CN207307262U - A kind of multi-path Two way chromatograms instrument - Google Patents
A kind of multi-path Two way chromatograms instrument Download PDFInfo
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- CN207307262U CN207307262U CN201720845007.2U CN201720845007U CN207307262U CN 207307262 U CN207307262 U CN 207307262U CN 201720845007 U CN201720845007 U CN 201720845007U CN 207307262 U CN207307262 U CN 207307262U
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Abstract
The utility model proposes a kind of multi-path Two way chromatograms instrument, including one-dimensional chromatographic fractionation system and multi-path Two way chromatograms piece-rate system, wherein one-dimensional chromatographic fractionation system is made of one-dimensional chromatogram flow phase reservoir M, one-dimensional chromatography high-pressure pump P, one-dimensional chromatography column feed materials valve V, one-dimensional chromatography chromatographic column C and one-dimensional chromatographic detector D；Multi-path Two way chromatograms piece-rate system is made of multiple Two way chromatograms mobile phase reservoir M1 to M8, multiple Two way chromatograms high-pressure pump P1 to P8, multiple Two way chromatograms chromatographic column C1 to C8, multiple Two way chromatograms detector D1 to D8 and fraction collector；The utility model separative efficiency is high, highly practical, is particularly suitable for the separation of the difficult separate substances such as the separation of full component and the structure analogue compounds of the complex systems such as Chinese medicine, body fluid.
Description
Technical field
This application involves a kind of multi-path Two way chromatograms instrument, belong to instrument and equipment manufacturing technology field, be a kind of efficient color
Spectrum separation analytical equipment.
Background technology
Chromatographic process have the characteristics that efficiently, it is quick, be widely used, oneself solves organic substance research through developing at present
In it is various separation, analysis problem key technologies, pharmacy, life science, medicine, Food Science, petrochemical industry and environment protect
The fields such as shield are widely used.Common chromatograph is by mobile phase holder, mobile phase pump, injector, chromatographic column, detection
Device, recorder etc. form, more in application process to be separated using a root chromatogram column, that is, one-dimensional chromatographic isolation.For multiple
Miscellaneous system, such as natural products, body fluid etc., contain tens or even hundreds of kind of component in a usual sample, and each group point it
Between structure it is similar, limited by one-dimensional chromatographic resolution rate and peak capacity etc., can not meet the needs of complex separations.
Two-dimensional liquid chromatography is the technology to grow up on the basis of one-dimensional chromatography, it uses an one-dimensional chromatographic column
With a Two way chromatograms column, one-dimensional chromatographic column separate fraction is introduced into the second chromatographic column and carries out two dimensional separation.With one-dimensional liquid phase color
Spectra system is compared, and the advantage of Two way chromatograms is the provision of the peak capacity of bigger, so as to more effectively solve complicated body
It is the problem analysis of sample.
Chinese patent " a kind of separation method of natural products "（Application number 201210022094.3）It is one-dimensional using one
Chromatographic column, a Two way chromatograms column, an enriching column and two six-way valves, by closing down for high-pressure pump, utilize enriching column
Enrichment, sample introduction alternating, realize two dimensional separation.Chinese patent " a kind of preparative multidimensional liquid chromatograph "（Application number
201110256302.1）, using an one-dimensional splitter, a two dimensional separation column, two enriching columns and two ten-way valves,
Two enriching columns are connected on two ten-way valves by two dimensional separation column, and two quantity tubes are alternately enriched with, sample introduction, realize two dimension point
From.Chinese patent " a kind of full bidimensional capillary liquid chromatography separation system "（Application number 200410098443.5）, using one
One-dimensional splitter, two two dimensional separation columns, an enriching column, two six-way valves, two ten-way valves, realize two dimension point
From.Chinese patent " full two dimension super-pressure high performance liquid chromatography separation system "（Application number 201010256470.6）, using one
Conventional high-pressure liquid-phase chromatographic column, a ultrahigh pressure liquid phase chromatographic column, two quantitative loops, two ten-way valves, conventional high-pressure liquid
Phase chromatographic column is one-dimensional splitter, and ultrahigh pressure liquid phase chromatographic column is two dimensional separation column, makes two using the rotation of two ten-way valves
Quantitative loop alternating sampling, sample introduction, realize two dimensional separation.
