CN206146889U - Take full multidimensional high performance liquid chromatography appearance of multi -functional diverter valve - Google Patents
Take full multidimensional high performance liquid chromatography appearance of multi -functional diverter valve Download PDFInfo
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- CN206146889U CN206146889U CN201621160362.8U CN201621160362U CN206146889U CN 206146889 U CN206146889 U CN 206146889U CN 201621160362 U CN201621160362 U CN 201621160362U CN 206146889 U CN206146889 U CN 206146889U
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- switching valve
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/38—Flow patterns
- G01N30/46—Flow patterns using more than one column
- G01N30/461—Flow patterns using more than one column with serial coupling of separation columns
- G01N30/463—Flow patterns using more than one column with serial coupling of separation columns for multidimensional chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/38—Flow patterns
- G01N30/46—Flow patterns using more than one column
- G01N30/461—Flow patterns using more than one column with serial coupling of separation columns
- G01N30/465—Flow patterns using more than one column with serial coupling of separation columns with specially adapted interfaces between the columns
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Abstract
The utility model provides a take full multidimensional high performance liquid chromatography appearance of multi -functional diverter valve, take full multidimensional high performance liquid chromatography appearance of multi -functional diverter valve is by one -dimensional chromatogram flowing phase reservoir M1, one -dimensional chromatogram high -pressure pump P1, one -dimensional chromatogram admission valve V1, one -dimensional chromatogram chromatographic column C1, one -dimensional chromatographic detector D1, two -dimensional chromatographic flowing phase reservoir M2, two -dimensional chromatographic high -pressure pump P2, multi -functional diverter valve V, a plurality of two -dimensional separation post C2 1 to C2 8, two -dimensional chromatographic detector D, fraction collector F constitutes. The utility model discloses an outstanding effect is: 1. Adopt a plurality of two -dimensional chromatographic posts to carry out two -dimensional separation, stationary phase optional kind is many, and separation efficiency is high, separates effectually, can realize complicated sample's full composition separation and analysis. 2. The system is equipped with a plurality of detectors, can guarantee the disengaging process accurate control, improves the separation effect.
Description
Technical field
This utility model is related to a kind of full two-dimensional highly effective liquid phase chromatographic instrument and for the detached method of comprehensive two dimensional gas chromatography, belongs to
Instrument and equipment manufacturing technology field, is a kind of high performance liquid chromatography separation analytical equipment.
Background technology
High performance liquid chromatography is examined with high-pressure delivery mobile phase using high-effective fixed phase and higher sensitivity detector
Survey, with it is efficient, quick, be widely used the characteristics of, at present own Jing develop into various separation in solution organic substance research, point
The key technology of an analysis difficult problem, obtains extensively in fields such as pharmacy, life sciences, medical science, Food Science, petrochemical industry and environmental conservation
General application.
Common high performance liquid chromatograph is by groups such as reservoir, high-pressure pump, injector, chromatographic column, detector, monitors
Into, it is many in application process to be separated using a root chromatogram column, that is, one-dimensional chromatographic isolation.In one-dimensional chromatographic separation process
In, the eluent Jing high-pressure pumps in reservoir are conveyed through injector, and carry sample in injector is carried out point into chromatographic column
From exiting into detector from chromatographic column successively by separation component.For complex systems such as natural product, body fluid, usual one
Tens even hundreds of kind of components are contained in sample, and structure is similar between each component, the difference of amount is generally again very big, by one-dimensional
The restriction of Resolution of Liquid Chromatography and peak capacity etc., it is impossible to meet the needs of complex separations.
Two-dimensional liquid chromatography is the technology grown up on the basis of high performance liquid chromatography, it by technically and
Improvement on equipment, using an one-dimensional chromatographic column and a Two way chromatograms post, by one-dimensional chromatographic column separate fraction second is introduced
Chromatographic column carries out two dimensional separation.Compared with one-dimensional liquid chromatographic system, the advantage of Two way chromatograms there are provided bigger peak and hold
Amount such that it is able to more effectively solve the problem analysis of complex system sample.
