CN206270305U - For the miniaturization device of GPC cleanup system system - Google Patents

For the miniaturization device of GPC cleanup system system Download PDF

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Publication number
CN206270305U
CN206270305U CN201621347123.3U CN201621347123U CN206270305U CN 206270305 U CN206270305 U CN 206270305U CN 201621347123 U CN201621347123 U CN 201621347123U CN 206270305 U CN206270305 U CN 206270305U
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China
Prior art keywords
interface
selector valve
interfaces
path selector
connects
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Withdrawn - After Issue
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CN201621347123.3U
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Chinese (zh)
Inventor
刘永利
苏丽评
朱苗苗
芦明星
谢新刚
丁一
牛宗萌
张晓辉
胡克
邓宛梅
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BEIJING LABTECH INSTRUMENT Co Ltd
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BEIJING LABTECH INSTRUMENT Co Ltd
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Priority to CN201621347123.3U priority Critical patent/CN206270305U/en
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Abstract

The utility model provides a kind of miniaturization device for GPC cleanup system system, include the first path selector valve and alternate path selector valve, the first path selector valve is two six-way valves, one orifice injection port, its No. three interfaces are by its No. six interfaces of quantitative pipeline connection, its No. four orifices to gel chromatographic columnses arrival end, its No. five orifice infusion pumps;The alternate path selector valve is also two six-way valves, and its first interface connection caching pipeline connects sample introduction needle again, its second interface connection syringe pump, the port of export of its 6th orifice to gel chromatographic columnses;In the course of the work, by switching the working condition of the first path selector valve and alternate path selector valve, and make infusion pump and refraction pump alternate run, GPC cleanup system work can be smoothly completed.

