introduction driving pipeline is connect with switching valve group;The cleaning Mechanism includes detergent line, and the detergent line is connect with the switching valve group;
The switching valve group can act, cut with described in the second sample needle in first state and the second state transformation Change valve group connection, and when the switching valve group is in first state: the first sample needle is connected with the first sample introduction pipeline, Sample introduction driving pipeline and the first sample introduction pipeline connection, the sample introduction driving mechanism can drive the first sample needle to first into Sample introduction in sample pipeline;The second sample needle and the second sample introduction pipeline disconnect, and the second sample introduction pipeline can be with chromatography Column connection, with to chromatography in-column injection;Second sample needle can be connected to detergent line, for cleaning the second sample needle;
It is connected in the second sample needle with the switching valve group, and when the switching valve group is in the second state: the first sample Needle and the first sample introduction pipeline disconnect, and the first sample introduction pipeline can be connected to chromatographic column, with to chromatography in-column injection;It is described clear Washing pipeline can be connected to the first sample needle, to clean the first sample needle;The second sample needle and second sample introduction Pipeline conducting, wherein when the second sample needle is connected with the second sample introduction pipeline, the sample introduction drive pipeline and second into Sample pipeline connection, the sample introduction driving mechanism can drive the second sample needle sample introduction into the second sample introduction pipeline;
The second sample needle and detector outlet, and when the switching valve group is in first state, first sample Needle is connected with the first sample introduction pipeline, the sample introduction driving pipeline and the first sample introduction pipeline connection, the sample introduction driving mechanism The first sample needle sample introduction into the first sample introduction pipeline can be driven;
The second sample needle and detector outlet, and when the switching valve group is in the second state: the first sample needle and First sample introduction pipeline disconnects, and the first sample introduction pipeline can be connected to chromatographic column, with to chromatography in-column injection;The cleaning pipe Road can be connected to the first sample needle, to clean the first sample needle.
4. sample introduction fraction collector according to claim 3, which is characterized in that the switching valve group includes two ten logical Valve, 10 valve openings of two ten-way valves are respectively the first valve opening, the second valve opening, third valve opening, the 4th valve set gradually Hole, the 5th valve opening, the 6th valve opening, the 7th valve opening, the 8th valve opening, the 9th valve opening and the tenth valve opening;
First valve opening for connect with the infusion pump of chromatogram arrangement, and first valve opening for the tenth valve opening and Second valve opening selects a connection, and the tenth valve opening is connected to by the second sample introduction pipeline with the 4th valve opening, described Second valve opening is connected to by the first sample introduction pipeline with the 6th valve opening;5th valve opening is connected to chromatographic column, and described Five valve openings with the 4th valve opening and the 6th valve opening for selecting one and being connected to;The third valve opening and the sample introduction drive pipeline Connection, and the third valve opening with the 4th valve opening and second valve opening for selecting one and being connected to;7th valve opening and institute The connection of the first sample needle is stated, the 9th valve opening can be connected to the second sample needle, the 8th valve opening and the cleaning Pipeline connection, and the 8th valve opening can select one and be connected to the 7th valve opening and the 9th valve opening;
Wherein, when two ten-way valves are in first state: first valve opening is connected to the tenth valve opening, and the described 4th Valve opening is connected to the 5th valve opening, to realize the chromatographic column sample introduction of the second sample feeding pipe road direction chromatogram arrangement;Second valve opening It is connected to the third valve opening, the 6th valve opening is connected to the 7th valve opening, to realize that the sample introduction driving mechanism can Drive the first sample needle sample introduction into the first sample introduction pipeline;8th valve opening is connected to the 9th valve opening, In When the second sample needle is connected to the 9th valve opening, to realize the cleaning of the second sample needle;
When two ten-way valves are in the second state, first valve opening is connected to second valve opening, the 5th valve opening It is connected to the 6th valve opening, to realize the chromatographic column sample introduction of the first sample feeding pipe road direction chromatogram arrangement;4th valve opening and institute The connection of third valve opening is stated, the tenth valve opening is connected to the 9th valve opening, and the 9th valve opening and the second sample needle connect When logical, to realize that the sample introduction driving mechanism can drive the second sample needle sample introduction into the second sample introduction pipeline;Institute It states the 8th valve opening to be connected to the 7th valve opening, to realize the cleaning of the first sample needle.
