CN106908555A - A kind of chromatogram peak type adjusting means - Google Patents
A kind of chromatogram peak type adjusting means Download PDFInfo
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- CN106908555A CN106908555A CN201710094910.4A CN201710094910A CN106908555A CN 106908555 A CN106908555 A CN 106908555A CN 201710094910 A CN201710094910 A CN 201710094910A CN 106908555 A CN106908555 A CN 106908555A
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- adjusting means
- peak type
- chromatogram
- chromatogram peak
- chromatographic column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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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
- G01N30/28—Control of physical parameters of the fluid carrier
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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
- G01N30/60—Construction of the column
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- General Health & Medical Sciences (AREA)
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention relates to a kind of adjusting means of the chromatogram peak type that can change liquid chromatogram.Adjusting means can be as a kind of individual member of chromatographic column, and chromatogram peak type adjusting means is arranged on the top of chromatographic column inner outlet end sieve plate or the bottom of entrance point sieve plate, and circle convex body structure is extended in the middle of chromatographic column medium.Chromatogram peak type adjusting means is divided into 2 parts：Cup dolly and circle convex body structure, can design the diameter of cup dolly according to the internal diameter of chromatographic column.The component of chromatogram peak type adjusting means core is that, without infiltrative round convex body structure, surface is smooth, symmetrical；The boss body basal diameter of central solid portion and the ratio 0.1 0.9 of chromatogram column internal diameter, the height of boss body and the ratio of column's length are：0.01‑0.30.The periphery of cup dolly is permeable porous network structure, and the two is combined into an entirety.The material of device is including but not limited to stainless steel, lucite, the material without specific adsorption such as polytetrafluoroethylene (PTFE).
Description
Technical field
The present invention relates to chromatographic technology field, and in particular to a kind of adjustable chromatogram peak type in liquid-phase chromatographic column
Device.
Background technology
Liquid chromatography technology is that one kind efficiently separates purification technique, is widely applied in many fields, such as：Chemical industry,
Biology, food, medicine etc..Wherein, chromatographic column is the core of liquid chromatogram, is to realize the main place that material is separate, energy
The performance for isolating and purifying is directly affected, is all the time core and the forward position of liquid chromatography technology research field.
The separating effect of chromatographic column is depending on the property of fixing phase and its power interacted with solute (mainly by separating
The property of medium is determined)；Meanwhile, also with widening about (the main flow regime institute by mobile phase inside chromatographic column
Determine).1966, Knox et al. disclosed common filled-type chromatographic column and there is radial direction heterogeneity by the method for local detection
Property.Afterwards, the inhomogeneity of the chromatographic column such as integral post is confirmed successively.Research shows：Mobile phase linear flow rate, chromatographic column office
There is radial direction inhomogeneity in the local concentration of portion post effect and determinand, the relation of these values and radial position parabolically shape
Shape.Wherein, the linear flow rate about 2%-8% lower than central region flow velocity at chromatographic column post jamb, occurrence depends on filling
Property；The component efficiency highest of chromatographic column central area；Analyte concentration shows certain in the radial direction in chromatographic column
Fluctuation.
Then, G.Guiochon researchs show to imitate chromatographic column higher for post, and inhomogeneity influences bigger to it；And
In card actual efficiency highest chromatographic column, the difference that gained local velocity, component efficiency and analyte local concentration show is most
It is small.D.V.Dusschoten et al. thinks that the post effect of chromatographic column depends on the radially uniform property of chromatographic column, packed density
Localised waving can corresponding affect on local porosity, permeability and chromatographic column keeping characteristics.
The radial direction inequality of chromatographic column directly results in analyte band distance stretching diametrically, causes chromatographic peak to become
Width, hangover increases, column efficiency reduction.And this radial direction inequality is generally existing and is difficult to eliminate, column efficiency
Chromatographic column higher, the influence that its radial direction inequality is brought is bigger.
The research of radial direction inequality increasingly becomes a focus in chromatogram research field.In recent years by Camenzuli etc.
A kind of parallel divisional flow chromatography technology for proposing has been widely recognized and studies.The core design of this technology is one same
The dispenser of heart circle, its core and outer perimeter section are the porous materials of water penetration, and a ring of centre is non-permeable
Peek materials, matching is special termination design, and mobile phase can be divided into outer peripheral portion and core by it.