Description

For the miniaturization device of GPC cleanup system system
Technical field
The utility model is related to a kind of miniaturization device for GPC cleanup system system, is exactly specifically for preceding The miniaturized system of the GPC cleanup system system for the treatment of and purification, by, setting receipts online with the direct carry of other processing platforms Collection time started and collection end time, certain section of chromatography column effluent of time is obtained, be directly connected to gas chromatograph sampling point Analysis is collected to ad-hoc location.
Background technology
Gel permeation chromatography (Gel Permeation Chromatography), also known as gel purification chromatogram, volume exclusion Chromatogram etc. (Size Exclusion Chromatography) SEC, abbreviation GPC, is a more traditional isolation technics, GPC Pillar be made up of chemically inert hollow bead, the principle of utilization space exclusion is separated to sample.
Gel permeation chromatography (GPC) is a kind of isolation technics for growing up in the sixties, and it is based on porous gel pair Different size of exclusion effect is separated.Be mainly used in agricultural product and Pesticide Residues, in field of Environment Protection to soil, The purified treatment of residual compounds in sewage.Separated according to solute molecule size in different sample solvents, gel chromatographic columnses The gel filled has various sizes of hole, and gel aperture is corresponding to separation component molecular size, when group of different sizes Fractionated molecule enters gel with mobile phase, and the reserving degree caned in hole is different, and macromolecular can not enter hole, and molecule is smaller It is deeper into hole, thus retention time is different, each component carries out wash-out when sample enters gel column by molecular size in sample When, macromolecular substances are such as:Protein, pigment, fat etc. are excluded outside the aperture of gel filler, directly flow out color with mobile phase Spectrum post.
In recent years, with the increase in demand in food and environmental analysis to GPC sample preparations, being purified using GPC can be from Macromolecular complex mass-energy is removed in soil, mud, the extractive with organic solvent of animal tissue and greatly improves operating efficiency, and can The not contaminated damage of analytical instrument is protected, extends the service life of analytical instrument.
With the popularization of the instruments such as GC, GC-MS, traditional GPC cleaning systems defect is increasingly highlighted.For example:The sides of EPA 3640 The post specification that law regulation is used is 25mm × 70cm, and standard flow rate is 5ml/min.Sampling volume is 2~10ml, is generally received The collection time is 12~30min, and according to this condition, the standard substance collection solvent mixed with mobile phase after purification is near 60~150ml is collected less, and the sample size of the instrument such as GC, GC-MS is μ L grades, collected solvent needs just enter after being concentrated The measure of row object, removes detection time time about at 1~2 hour or so, and centre has repeatedly transfer and locates The process of reason, easily causes object and has certain loss.Waste of solvent but also concentration process are not only caused more than collection solvent A large amount of solvents can be outwards discharged, it is very unfriendly to environment.
So the shortcoming of tradition GPC cleaning systems highlight for need the plenty of time, waste solvent, easily cause secondary pollution, The loss impact analysis that easily causes object is quantitative, qualitative results.
Utility model content
The purpose of this utility model is to provide a kind of miniaturization device for GPC cleanup system system, i.e., according to gel The principle of chromatogram, sample material can be according to the volume size order of molecule by gel chromatographic columnses, and macromolecular passes through gel first Chromatographic column, the small molecule target substance being retained afterwards then flows out gel chromatographic columnses.It is crucial so for GPC cleaning systems It is that can improve operating efficiency, reduces the use of solvent, adapts to analysis means and promotion environmental protection in Contemporary Environmental.For For GPC method, it is important to which system can provide the rate of recovery of stabilization, can be to the beginning acquisition time of test substance and end Acquisition time is controlled, and the interfering material that makes needed for so just meeting application is separated with test substance, is obtained stabilization and is purified Purpose.
To achieve the above object, the technical solution adopted in the utility model is:
A kind of miniaturization device for GPC cleanup system system, it is characterised in that:Include the first path selector valve With alternate path selector valve, wherein:
The first path selector valve is two six-way valves, and one orifice injection port, its No. three interfaces pass through fixed Amount pipeline connection its No. six interfaces, the arrival end of its No. four orifices to gel chromatographic columnses, its No. five orifice infusion pumps;
The alternate path selector valve is also two six-way valves, and its first interface connection caching pipeline connects sample introduction needle again, Its second interface connects syringe pump, the port of export of its 6th orifice to gel chromatographic columnses;
The first path selector valve is respectively provided with totally two work of first state and the second state with alternate path selector valve State, wherein:
In the first state, No. six interfaces of an orifice, No. three interfaces of No. two orifices, No. four orifices five Number interface;First interface connects the 6th interface, and second interface connects the 3rd interface, the interface of the 4th orifice the 5th;
In the second condition, No. two interfaces of an orifice, No. four interfaces of No. three orifices, No. five orifices No. six interfaces;First interface connects second interface, the interface of the 3rd orifice the 4th, the interface of the 5th orifice the 6th.
The described miniaturization device for GPC cleanup system system, wherein:No. two of the first path selector valve The waste-solution line of orifice first.
The described miniaturization device for GPC cleanup system system, wherein:The 3rd of the alternate path selector valve Interface and the 4th interface are spare interface.
The described miniaturization device for GPC cleanup system system, wherein:The 5th of the alternate path selector valve The waste-solution line of orifice second.
The described miniaturization device for GPC cleanup system system, wherein:The gel chromatographic columnses are provided with temperature control dress Put.
Compared to the sample injection method and purification process of traditional GPC cleanup system system, advantage of the present utility model is such as Under:
(1), the miniaturization of the utility model application GPC cleanup system system, the sample introduction for solving small samples is asked Topic, sample size only needs 10~20ul;
(2), the utility model uses micro-compliant mechanism, and column flow rate saves solvent load in 100ul/min, reduces experiment Cost;
(3), the sample direct injected that the utility model online with other injectors can be solved the problems, such as after sample preparation;
(4), the utility model object collected volume can be controlled within 200ul, coordinate GC large volume sample injections, completely Can direct injected after collection, and without further concentration, saved very big a period of time, improve the whole of gel purification Body efficiency;
(5), the utility model avoids the use of a large amount of solvents and to discharge in environment while reach saving solvent, reduction Experimental cost, the purpose of environmental protection;
(6), the utility model can be controlled to column temperature, reach the experimental situation of stabilization, solve experiment uniformity.
Brief description of the drawings
Fig. 1 is the utility model systematic schematic diagram;
Fig. 2 is the utility model device in preceding treatment sample introduction platform carry schematic diagram;
Fig. 3 is sample analysis result after the utility model device real work.