Current Two way chromatograms pattern be mostly by with interface modes such as 1-2 two six-way valve, eight ways valve, ten-way valves,
Using 1 one-dimensional splitter and 1 two dimensional separation column, one-dimensional chromatographic column separate fraction is introduced into the second chromatographic column and carries out two dimension point
From.In existing instrument, limited by interface modes, it is desirable to which one-dimensional flow velocity is very small, and the length of two dimensional separation column will be very
It is short, it is difficult to which that the conventional chromatographic column of application is separated as Two way chromatograms column, this causes whole separating effect to be restricted.For
Large capacity preparative separation, the prior art can not meet demand, can not directly apply to component separation prepare.This
Outside, existing two dimensional technique is separated using an one-dimensional chromatographic column, a Two way chromatograms column, can only at most use two kinds every time
Stationary phase chromatographic column carries out cooperation separation, it is difficult to meets the separation needs of complex sample.
Utility model content
The defects of to solve present in the prior art, the present invention provides a kind of multi-path two-dimensional highly effective liquid phase chromatographic instrument,
Connected by multiple two six-way valves and switched with changing so that one-dimensional separation efflux is sequentially switched in multiple Two way chromatograms columns
Two dimensional separation is carried out, Two way chromatograms separation component is collected by fraction collector.
To achieve these goals, the technical solution specifically used of the utility model is as follows：
A kind of multi-path Two way chromatograms instrument, including one-dimensional chromatographic fractionation system and multi-path Two way chromatograms piece-rate system, its
In one-dimensional chromatographic fractionation system by one-dimensional chromatogram flow phase reservoir M, one-dimensional chromatography high-pressure pump P, one-dimensional chromatography column feed materials valve V, one
Tie up chromatography chromatographic column C and one-dimensional chromatographic detector D compositions；Multi-path Two way chromatograms piece-rate system is by multiple Two way chromatograms mobile phases
Reservoir M1 to M8, multiple Two way chromatograms high-pressure pump P1 to P8, multiple Two way chromatograms chromatographic column C1 to C8, the inspection of multiple Two way chromatograms
Survey device D1 to D8 and fraction collector composition；One-dimensional chromatographic fractionation system and multi-path Two way chromatograms piece-rate system passes through multiple two
Position six-way valve V1 to V8 connections, are mounted on a trapping column on each two six-way valves, are represented respectively with F1 to F8；
Connection relation between each component is：The 1. number mouth of each two six-way valves is connected with the outlet that Two way chromatograms pump, 2.
Number mouth is connected with the import of Two way chromatograms column, and the outlet of Two way chromatograms column is connected with the import of two-dimensional detector, two-dimensional detector
Outlet be connected with Fraction collection device, for the two dimensional separation system of 8 paths, formed M1 → P1 → V1 1. V1 2. → C1
→ D1 → collector 1, M2 → P2 → V2 1. V2 2. → C2 → D2 → collector 2, M3 → P3 → V3 1. V3 2. → C3 → D3 →
Collector 3, M4 → P4 → V4 1. V4 2. → C4 → D4 → collector 4, M5 → P5 → V5 1. V5 2. → C5 → D5 → collector
5, M6 → P6 → V6 1. V6 2. → C6 → D6 → collector 6, M7 → P7 → V7 1. V7 2. → C7 → D7 → collector 7, M8 →
P8 → V8 1. V8 2. → the two dimensional separation connection mode of C8 → D8 → collector 8；Each two six-way valves（V1-V8）3. mouth
6. be connected 1 trapping column between number mouth（F1-F8）；One-dimensional piece-rate system is connected by M → P → V → C → D → connectable order,
Its outlet is connected to the 4. number mouth of two six-way valve V1 after being mixed with modifier, the 5. number mouth of V1 connects the 4. number mouth of V2, and V2 is 5.