Jorgenson et al. realized for the first time " complete early in 1990 on the basis of research " heartcut " technology
Two dimension cutting ", they are connected to two quantity tubes in one eight ways valve, and two quantity tube alternating samplings, sample introductions realize two
Dimension is separated.Chinese patent " a kind of preparative multidimensional chromatograph of liquid "(Application number 201110256302.1), it is one-dimensional using one
Detached dowel, a two dimensional separation post, two enriching columns and two ten-way valves, two dimensional separation post is connected to two enriching columns
On two ten-way valves, two quantity tubes replace enrichment, sample introduction, realize two dimensional separation.Chinese patent " a kind of natural product point
From method "(Application number 201210022094.3)Using an one-dimensional chromatographic column, a Two way chromatograms post, an enriching column and
One two six-way valve, closing down by high-pressure pump is replaced using enriching column enrichment, sample introduction, realizes two dimensional separation.It is Chinese special
Sharp " a kind of full bidimensional capillary liquid chromatography separation system "(Application number 200410098443.5), using an one-dimensional separation
Post, two two dimensional separation posts, enriching column, two six-way valves, two ten-way valves, realize two dimensional separation.It is Chinese special
Profit " full two dimension supertension high performance liquid chromatography separation system "(Application number 201010256470.6), using a conventional high-pressure
Liquid-phase chromatographic column, ultrahigh pressure liquid phase chromatographic column, two quantitative loops, two ten-way valves, conventional high-pressure liquid-phase chromatographic column
For one-dimensional detached dowel, ultrahigh pressure liquid phase chromatographic column is two dimensional separation post, and using the rotation of two ten-way valves two quantitative loops are handed over
For sampling, sample introduction, two dimensional separation is realized.
For now, full two dimension or multi-dimensional chromatograph pattern are by with the interface mould such as six-way valve, eight ways valve, ten-way valve
Formula, one-dimensional chromatographic column separate fraction is introduced into the second chromatographic column carries out two dimensional separation.Two dimensional separation post is required in separation process
Short, analyze speed is fast, and this causes whole separating effect to be restricted.For jumbo preparative separation, prior art can not
Enough meet demand, it is impossible to prepared by the separation for directly applying to composition.Prior art uses an one-dimensional chromatographic column, a two-dimentional color
Spectrum post is separated, and can only be separated using most two kinds of fixing phase chromatographic columns every time in separation process, it is difficult to meet complicated
The separation of sample needs.
Utility model content
To solve the defect existing for existing Two way chromatograms technology, this utility model provides a kind of band Multifunctional switching valve
Full two-dimensional highly effective liquid phase chromatographic instrument, switched by the conversion of valve so that one-dimensional separation effluent is sequentially switched to multiple two dimensions
Two dimensional separation is carried out in chromatographic column, the part that Two way chromatograms are separated is collected by fraction collector.
To achieve these goals, the technical solution adopted in the utility model is:
A kind of full two-dimensional highly effective liquid phase chromatographic instrument with Multifunctional switching valve, the full two-dimensional highly effective liquid with Multifunctional switching valve
Chromatography is by one-dimensional chromatogram flow phase reservoir M1, one-dimensional chromatograph high-pressure pump P1, one-dimensional chromatography column feed materials valve V1, one-dimensional chromatograph color
Spectrum post C1, one-dimensional chromatographic detector D1, Two way chromatograms mobile phase reservoir M2, Two way chromatograms high-pressure pump P2, Multifunctional switching valve
V, multiple two dimensional separation post C2-1 to C2-8, Two way chromatograms detector D, fraction collector F compositions.