Description of reference numerals:1 infusion pump;2 first path selector valves;3 quantitative pipelines;4 gel chromatographic columnses;41 temperature controls are filled Put;5 alternate path selector valves;6 syringe pumps;7 caching pipelines;8 sample introduction needles;9 injection ports;10 liquid storage bottles;11 mounting brackets;12 Communication module;13 pre-treatment sample introduction platforms;14 first waste-solution lines;15 second waste-solution lines.
Specific embodiment
The invention of this reality is further described below in conjunction with brief description of the drawings.
It is the utility model systematic schematic diagram, as seen from the figure shown in Fig. 1:
A kind of miniaturization device for GPC cleanup system system, includes the first path selector valve 2 and alternate path Selector valve 5, wherein:
The first path selector valve 2 is two six-way valves, one interface A connection injection ports 9, secondly number interface B connects Logical first waste-solution line 14, its No. three interface C connect its No. six interface F by quantitative pipeline 3, and its No. four interface D are communicated to solidifying The arrival end of glue chromatographic column 4, its No. five interface E connection high pressure pumps 1;
The alternate path selector valve 5 is also two six-way valves, and its first interface a connection caching pipelines 7 connect sample introduction again Pin 8, its second interface b connection syringe pumps 6, its 3rd interface c and the 4th interface d is spare interface, and its 5th interface e connects the Two waste-solution lines 15, its 6th interface f is communicated to the port of export of gel chromatographic columnses 4, and the gel chromatographic columnses 4 are provided with attemperating unit 41;
The working method of the first path selector valve 2 and alternate path selector valve 5 is the same, with first state and Second state totally two working conditions, in the first state, an interface A connects No. six interfaces F, No. two interface B and connects No. three Interface C, No. four interface D connect No. five interface E, and in the second condition, an interface A connects No. two interface B, No. three interface C companies Logical No. four interfaces D, No. five interface E connect No. six interface F.
The utility model miniaturization can on-line unit, be provided with what is be connected with other analytical instrument or sample pre-treatments platform Mounting bracket, pipeline, connection or wireless communication module etc. (as shown in Figure 2), can work independently also on-line working, its work Process is as follows:
The first path selector valve 2 is in first state, and alternate path selector valve 5 is in the second state, sample introduction needle 8 The liquid storage bottle top for being loaded with sample to be clean is moved to, sample to be clean is sucked via sample introduction needle 8 by the reverse operation of syringe pump 6 In syringe pump 6, sample introduction needle 8 moves to the top of injection port 9, and sample to be clean pumps into alternate path selector valve 5 by the forward direction of syringe pump 6 Second interface b, flows through first interface a feeding sample introduction needles 8, and be then delivered to the first path selector valve 2 from injection port 9 first connects Mouth a, then enters in quantitative pipeline 3 through the 6th interface f of the first path selector valve 2;
Then adjust the first path selector valve 2 and enter the second state, infusion pump 1 is started working, flowing carrier fluid is delivered to 5th interface e of the first path selector valve 2, drives the sample to be clean in quantitative pipeline 3 logical through first after flowing through the 6th interface f 3rd interface c, the 4th interface d of road selector valve 2 flow into the arrival end of gel chromatographic columnses 4, carry out GPC purifications, so that treating net Interfering material in change sample is produced in gel chromatographic columnses 4 with target substance and separated, by the first big after small order of molecule certainly Flowed out in gel chromatographic columnses 4;
After the target substance is from the port of export outflow of gel chromatographic columnses 4, adjustment alternate path selector valve 5 enters first State, carry the target substance collection liquid flow through the 6th interface f, the first interface a of alternate path selector valve 5 after cache Into caching pipeline 7, until the target substance flows out from gel chromatographic columnses 4 completely;
Afterwards, the sample introduction needle 8 is moved to the top of gas chromatographic sample introduction mouthful 9, and syringe pump 6 works, by caching pipeline 7 The target substance is pumped into gas-chromatography detection system, so as to be analyzed to the target substance;
Finally, the first path selector valve 2 is reset to initial position with alternate path selector valve 5, stream is exported by infusion pump 1 Dynamic load liquid is cleaned to the fluid loop including gel chromatographic columnses 4;Cleaning solvent is drawn by syringe pump 6, to buffering pipeline and Injection port 9 is cleaned.
Below in conjunction with Fig. 2 to the utility model further instruction:As shown in Figure 2, the utility model passes through mounting bracket 11 can directly hang over pre-treatment sample introduction platform 13, and can carry out communication with pre-treatment sample introduction platform 11 by communication module 12 cooperates with Work, the caching pipeline 7 is connected with sample introduction needle 8, can carry out sampling and the collection work of sample.
To those skilled in the art, the utility model can make many equivalent on the basis of above-described embodiment Replace, for example:
The gel chromatographic columnses 4 are placed in the cavity of temperature controllable.
The injection port 9 is provided with the interface for being sealed with sample introduction needle 8.
The cleaning of the pumping into of testing sample, injection port 9 and quantitative pipeline 3 can be carried out using sample introduction needle 8, it is possible to use Other sample introduction instruments set by tripartite, such as syringe, sample introduction needle 8 are capable of achieving its sample introduction, cleaning function.
The feasibility of the utility model device is further detailed with reference to Fig. 3:17 kinds of organo-chlorine pesticides will be contained Sample to be clean purified by the utility model device, collected, collection liquid is finally directly entered gas chromatography-mass spectrum With the injection port 9 of instrument and it is analyzed, the analysis result obtained after real work is as shown in Fig. 3.Can be found out completely in Fig. 3 The chromatographic peak of corresponding 17 kinds of organo-chlorine pesticides, and peak type is good, signal base line is clean, illustrates by the utility model device Impurity is separated 17 kinds of organo-chlorine pesticides of purification well and in sample, and the loss without target peak.This practicality is new Type device can be very good to realize in-line purification, collect and the function online with GC, GC/MS.
Following table is invention device and tradition GPC devices otherness contrast table in use:
Project Traditional GPC Miniaturization GPC
Sampling volume 2~10mL 10~20 μ L
It is time-consuming 1~2 hour 15 minutes
Solvent load More than 150mL 1~2mL
It is combined with GC Can not Can be with
As shown above, traditional GPC devices are general makees a sample and needs 2~10mL sample sizes, 1~2 hour time-consuming, Solvent of the consumption more than 150mL, and can not realize online with the detecting instrument such as GC, GC/MS.And the utility model device does One sample only needs 10~20 μ L sample amounts, and 15 minutes or so, solvent consumption was filled in only 1~2mL, and the utility model Put can be carried out with the detecting instrument such as GC, GC/MS it is online.The utility model device relative to traditional GPC devices solvent and when Between be significantly improved on cost, and reduce manual operation, improve overall stability and reliability.
It is described above to be merely exemplary for the utility model, and nonrestrictive, those of ordinary skill in the art Understand, in the case where the spirit and scope that claim is limited are not departed from, can many modifications may be made, change or it is equivalent, but Fall within protection domain of the present utility model.