Number mouth connects the 4. number mouth of V3, and the 5. number mouth of V3 connects the 4. number mouth of V4, and the 5. number mouth of V4 connects the 4. number mouth of V5, and a 5. number mouth of V5 connects V6
4. number mouth, the 5. number mouth of V6 connects the 4. number mouth of V7, and the 5. number mouth of V7 connects the 4. number mouth of V8, and a 5. number mouth of V8 connects mobile phase recycling
Device W, formed M → P → V → C → D → V1 4. V1 5. → V2 4. V2 5. → V3 4. V3 5. → V4 4. V4 5. → V5 4. V5
5. → V6 4. V6 5. → V7 4. V7 5. → V8 4. V8 5. → connection mode of W.
A kind of multi-path Two way chromatograms instrument, the number of described two six-way valves is 4-16.
A kind of multi-path Two way chromatograms instrument, described reservoir M, M1, M2, M3, M4, M5, M6, M7, M8 are that resistance to have
The corrosion resistant glass container of solvent or organic material container or rustless steel container.
A kind of multi-path Two way chromatograms instrument, described high-pressure pump P, P1, P2, P3, P4, P5, P6, P7, P8 are to carry
For steady pressure and the constant flow pump or constant pressure pump of flow velocity.
A kind of multi-path Two way chromatograms instrument, the sampling valve V are the sampling valve or sampling pump of fixed volume.
A kind of multi-path Two way chromatograms instrument, the chromatographic column C and C1, C2, C3, C4, C5, C6, C7, C8 are glass
Glass, stainless steel, PEEK；The filler of filling is ion exchange material, normal-phase chromatography filler, reverse-phase chromatography filler, gel filler, is filled out
The amount of material is analytic type, semi-preparative, preparative.
A kind of multi-path Two way chromatograms instrument, described detector D, D1, D2, D3, D4, D5, D6, D7, D8 are ultraviolet
Detector, fluorescence detector, differential refraction detector；The detection cell of detector D is high pressure resistant detection cell.
A kind of multi-path Two way chromatograms instrument of the utility model, has superpower separating capacity；In addition, the utility model
Protrusion effect be：
1. using multi-path two dimensional separation system, it is more that stationary phase may be selected species, and separative efficiency is high, and good separating effect can
Realize the full constituent separation and analysis of complex sample；
2. using multi-path two dimensional separation system, each passage flows phase composition independent control, it is ensured that separation process essence
Really control, improves separating effect；
3. trapping one-dimensional separation component using trapping column, the separated peak stretching of Two way chromatograms, separating effect are effectively inhibited
More preferably；
4. trapped using trapping column and with multiple Two way chromatograms columns be combined carry out two dimensional separation, it is allowed to one-dimensional chromatographic column with
The flow rate of mobile phase of higher is separated, and the preparative available for large sample amount separates；
5. being trapped using trapping column and being combined carry out two dimensional separation with multiple Two way chromatograms columns, the time for having abundance carries out
Two dimensional separation, it is allowed to carry out two dimensional separation using longer Two way chromatograms column, separating effect is more preferable, suitable for all kinds of COMPLEX MIXEDs
Thing isolates and purifies；
6. the trapping of greater number of trapping column can be used, which to be combined with Two way chromatograms column, carries out especially complex sample
Separation, this is not available for current other instruments；
7. the utility model applicability is wide, suitable for normal-phase chromatography, reverse-phase chromatography, ion chromatography, gel chromatography, super face
A variety of chromatographic processes such as boundary's chromatography.
Brief description of the drawings
Fig. 1 is the structure diagram of embodiment multi-path Two way chromatograms instrument；
Fig. 2 is embodiment one-dimensional detector D output signal schematic representations；
Fig. 3 is embodiment two-dimensional detector output signal schematic representation.
Embodiment
The technical solution of the utility model, but protection domain not limited to this are described in detail with reference to embodiment and attached drawing.
Embodiment 1 is as shown in Figure 1, a kind of multi-path Two way chromatograms instrument, including one-dimensional chromatographic fractionation system and multi-path two
Chromatographic fractionation system is tieed up, one-dimensional chromatographic fractionation system is by one-dimensional chromatogram flow phase reservoir M, one-dimensional chromatography high-pressure pump P, one-dimensional color
Sampling valve V, one-dimensional chromatography chromatographic column C and one-dimensional chromatographic detector D compositions are composed, Two way chromatograms piece-rate system is by multiple Two way chromatograms
Mobile phase reservoir M1 to M8, multiple Two way chromatograms high-pressure pump P1 to P8, multiple Two way chromatograms chromatographic column C1 to C8, multiple two dimensions
Chromatographic detector D1 to D8 and fraction collector composition；One-dimensional chromatographic fractionation system and Two way chromatograms piece-rate system passes through multiple two
Position six-way valve V1 to V8 connections, are mounted on a trapping column on each two six-way valves（F1 to F8）.