Annexation between each part is:No. 0 passage of Multifunctional switching valve V connects with M1 → P1 → V1 → D1 pipelines
Connect, No. 1-No. 8 passages of Multifunctional switching valve V are connected respectively with the entrance point of Two way chromatograms post C2-1-C2-8, Two way chromatograms
The port of export of post C2-1 to C2-8 respectively connects a detector D, and the outlet of detector D is connected to fraction collector F.It is multi-functional
No. 9 of switching valve V to the outlet that No. 16 passages lead to more with is connected together, and more logical import is connected with M2 → P2 pipelines.
Stream during use is:M1 → P1 → V1 → D1 → Multifunctional switching valve V(No. 0 passage)→ Multifunctional switching valve V
(1-8 passages successively), M2 → P2 → Multifunctional switching valve V(9-16 passages)→ Two way chromatograms post(Difference C2-1- C2-
8)→ detector D(Respectively)→ fraction collector F.
Described Multifunctional switching valve V port numbers and channel number is not limited only to the passage count of above-mentioned fixation, also including profit
Realize that other of this utility model situation are connected situation with similar with Multifunctional switching valve V designs.
Described reservoir M1, M2 can be the corrosion resistant glass container of organic solvent-resistant or organic material container etc..
Described high-pressure pump P1, P2 can be the constant flow pumps or constant pressure pump etc. that can provide steady pressure and flow velocity.
The injection valve V1 can be injection valve or sampling pump of fixed volume etc..
Chromatographic column C1 and multiple two dimensional separation post C2-1, C2-2, C2-3, C2-4, C2-5, C2-6, C2-7, C2-8 can
Being glass, rustless steel, PEEK etc..The filler of filling can be filled out for ion exchange material, normal-phase chromatography filler, reversed phase chromatography
Material, gel filler etc., the amount of filler can be analytical type, semi-preparative, preparative etc..
The Multifunctional switching valve V is one one and enters logical selector valve more than the multidigit having more.
Described detector D1, D can be the detections of the flow types such as UV-detector, fluorescence detector, differential refraction detector
Device etc..The detection cell of detector D1 is high pressure resistant detection cell.
This utility model also proposed the chromatography separating method of the full two-dimensional highly effective liquid phase chromatographic instrument:In reservoir M1
Eluent Jing high-pressure pump P1 are conveyed through injection valve V1, and the sample carried in injection valve V1 carries out one-dimensional point into chromatographic column C1
From the effluent of chromatographic column C1 enters No. 0 through hole of Multifunctional switching valve V, is switched successively by multifunctional rotary switching valve V
Into chromatographic column C2-1, C2-2, C2-3, C2-4, C2-5, C2-6 being connected on the 1-8 through holes of Multifunctional switching valve V,
C2-7、C2-8.Eluent Jing high-pressure pump P2 in reservoir M2 are conveyed through 9-16 through holes, the 1-8 of Multifunctional switching valve V
Number through hole enters chromatographic column C2-1, C2-2, C2-3, C2-4, C2-5, C2-6, C2-7, C2-8, carries out two dimensional separation, two dimensional separation
Effluent detects that the effluent of detector D is collected into fraction collector F into detector D.The one-dimensional separation of separation process
Eluent glide path is:M1→P1→V1→D1→V(0)→V(1-8)→ C2-1 to C2-8(Successively), two dimensional separation eluting
Liquid glide path is:M2→P2→V(9-16)→V(1-8)→ C2-1 to C2-8(It is parallel)→D(It is parallel)→F(It is parallel).
A kind of full two-dimensional highly effective liquid phase chromatographic instrument with Multifunctional switching valve of this utility model and for comprehensive two dimensional gas chromatography point
From method, with superpower separating power.
In addition, prominent effect of the present utility model is:
1. two dimensional separation is carried out using multiple Two way chromatograms posts, the optional species of fixing phase is more, and separation efficiency is high, separates
Effect is good, and the whole part for being capable of achieving complex sample is separated and analysis.
2. system is provided with multiple detectors, it is ensured that separation process precise control, improves separating effect.
