CN217909072U - Non-equal-diameter extraction column - Google Patents
Non-equal-diameter extraction column Download PDFInfo
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- CN217909072U CN217909072U CN202222195391.XU CN202222195391U CN217909072U CN 217909072 U CN217909072 U CN 217909072U CN 202222195391 U CN202222195391 U CN 202222195391U CN 217909072 U CN217909072 U CN 217909072U
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Abstract
The utility model provides a non-equal footpath extraction column, including the column pipe to the inflow end of mobile phase is as the upper end, the column pipe divide into upper segment and hypomere, and the internal diameter of upper segment > the internal diameter of hypomere. The non-equal-diameter extraction column can bear large-volume sample introduction and focus a target object in a large-volume sample, and has good column effect and long service life.
Description
Technical Field
The utility model relates to a liquid chromatogram field, concretely relates to extraction column.
Background
In solid phase extraction systems, on-line processing of samples is often performed using a chromatography column, typically an extraction column for sample processing. During the hue chromatographic analysis, certain samples have relatively complex components and low target object content, and large-volume sample injection is needed during online extraction, so that the function of enriching and purifying the target object is realized. However, for large-volume sample injection, the conventional extraction column is difficult to bear (the sample injection amount is generally about 20-50 microliters), most of the conventional extraction columns are equal-diameter extraction columns, the linear velocities of mobile phases in the columns are kept consistent, and for some medicines which are not easy to focus, the problems of poor focusing capability and the like occur. Meanwhile, the mobile phase can generate impurities such as particles, and when the radius of a column head is smaller, the column pressure is easier to rise, so that the service life of the extraction column is influenced.
According to the search, the prior art also has a chromatographic column with non-equal diameter, for example, CN02106928.X discloses a conical high performance liquid chromatography preparation column. Mainly comprises a column head, a column body and a column tail, and is a conical column body, wherein the inner diameter (2R) of an inlet of the column head is larger than the inner diameter (2R) of an outlet of the column tail. The column head is composed of a conical liquid flow guide groove, a distribution disc and a sieve plate to form a liquid flow distribution system. The distribution disc is composed of a plurality of radial liquid flow channels, concentric liquid flow collecting channels and liquid seepage holes. The inner diameter of the inlet of the column body is 2R = 10mm-2000mm, the inner diameter of the outlet of the column body is 2r = 3mm-1800mm, the column length L = 5cm-100cm, the cone angle is in the range of 1-20 degrees, and various types of chromatographic separation media can be filled in the cone. The conical preparative column can obviously improve the column effect and the sample loading capacity, and the dilution effect on the separation components is lower than that of a cylindrical chromatographic column. However, the column is complicated to process and is not a conventional cylindrical column.
CN201110071563.6 discloses a parabolic high performance liquid chromatography preparative column, which comprises: a column head located at the upper part of the column body, a parabolic tubular column body and a column tail located at the lower part of the column body; the inlet end and the outlet end of the parabolic tubular column body are respectively provided with a special sealing extending piece, the column body is designed in a parabolic shape, and the parabolic equation corresponds to the flow velocity, so that a perfect plug-shaped chromatographic band can be obtained, and the column effect of the chromatographic column is greatly improved; the inner diameter of the column body is gradually reduced, the sample loading amount of the chromatographic column is increased, and a certain amount of enrichment effect is realized on the sample. Such columns should remain in the theoretical stage only and be expensive to process.
Above non-equal diameter chromatographic column all is in order to overcome "pipe wall effect" and research and development, with the utility model discloses a purpose is different, the utility model discloses a solve the liquid chromatogram bulky and advance kind to and focusing power is poor when partial medicine bulky advances kind, the column effect is not good, life is short problem.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a not isodiametric extraction post, solve the problem that the focusing effect of target object is not good, pressure is high easily when the big volume of current extraction post advances kind, the big volume advances kind and is referred to the volume of advancing kind more than 200 mu L.
The technical scheme of the utility model is that:
a non-isodiametric extraction column comprises a column tube, the inflow end of a mobile phase is taken as the upper end, the column tube is divided into an upper section and a lower section, and the inner diameter of the upper section is larger than that of the lower section.