Connection relation between each component is：The 1. number mouth of each two six-way valves is connected with the outlet that Two way chromatograms pump, 2.
Number mouth is connected with the import of Two way chromatograms column, and the outlet of Two way chromatograms column is connected with the import of two-dimensional detector, two-dimensional detector
Outlet be connected with Fraction collection device, for the two dimensional separation system of 8 paths, formed M1 → P1 → V1 1. V1 2. → C1
→ D1 → collector 1, M2 → P2 → V2 1. V2 2. → C2 → D2 → collector 2, M3 → P3 → V3 1. V3 2. → C3 → D3 →
Collector 3, M4 → P4 → V4 1. V4 2. → C4 → D4 → collector 4, M5 → P5 → V5 1. V5 2. → C5 → D5 → collector 5,
M6 → P6 → V6 1. V6 2. → C6 → D6 → collector 6, M7 → P7 → V7 1. V7 2. → C7 → D7 → collector 7, M8 → P8
→ V8 1. V8 2. → the two dimensional separation connection mode of C8 → D8 → collector 8；Each two six-way valves（V1-V8）3. mouth and
6. be connected 1 trapping column between number mouth（F1-F8）；One-dimensional piece-rate system is connected by M → P → V → C → D → connectable order, its
Outlet is connected to the 4. number mouth of two six-way valve V1 after being mixed with modifier, the 5. number mouth of V1 connects the 4. number mouth of V2, V2 5. number
Mouth connects the 4. number mouth of V3, and the 5. number mouth of V3 connects the 4. number mouth of V4, and the 5. number mouth of V4 connects the 4. number mouth of V5, and a 5. number mouth of V5 connects V6's
4. number mouth, the 5. number mouth of V6 connects the 4. number mouth of V7, and the 5. number mouth of V7 connects the 4. number mouth of V8, and a 5. number mouth of V8 connects mobile phase recover
W, formed M → P → V → C → D → V1 4. V1 5. → V2 4. V2 5. → V3 4. V3 5. → V4 4. V4 5. → 4. V5 is 5. by V5
→ V6 4. V6 5. → V7 4. V7 5. → V8 4. V8 5. → connection mode of W.
F1 trapping columns first rotate V2 close to during trapping completion, connect the 1. 2. internal of V2,4. 3. internal connection, 6. 5.
Inside connection, makes F2 be in trapping state, and then rotating V1 makes V1 1. 6. connect, and 5. 4. connects, 3. 2. connects, V1 connects two dimension
System is in discrete state, and one-dimensional chromatography fluid sequence of flow is at this time：M → P → V → C → D → V1 4. → V1 5. → V2
④→V2③→F2→V2⑥→V2⑤→V3④→V3⑤→V4④→V4⑤→V5④→V5⑤→V6④→V6⑤→V7
4. → V7 5. → V8 4. → V8 5. → W, two-dimentional system fluid sequence of flow is：M1→P1→V1①→V1⑥→F1→V1③→
V1 2. → C1 → D1 → collector 1, M2 → P2 → V2 1. → V2 2. → C2 → D2 → collector 2, M3 → P3 → V3 1. → V3 6.
→ F3 → V3 3. → V3 2. → C3 → D3 → collector 3, M4 → P4 → V4 1. → V4 6. → F4 → V4 3. → V4 2. → C4 → D4
→ collector 4, M5 → P5 → V5 1. → V5 6. → F5 → V5 3. → V5 2. → C5 → D5 → collector 5, M6 → P6 → V6 1. →
V6 6. → F6 → V6 3. → V6 2. → C6 → D6 → collector 6, M7 → P7 → V7 1. → V7 6. → F7 → V7 3. → V7 2. → C7
→ D7 → collector 7, M8 → P8 → V8 1. → V8 6. → F8 → V8 3. → V8 2. → C8 → D8 → collector 8.V2 connects at this time
F2 is in trapping state, and V1 connects Two way chromatograms system and is in discrete state, and the efflux of detector D1 enters fraction collector
F1 is collected.