5. sample introduction fraction collector according to claim 4, which is characterized in that 10 valve openings of two ten-way valves It is successively uniformly distributed along circularizing clockwise;
The switching valve group further includes switched conductive pipeline, and the quantity of the switched conductive pipeline is 5, two ten-way valves In first state, 5 switched conductive pipelines be respectively used to the first valve opening be connected to the tenth valve opening, the 4th valve opening and the 5th Valve opening connection, the second valve opening is connected to third valve opening, the 6th valve opening is connected to the 7th valve opening and the 8th valve opening and the 9th valve opening Connection;
When two ten-way valves turn to the second state, 5 switched conductive pipelines are respectively used to the first valve opening and second Valve opening connection, the 5th valve opening is connected to the 6th valve opening, the 4th valve opening is connected to third valve opening, the tenth valve opening and the 9th valve opening connect Logical and the 8th valve opening is connected to the 7th valve opening.
6. sample introduction fraction collector according to claim 4 or 5, which is characterized in that the sample introduction fraction collector Further include the first two-position three-way valve, first two-position three-way valve for select one be mounted on detector outlet with the second sample needle it Between between detergent line and the 8th valve opening;
Wherein, when first two-position three-way valve is mounted between detector outlet and the second sample needle, the second sample needle For fraction collection;
When first two-position three-way valve is mounted between the detergent line and the 8th valve opening, the second sample needle can be by Cleaning;
When first two-position three-way valve is mounted between detector outlet and the second sample needle, first two-position three-way valve Remaining interface is connect with waste liquid storage container.
7. sample introduction fraction collector according to claim 6, which is characterized in that the wiper mechanism further includes first clear Washing lotion reservoir and the second cleaning solution reservoir, first two-position three-way valve be connected to the detergent line and the 8th valve opening it Between when, three interfaces of first two-position three-way valve respectively with the first cleaning solution reservoir, the second cleaning solution reservoir It is connected to the 8th valve opening;
The cleaning pump to the 8th valve opening feed flow is provided in the detergent line;
The wiper mechanism further includes the first rinse bath and the second rinse bath, and first rinse bath is used to place need to clean the A sample needle, second rinse bath is for placing the second sample needle that need to be cleaned;
First rinse bath and the second rinse bath are connect by the first three-way connection with waste liquid storage container.
8. sample introduction fraction collector according to claim 7, which is characterized in that the sample introduction driving mechanism further includes Two two-position three-way valves and sampling injector;
Three interfaces of second two-position three-way valve are stored with the sampling injector, the third valve opening and waste liquid respectively Container connection.
9. sample introduction fraction collector according to claim 2, which is characterized in that the first sample feeding pipe road is provided with First quantitative loop, the second sample feeding pipe road are provided with the second quantitative loop.
10. a kind of sample introduction fraction collection system, which is characterized in that including any one of liquid-chromatography apparatus and claim 1-9 The sample introduction fraction collector;
Wherein, the liquid-chromatography apparatus includes detector, infusion pump, chromatographic column and mobile phase bottle, the import of the detector It is connect with the chromatographic column, a connection is selected in the outlet of the detector and waste liquid storage container and the second sample needle;
The infusion pump is for driving the solution of mobile phase bottle that the sample in corresponding sample introduction pipeline is pushed to enter the chromatographic column.
CN201910772089.6A 2019-08-20 2019-08-20 Sampling fraction collecting device and system Active CN110455970B (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110658293A (en) * 2019-11-18 2020-01-07 大连依利特分析仪器有限公司 Sample introduction device and sample analysis system
CN110988228A (en) * 2019-11-25 2020-04-10 清华大学 Automatic sample introduction and analysis device for multiple samples
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CN110658293A (en) * 2019-11-18 2020-01-07 大连依利特分析仪器有限公司 Sample introduction device and sample analysis system
CN110988228A (en) * 2019-11-25 2020-04-10 清华大学 Automatic sample introduction and analysis device for multiple samples
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WO2021249347A1 (en) * 2020-06-10 2021-12-16 上海贝高医疗科技有限公司 Static sample injection and fraction collection apparatus for use with liquid chromatograph
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CN114994223A (en) * 2022-04-29 2022-09-02 天津博纳艾杰尔科技有限公司 Automatic sample injection liquid path system and automatic sample injection method
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