3. two dimensional separation is carried out using multiple Two way chromatograms posts, do not existed to one-dimensional column size and flow rate of mobile phase
Restriction, can be used for large sample amount preparative separate.
4. two dimensional separation is carried out using multiple Two way chromatograms posts, the time for having abundance carries out two dimensional separation, does not exist to two
Dimension chromatographic column must be the restriction of short column.
5. system design is simple, good separating effect, it is adaptable to which all kinds of complex mixtures are isolated and purified, and practicality is extremely strong.
Description of the drawings
Fig. 1 is the structural representation of the full two-dimensional highly effective liquid phase chromatographic instrument of this utility model embodiment.
Fig. 2 is embodiment one-dimensional detector output signal schematic diagram.
Fig. 3 is embodiment two-dimensional detector output signal schematic diagram.
Specific embodiment
This utility model is described in detail with reference to embodiment and accompanying drawing, but protection domain is not limited by this.
Embodiment 1 is as shown in figure 1, a kind of full two-dimensional highly effective liquid phase chromatographic instrument with Multifunctional switching valve and for complete two
The method of dimension chromatographic isolation, full two-dimensional highly effective liquid phase chromatographic instrument is by one-dimensional chromatogram flow phase reservoir M1, one-dimensional chromatograph high-pressure pump
P1, one-dimensional chromatography column feed materials valve V1, one-dimensional chromatograph chromatographic column C1, one-dimensional chromatographic detector D1, Two way chromatograms mobile phase reservoir M2,
Two way chromatograms high-pressure pump P2, Multifunctional switching valve V, Two way chromatograms chromatographic column C2-1 to C2-8, Two way chromatograms detector D, fraction
Catcher F is constituted.
Eluent Jing high-pressure pump P1 in reservoir M1 are conveyed through injection valve V1, and the sample carried in injection valve V1 is entered
Chromatographic column C1 carries out one-dimensional separation, and the effluent of chromatographic column C1 enters No. 0 through hole of Multifunctional switching valve V, by rotating many work(
Energy switching valve V switches into successively chromatographic column C2-1, C2-2, the C2- being connected on the 1-8 through holes of Multifunctional switching valve V
3、C2-4、C2-5、C2-6、C2-7、C2-8.Eluent Jing high-pressure pump P2 in reservoir M2 are conveyed through Multifunctional switching valve V
9-16 through holes, 1-8 through holes enter chromatographic column C2-1, C2-2, C2-3, C2-4, C2-5, C2-6, C2-7, C2-8, carry out
Two dimensional separation, two dimensional separation effluent detects that the effluent of detector D is received into fraction collector F into detector D
Collection.The one-dimensional separation eluent glide path of separation process is:M1→P1→V1→D1→V(0)→V(1-8)→ C2-1-8, two dimension
Separation eluent glide path is:M2→P2→V(9-16)→V(1-8)→ C2-1 to C2-8(It is parallel)→D(It is parallel)→F(It is flat
OK)..
By above-mentioned connection and mode of operation, the comprehensive two dimensional gas chromatography for carrying out Fructus Sophorae extract is separated:
First dimension chromatographic column is C18 posts, and length is 10cm.Second dimension chromatographic column C2-1, C2-2, C2-3, C2-4, C2-5,
C2-6, C2-7, C2-8 are followed successively by C4 posts, C4 posts, benzene post, benzene post, C8 posts, C8 posts, C18 posts, C18 posts, and length is 10cm.It is one-dimensional
Mobile phase is methanol-water(Volume ratio is 40/60), flow velocity is 1ml/min, and two-dimensional flow is mutually washed for the formic acid gradient of acetonitrile -0.1%
De-, 0-30min, acetonitrile is changed into 80% from 20%, and the flow velocity of two-dimensional flow phase is 1.0ml/min.