Preferably, the length of the upper section of the non-uniform diameter extraction column accounts for 1/5-3/10 of the whole length of the column tube extraction column. After a great deal of research by the inventor, the method is suitable in the range, can be suitable for large-volume sample injection, also keeps good column efficiency of the whole body, and does not greatly increase the cost and the analysis time.
Preferably, the ratio of the inner diameter of the upper section to the inner diameter of the lower section of the non-uniform-diameter extraction column is 1.2-1.5. After a great deal of research by the inventor, the method is suitable in the range, can be suitable for large-volume sample introduction, also keeps overall good column efficiency, and does not greatly increase the cost and the analysis time.
Preferably, the column tube is provided with a first connecting section and a first connecting section at the periphery for connecting with the column head, and the outer diameter of the first connecting section and the first connecting section is larger than that of the column tube.
Preferably, the non-uniform-diameter extraction column comprises a column head, a front end column cap, a column tube, a tail end column cap and a column head which are sequentially connected from top to bottom.
Preferably, the column head is provided with an inflow hole for inflow of the mobile phase or an outflow hole for outflow of the mobile phase.
Preferably, the non-isodiametric extraction column, the column tube is filled with the stationary phase.
Preferably, the inlet end of the column tube is provided with a front-end column cap, the outlet end of the column tube is provided with a tail-end column cap, the inlet end and the outlet end of the column tube are arranged in the column head, internal threads are arranged in the column head, and the column tube is connected with the column head through threads.
Preferably, the non-uniform-diameter extraction column is characterized in that the column tube and the column head are made of stainless steel.
Preferably, the upper section and the lower section are filled with different fillers, respectively. Preferably, the upper stage may be filled with a filler such as an inverted filler or an ionic filler, and the lower stage may be filled with a filler such as an inverted filler or an ionic filler, and the filler particle size of the upper stage is larger than that of the lower stage, and the adsorption effect of the upper stage on the target substance is better than that of the lower stage. The two fillers are separated by a stainless steel sieve sheet. Furthermore, the grain diameter of the upper section is between 5 and 50 mu m, and the grain diameter of the lower section is between 2 and 10 mu m.
The utility model discloses a research and development principle explains:
the most common form of van der waals equation is shown below,
wherein H is the height of the theoretical plate, A, B and C are constants, and u represents the linear velocity of the mobile phase in the chromatographic column. This formula intuitively reflects the effect of the linear velocity of the mobile phase in the column on the separation. The greater the linear velocity of the mobile phase in the column, the poorer the column efficiency.
In addition, according to the column rate constant theory, the linear velocity of the mobile phase in the column is inversely proportional to the square of the inner diameter of the column, that is, the smaller the inner diameter of the column, the higher the linear velocity of the mobile phase in the column, and the worse the column efficiency.
Meanwhile, the auxiliary mobile phase is added, so that the flowing elution strength is changed, a large number of target objects in a large-volume sample are gathered together, and the target objects are further separated from other protein impurities.
Then, for large volume injection, in order to obtain better column efficiency, it can be considered to solve the problem of large volume injection from the viewpoint of changing the inner diameter of the column tube, but other problems may also occur if the inner diameter of the extraction column is simply enlarged, such as: 1. more fillers need to be filled, so that the cost of the extraction column is increased; 2. the more the filler, the longer the analysis time; 3. the larger the inner diameter of the chromatographic column is, the more the solvent is contained, and the solvent contained in the chromatographic column can diffuse when being transferred to the next chromatographic column, so that the subsequent analysis is influenced.
Through a great deal of research of the inventor, the inventor develops the non-equal-diameter chromatographic column, which can meet the requirement of large-volume sample introduction, maintain good column efficiency, save the cost and ensure proper analysis time.
The inner diameter of the upper section of the non-isodiametric chromatographic column is larger than the inner diameter of the lower section, the linear velocity of a flowing phase in the upper section of the chromatographic column is small, the separation and the aggregation are facilitated, the non-isodiametric chromatographic column can be well suitable for large-volume sample introduction, the overall good column effect is also kept, meanwhile, the inner diameter of the upper section is relatively large, the pressure is low, the damage to the chromatographic column during large-volume sample introduction can be reduced, and the service life of the extraction column is prolonged. Through the buffering of the upper section of the chromatographic column, the inner diameter of the lower section of the chromatographic column is not required to be as large as that of the upper section, the inner diameter can be reduced, the flow velocity of the mobile phase is improved relative to that of the upper section, the analysis time can be reduced, the using amount of the filler is reduced, and the cost is saved.