When F2 trap complete when, then rotate V3 and V2, F3 be in trapping state, V2 connects Two way chromatograms system in dividing
From state, operate successively to V8.If one-dimensional separation does not complete also at this time, subsequent cycle can be proceeded by from V1, until one-dimensional
Chromatographic isolation is completed.
By above-mentioned connection and mode of operation, the Two way chromatograms separation of Fructus Sophorae extract is carried out：
First dimension chromatographic column is ODS columns, and length is 25 cm.One-Dimensional flows are mutually the phosphoric acid of methanol -0.1%, gradient elution（First
Alcohol is changed into 60% in 0-20min from 5%, volume ratio）, flow velocity 1ml/min.Second dimension chromatographic column is ODS columns, length 25
cm.Two-dimensional flow phase M1 is the phosphoric acid of methanol -0.1%（0-20min is 70/30 after being 10/90,20min, volume ratio）, M2 is
The phosphoric acid of methanol -0.1%（0-20min is 70/30 after being 15/85,20min, volume ratio）, M3 is the phosphoric acid of methanol -0.1%（0-
20min is 70/30 after being 25/75,20min, volume ratio）, M4 is the phosphoric acid of methanol -0.1%（0-20min is 35/65,
It is 75/25 after 20min, volume ratio）, M5 is the phosphoric acid of methanol -0.1%（0-20min is 75/25 after being 45/55,20min,
Volume ratio）, M6 is the phosphoric acid of methanol -0.1%（0-20min is 75/25 after being 55/45,20min, volume ratio）, M7 for methanol-
0.1% phosphoric acid（0-20min is 75/25 after being 65/35,20min, volume ratio）, M8 is the phosphoric acid of methanol -0.1%（0-20min
To be 75/25 after 70/30,20min, volume ratio）.The flow velocity of two-dimensional flow phase is 1.0ml/min.Each trapping column trapping
Time is 2min, and each detector is UV detector, and Detection wavelength is 254nm.
One-dimensional detector D output signal schematic representations when the utility model embodiment is separated are shown in attached drawing 2, two-dimensional detection
Device output signal schematic representation is shown in attached drawing 3, and one-dimensional separation can be separated main component it can be seen from Fig. 2 and Fig. 3, but be gone back
There are some components to separate undesirable, chromatographic peak has coincidence, and two dimensional separation can be completely isolated by the peak component of coincidence.
Thus the utility model separative efficiency height is illustrated, it is highly practical, it is particularly suitable for the complex systems such as Chinese medicine, body fluid
The separation of the difficult separate substance such as full component separation and structure analogue compounds.
The present invention is in project of national nature science fund project（21675071）Support under complete, hereby thank you.
Claims (7)
1. a kind of multi-path Two way chromatograms instrument, it is characterized in that, including one-dimensional chromatographic fractionation system and the separation of multi-path Two way chromatograms
System, wherein one-dimensional chromatographic fractionation system is by one-dimensional chromatogram flow phase reservoir M, one-dimensional chromatography high-pressure pump P, one-dimensional chromatography column feed materials
Valve V, one-dimensional chromatography chromatographic column C and one-dimensional chromatographic detector D compositions；Multi-path Two way chromatograms piece-rate system is by multiple Two way chromatograms
Mobile phase reservoir M1 to M8, multiple Two way chromatograms high-pressure pump P1 to P8, multiple Two way chromatograms chromatographic column C1 to C8, multiple two dimensions
Chromatographic detector D1 to D8 and fraction collector composition；One-dimensional chromatographic fractionation system and multi-path Two way chromatograms piece-rate system passes through
Multiple two six-way valve V1 to V8 connections, are mounted on a trapping column on each two six-way valves, are represented respectively with F1 to F8；
Connection relation between each component is：The 1. number mouth of each two six-way valves is connected with the outlet that Two way chromatograms pump, 2. number mouth
Import with Two way chromatograms column is connected, and the outlet of Two way chromatograms column is connected with the import of two-dimensional detector, and two-dimensional detector goes out
Mouthful be connected with Fraction collection device, for the two dimensional separation system of 8 paths, formation M1 → P1 → V1 1. V1 2. → C1 → D1
→ collector 1, M2 → P2 → V2 1. V2 2. → C2 → D2 → collector 2, M3 → P3 → V3 1. V3 2. → C3 → D3 → collection
Device 3, M4 → P4 → V4 1. V4 2. → C4 → D4 → collector 4, M5 → P5 → V5 1. V5 2. → C5 → D5 → collector 5, M6
→ P6 → V6 1. V6 2. → C6 → D6 → collector 6, M7 → P7 → V7 1. V7 2. → C7 → D7 → collector 7, M8 → P8 →
V8 1. V8 2. → the two dimensional separation connection mode of C8 → D8 → collector 8；Each two six-way valves（V1-V8）3. mouth and 6.