One-dimensional chromatogram and two-dimensional chromatogram when this utility model embodiment is separated is shown in accompanying drawing 2,3, illustrates this
Utility model separation efficiency is high, practical, and the whole part for being particularly suited for the complex systems such as Chinese medicine, body fluid is separated and chiralityization
The separation of the hardly possible separate substance such as compound, structure analogue compounds.
The above is only embodiment of the present utility model, it is noted that for the ordinary skill people of the art
Member, without departing from the concept of the premise utility, can also make some improvements and modifications, and these improvements and modifications also should
It is considered as in protection domain of the present utility model.
It is of the present utility model to complete to have benefited from grant of national natural science foundation(Project approval number:21675071).
Claims (5)
1. a kind of full two-dimensional highly effective liquid phase chromatographic instrument with Multifunctional switching valve, is characterized in that, by one-dimensional chromatogram flow phase liquid storage
Device M1, one-dimensional chromatograph high-pressure pump P1, one-dimensional chromatography column feed materials valve V1, one-dimensional chromatograph chromatographic column C1, one-dimensional chromatographic detector D1, two dimension
Chromatogram flow phase reservoir M2, Two way chromatograms high-pressure pump P2, Multifunctional switching valve V, multiple two dimensional separation post C2-1 to C2-8, two
Dimension chromatographic detector D, fraction collector F compositions;No. 0 passage of Multifunctional switching valve V connects with M1 → P1 → V1 → D1 pipelines
Connect, No. 1-No. 8 passages of Multifunctional switching valve V are connected respectively with the entrance point of Two way chromatograms post C2-1-C2-8, Two way chromatograms
The port of export of post C2-1 to C2-8 respectively connects a detector D, and the outlet of detector D is connected to fraction collector F;It is multi-functional
No. 9 of switching valve V to the outlet that No. 16 passages lead to more with is connected together, and more logical import is connected with M2 → P2 pipelines.
2. the full two-dimensional highly effective liquid phase chromatographic instrument with Multifunctional switching valve as claimed in claim 1, is characterized in that, described is more
Function switching valve V port number and channel number are not limited only to fixed passage count.
3. the full two-dimensional highly effective liquid phase chromatographic instrument with Multifunctional switching valve as claimed in claim 1, is characterized in that, the liquid storage
Device M1, M2 are corrosion resistant glass container or organic material container.
4. the full two-dimensional highly effective liquid phase chromatographic instrument with Multifunctional switching valve as claimed in claim 1, is characterized in that, the high pressure
Pump P1, P2 are the constant flow pumps or constant pressure pump that can provide steady pressure and flow velocity.
5. the full two-dimensional highly effective liquid phase chromatographic instrument with Multifunctional switching valve as claimed in claim 1, is characterized in that, the sample introduction
Valve V1 is the injection valve or sampling pump of fixed volume.
Priority Applications (1)
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CN201621160362.8U CN206146889U (en) | 2016-11-01 | 2016-11-01 | Take full multidimensional high performance liquid chromatography appearance of multi -functional diverter valve |
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CN201621160362.8U CN206146889U (en) | 2016-11-01 | 2016-11-01 | Take full multidimensional high performance liquid chromatography appearance of multi -functional diverter valve |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107037169A (en) * | 2016-11-01 | 2017-08-11 | 聊城大学 | A kind of full two-dimensional highly effective liquid phase chromatographic instrument and chromatography separating method with Multifunctional switching valve |
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2016
- 2016-11-01 CN CN201621160362.8U patent/CN206146889U/en not_active Expired - Fee Related
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107037169A (en) * | 2016-11-01 | 2017-08-11 | 聊城大学 | A kind of full two-dimensional highly effective liquid phase chromatographic instrument and chromatography separating method with Multifunctional switching valve |
CN107037169B (en) * | 2016-11-01 | 2018-12-04 | 聊城大学 | A kind of full two-dimensional highly effective liquid phase chromatographic instrument and chromatography separating method with Multifunctional switching valve |
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GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170503 Termination date: 20201101 |