This technology is respectively placed in the arrival end of chromatographic column and the port of export and can obtain two kinds of different application theories.When this structure is put
When chromatographic column arrival end, can be from central area sample introduction, then this can be just that mobile phase is not exposed in certain distance
Borderline region, reduces the influence of radial direction inequality.When this structure is placed in the port of export of chromatographic column, can only be received in sampling
Collect the sample of central area, can thus exclude is influenceed larger borderline region, great optimizing detection by radial direction inequality
Peak.Fabrice Gritti etc. have carried out the assessment of reality to the effect of parallel divisional stream, as a result show, parallel divisional stream can be with
It is effective to reduce inequality, improve post effect.But with the increase of column length, the lifting that parallel divisional stream is imitated to post can decline relatively,
But still have apparent effect.Meanwhile, particle diameter is bigger, and increase column length is smaller to the influence that post is imitated.Because, in speed
In the case of homogeneous, the mass transfer coefficient of dispersion increases with the increase of particle diameter.Generally speaking, parallel divisional stream is particularly suitable for analysis
The analytical column of small molecule.It is well suited for those short, chromatographic columns of narrower bore simultaneously, because the component of these pillars is in flowing
During can not reach radial equilibrium.
Mobile phase distributes the function of fluid by sieve plate after entering in chromatographic column, and mobile phase enters color with parallel planar
In spectrum post, its flow regime is determined by the property and occupied state of interior media.And research shows, flow regime is straight in chromatographic column
Connect influence its column efficiency, therefore, by change in chromatographic column flow regime so as to improve column efficiency have theoretical foundation and
Feasibility.
The content of the invention
The present invention relates to a kind of adjusting means of the chromatogram peak type that can change liquid chromatogram.Adjusting means can be as chromatogram
A kind of individual member of post, chromatogram peak type adjusting means is arranged on top or the entrance point sieve plate of chromatographic column inner outlet end sieve plate
Bottom, circle convex body structure is extended in the middle of chromatographic column medium.When adjusting means is arranged on chromatographic column inner outlet end, flowing
Along boss body structural outer flow down, the fast fluid of the center flow velocity fluid slower with nearly wall part flow velocity can be made to converge
Close, influence of the inequality to chromatographic peak profile in regulation chromatographic column.When adjusting means is arranged on entrance point in chromatographic column, stream
The dynamic convex body surface flow that hands down enters, natural to converge to center, with the migration of mobile phase, the stream at center mobile phase and nearly wall
Dynamic phase axially downwards coincide by migration distance, weakens the inequality of flowing.Experiment finds that chromatogram peak type adjusting means can be effective
Reduce the asymmetry of chromatographic peak, theoretical cam curve is dramatically increased, effectively improve post effect.
Chromatogram peak type adjusting means is divided into 2 parts：Cup dolly and circle convex body structure, can set according to the internal diameter of chromatographic column
Count the diameter of cup dolly.The component of chromatogram peak type adjusting means core is without infiltrative round convex body structure, surface light
It is sliding, it is symmetrical；The boss body basal diameter of central solid portion and the ratio 0.1-0.9 of chromatogram column internal diameter, the height of boss body
Spend and be with the ratio of column's length：0.01-0.30.The periphery of cup dolly is permeable porous network structure, and the two can
It is combined into an entirety.The material of device is including but not limited to stainless steel, lucite, and polytetrafluoroethylene (PTFE) etc. is inhaled without specificity
Attached material.Its schematic diagram is as shown in Figure 2.
For chromatogram peak type adjusting means, same chromatographic column is put into, changes the basal diameter and Gao Douke of boss body body
To change the peak type of chromatogram appearance, optimal ratio and size is selected according to actual conditions, peak figure is most preferably gone out to obtain.
Brief description of the drawings
Fig. 1 chromatogram peak type adjusting means structural representations (one of which) of the present invention.
The assembling schematic diagram of Fig. 2 chromatogram peak type adjusting meanss
Specific embodiment
The present invention devises a kind of chromatogram peak type adjusting means, chromatogram peak type adjusting means be arranged on column outlet end or
The sieve plate top of entrance point, circle convex body structure is extend into chromatographic column, and the device can change the migration of mobile phase in chromatographic column
Track, weakens the radial direction inequality of mobile phase in chromatographic column, is effectively improved the peak height that chromatogram goes out peak figure, peak width and peak it is symmetrical
Property, improve post effect.
Below with regard to chromatogram peak type adjusting means of the invention and produced effect, instantiation is coordinated to describe in detail such as
Under：
Example 1：
Internal diameter 25mm, the upper end of the chromatographic column of length 100mm are turned on, boss body portion ground is installed in chromatographic column entrance point
Radius surface is 15mm, the chromatogram peak type adjusting means of 10mm high, 400 mesh chromatography silica gels is washed with ethanol, then stirred into ethanol
, be uniformly filled in chromatography silica gel in gc column tube using homogenate method by homogenate, and chromatogram column cap is tightened after filling up.