Be connected 1 trapping column between number mouth（F1-F8）；One-dimensional piece-rate system is connected by M → P → V → C → D → connectable order, it goes out
Mouth is connected to the 4. number mouth of two six-way valve V1 after being mixed with modifier, the 5. number mouth of V1 connects the 4. number mouth of V2, the 5. number mouth of V2
Even the 4. number mouth of V3, the 5. number mouth of V3 connect the 4. number mouth of V4, and the 5. number mouth of V4 connects the 4. number mouth of V5,4. a 5. number mouth of V5 connects V6
Number mouth, the 5. number mouth of V6 connect the 4. number mouth of V7, and the 5. number mouth of V7 connects the 4. number mouth of V8, and a 5. number mouth of V8 connects mobile phase recover W,
Formed M → P → V → C → D → V1 4. V1 5. → V2 4. V2 5. → V3 4. V3 5. → V4 4. V4 5. → V5 4. V5 5. →
V6 4. V6 5. → V7 4. V7 5. → V8 4. V8 5. → connection mode of W.
2. a kind of multi-path Two way chromatograms instrument as claimed in claim 1, it is characterized in that, the number of described two six-way valves is
4-16.
3. a kind of multi-path Two way chromatograms instrument as claimed in claim 1, it is characterized in that, the reservoir M, M1, M2, M3, M4,
M5, M6, M7, M8 are the corrosion resistant glass container of organic solvent-resistant or organic material container or rustless steel container.
4. a kind of multi-path Two way chromatograms instrument as claimed in claim 1, it is characterized in that, the high-pressure pump P, P1, P2, P3, P4,
P5, P6, P7, P8 are the constant flow pump or constant pressure pump that can provide steady pressure and flow velocity.
5. a kind of multi-path Two way chromatograms instrument as claimed in claim 1, it is characterized in that, the sampling valve V is fixed volume
Sampling valve or sampling pump.
6. a kind of multi-path Two way chromatograms instrument as claimed in claim 1, it is characterized in that, the chromatographic column C and C1, C2, C3,
C4, C5, C6, C7, C8 are glass, stainless steel, PEEK；The filler of filling is ion exchange material, normal-phase chromatography filler, anti-phase color
Filler, gel filler are composed, the amount of filler is analytic type, semi-preparative, preparative.
7. a kind of multi-path Two way chromatograms instrument as claimed in claim 1, it is characterized in that, the detector D, D1, D2, D3, D4,
D5, D6, D7, D8 are UV detector, fluorescence detector, differential refraction detector；The detection cell of detector D is high pressure resistant detection
Pond.
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| CN201720845007.2U CN207307262U (en) | 2017-07-13 | 2017-07-13 | A kind of multi-path Two way chromatograms instrument |
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| CN201720845007.2U CN207307262U (en) | 2017-07-13 | 2017-07-13 | A kind of multi-path Two way chromatograms instrument |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107449839A (en) * | 2017-07-13 | 2017-12-08 | 聊城大学 | A kind of multi-path Two way chromatograms instrument and the method for Two way chromatograms separation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107449839A (en) * | 2017-07-13 | 2017-12-08 | 聊城大学 | A kind of multi-path Two way chromatograms instrument and the method for Two way chromatograms separation |
| CN107449839B (en) * | 2017-07-13 | 2020-04-14 | 聊城大学 | Multi-channel two-dimensional chromatograph and method for two-dimensional chromatographic separation |
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