Claims (5)

1. a kind of miniaturization device for GPC cleanup system system, it is characterised in that:Include the first path selector valve (2) With alternate path selector valve (5), wherein:
The first path selector valve (2) is two six-way valves, and one interface (A) connects injection port (9), its No. three interfaces (C) its No. six interfaces (F) are connected by quantitative pipeline (3), its No. four interfaces (D) are communicated to the arrival end of gel chromatographic columnses (4), Its No. five interfaces (E) connect infusion pump (1);
The alternate path selector valve (5) is also two six-way valves, its first interface (a) connection caching pipeline (7) connect again into Sample pin (8), its second interface (b) connects syringe pump (6), and its 6th interface (f) is communicated to the port of export of gel chromatographic columnses (4);
The first path selector valve (2) is respectively provided with first state and the second state totally two works with alternate path selector valve (5) Make state, wherein:
In the first state, an interface (A) connects No. six interfaces (F), and No. two interfaces (B) connect No. three interfaces (C), and No. four connect Mouth (D) connects No. five interfaces (E);First interface (a) connects the 6th interface (f), and second interface (b) connects the 3rd interface (c), the Four interfaces (d) connect the 5th interface (e);
In the second condition, an interface (A) connects No. two interfaces (B), and No. three interfaces (C) connect No. four interfaces (D), and No. five connect Mouth (E) connects No. six interfaces (F);First interface (a) connects second interface (b), and the 3rd interface (c) connects the 4th interface (d), the Five interfaces (e) connect the 6th interface (f).
2. the miniaturization device for GPC cleanup system system according to claim 1, it is characterised in that:Described first No. two interfaces (B) of path selector valve (2) connect the first waste-solution line (14).
3. the miniaturization device for GPC cleanup system system according to claim 1, it is characterised in that:Described second 3rd interface (c) of path selector valve (5) is spare interface with the 4th interface (d).
4. the miniaturization device for GPC cleanup system system according to claim 1, it is characterised in that:Described second 5th interface (e) of path selector valve (5) connects the second waste-solution line (15).
5. the miniaturization device for GPC cleanup system system according to claim 1, it is characterised in that:The gel Chromatographic column (4) is provided with attemperating unit (41).
CN201621347123.3U 2016-12-08 2016-12-08 For the miniaturization device of GPC cleanup system system Withdrawn - After Issue CN206270305U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201621347123.3U CN206270305U (en) 2016-12-08 2016-12-08 For the miniaturization device of GPC cleanup system system

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Application Number Priority Date Filing Date Title
CN201621347123.3U CN206270305U (en) 2016-12-08 2016-12-08 For the miniaturization device of GPC cleanup system system

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106546687A (en) * 2016-12-08 2017-03-29 北京莱伯泰科仪器股份有限公司 For the miniaturization device and its using method of GPC cleanup system system

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106546687A (en) * 2016-12-08 2017-03-29 北京莱伯泰科仪器股份有限公司 For the miniaturization device and its using method of GPC cleanup system system
CN106546687B (en) * 2016-12-08 2023-04-07 北京莱伯泰科仪器股份有限公司 Miniaturized device for gel chromatography purification system and use method thereof

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