Chromatogram peak type adjusting means is in chromatographic column entrance point.The chromatogram of device for installing and adjusting is not installed under the same conditions and
As a result post shows as control：Under certain size ratio, the chromatogram of the chromatographic column equipped with chromatogram peak type adjusting means goes out peak figure
Peak height be increased compared with common chromatographic column, peak width has also been reduced, meanwhile, chromatogram peak type adjusting means goes out dragging for peak figure
The tail factor is smaller than common chromatographic column, and chromatogram goes out peak figure symmetry and is obviously improved.
Example 2
Internal diameter 25mm, the upper end of the chromatographic column of length 100mm are turned on, boss body portion ground is installed at column outlet end
Radius surface is 15mm, the chromatogram peak type adjusting means of 15mm high, 400 mesh chromatography silica gels is washed with ethanol, then stirred into ethanol
, be uniformly filled in chromatography silica gel in gc column tube using homogenate method by homogenate, and chromatogram column cap is tightened after filling up.
Chromatogram peak type adjusting means is at column outlet end.The chromatogram of device for installing and adjusting is not installed under the same conditions and
As a result post shows as control：Under certain size ratio, the chromatogram of the chromatographic column equipped with chromatogram peak type adjusting means goes out peak figure
Peak height be increased compared with common chromatographic column, peak width has also been reduced, meanwhile, chromatogram peak type adjusting means goes out dragging for peak figure
The tail factor is smaller than common chromatographic column, and chromatogram goes out peak figure symmetry and is obviously improved.
Claims (6)
1. the device of a kind of adjustable chromatogram peak type in liquid-phase chromatographic column, by changing liquid-phase chromatographic column exit region stream
The migration path of dynamic phase, can influence the distribution of widening, so as to adjust the chromatogram peak type of detection response.Device master
Body structure is the compound framework of boss body and annular bottom, can be obtained by the different proportion of its size and gc column tube size
Obtain different chromatogram peak types.
2. chromatogram peak type adjusting means according to claim 1, it is characterised in that chromatogram peak type adjusting means is by without infiltration
Property boss body central component and peripheral permeable annular substructure member composition, an entirety can be combined into.
3. chromatogram peak type adjusting means according to claim 1, it is characterised in that the boss body bottom surface of central solid portion
Diameter, its size is the 0.1-0.9 of chromatogram column internal diameter, and the height of boss body and the ratio of column's length are：0.01-0.30.
4. chromatogram peak type adjusting means according to claim 1, it is characterised in that the bottom circle of chromatogram peak type adjusting means
Annular diameter size is matched with an applicable liquid-phase chromatographic column diameter dimension.
5. chromatogram peak type adjusting means according to claim 1, it is characterised in that chromatogram peak type adjusting means is placed in chromatogram
Post entrance point and outlet section, detachably.
6. chromatogram peak type adjusting means according to claim 1, it is characterised in that the material of device is to include but is not limited to
The material without specific adsorption such as stainless steel, lucite, polytetrafluoroethylene (PTFE).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710094910.4A CN106908555A (en) | 2017-02-22 | 2017-02-22 | A kind of chromatogram peak type adjusting means |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710094910.4A CN106908555A (en) | 2017-02-22 | 2017-02-22 | A kind of chromatogram peak type adjusting means |
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| CN106908555A true CN106908555A (en) | 2017-06-30 |
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| CN201710094910.4A Pending CN106908555A (en) | 2017-02-22 | 2017-02-22 | A kind of chromatogram peak type adjusting means |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108680685A (en) * | 2018-05-17 | 2018-10-19 | 北京化工大学 | A kind of multi-path parallel divisional ring chromatographic column |
| CN111737684A (en) * | 2020-08-10 | 2020-10-02 | 武汉生之源生物科技股份有限公司 | Data safety control method in biochemical analyzer system |
-
2017
- 2017-02-22 CN CN201710094910.4A patent/CN106908555A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108680685A (en) * | 2018-05-17 | 2018-10-19 | 北京化工大学 | A kind of multi-path parallel divisional ring chromatographic column |
| CN108680685B (en) * | 2018-05-17 | 2020-07-24 | 北京化工大学 | Multi-channel parallel segmentation ring chromatographic column |
| CN111737684A (en) * | 2020-08-10 | 2020-10-02 | 武汉生之源生物科技股份有限公司 | Data safety control method in biochemical analyzer system |
| CN111737684B (en) * | 2020-08-10 | 2020-12-08 | 武汉生之源生物科技股份有限公司 | Data safety control method in biochemical analyzer system |
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Application publication date: 20170630 |