Furthermore, because the flow rates of the upper section and the lower section are different, the filling of the filler is further researched, and the upper section and the lower section are respectively filled with different fillers, so that the requirements for separation or enrichment at different flow rates are met. The upper section can be filled with SCX ion filler with strong adsorbability. The lower section can be filled with C18, C8, phenyl, naphthyl and other fillers. The enrichment effect is better through the optimization of the internal filler.
Selection principle of the filler: the grain diameter of the upper section filler is larger than that of the lower section filler, the grain diameter of the upper section filler is generally between 5 and 50 mu m, and the grain diameter of the lower section filler is generally between 2 mu m and 10 mu m. The enrichment capacity of the upper section of the filler on the target object is larger than that of the lower section of the filler on the target object.
Compared with the prior art, the utility model has the advantages that:
the utility model discloses a non-constant diameter extraction post, the pipe diameter internal diameter of pillar pipe upper segment is greater than the internal diameter of hypomere, and when the bulky appearance of advancing, the velocity of flow of upper segment is low, does benefit to separation and gathering, and the adaptation bulky appearance of advancing that can be fine, and keeps whole good column effect equally, improves the life of extraction post, and can not a large amount of incremental cost and analysis time.
The detailed structure of the present invention will be further described with reference to the accompanying drawings and the detailed description.
Drawings
FIG. 1 is a schematic cross-sectional view of a column tube of a non-isometric extraction column;
FIG. 2 is a schematic view of a split structure of a non-isometric extraction column in example 1;
FIG. 3 is a schematic cross-sectional view of the non-isometric extraction column of FIG. 2;
FIG. 4 is a schematic cross-sectional view of an extraction column of example 2 (the upper and lower sections are filled with different packing materials);
FIG. 5 is a diagram of the peak formation of a large volume sample in which the upper and lower sections of a non-equal-diameter extraction column are filled with the same packing;
FIG. 6 is a peak-appearing diagram of a large-volume sample obtained by filling different fillers in the upper and lower sections of a non-equal-diameter extraction column;
FIG. 7 is a graph showing the peak formation of a large volume sample in which the same packing is packed in an equal-diameter extraction column;
FIG. 8 is a comparison chart of examples 1 and 2 and a comparative example;
FIG. 9 is a table comparing the properties of example 1, example 2 and comparative example;
wherein: 1 is column head, 2 is inflow hole, 3 is outflow hole, 4 is front end column cap, 5 is column tube, 5-1 is upper segment, 5-2 is lower segment, 6 is end column cap, 7 is stationary phase, 7-1 upper segment filler, 7-2 lower segment filler.
Detailed Description
Example 1
As shown in fig. 1-3, a non-uniform diameter extraction column comprises a column tube 5, the inflow end of a mobile phase is taken as an upper end, the column tube 5 is divided into an upper section 5-1 and a lower section 5-2, the inner diameter of the upper section 5-1 is 3.5mm, the inner diameter of the lower section 5-2 is 4.6mm, the length of the upper section 5-1 is 5mm, and the length of the lower section 5-1 is 20mm.
From top to bottom the extraction column includes column cap 1, front end cap 4, column tube 5, terminal cap 6 and column cap 1 that connect gradually. An inflow hole 2 for the inflow of the mobile phase or an outflow hole 3 for the outflow of the mobile phase is arranged in the column head 1. The column tube 5 is internally filled with a stationary phase 7.
Further, the inlet end of the column tube 5 is provided with a front-end column cap 4, the outlet end of the column tube 5 is provided with a tail-end column cap 6, the inlet end of the column tube 5 is arranged in the column head 1, internal threads are arranged in the column head 1, the outlet end of the column tube 5 is arranged in the column head 1, internal threads are arranged in the column head 1, and the column tube 5 is connected with the column head 1 through threads. The column tube 5 and the column cap 1 are both made of stainless steel.
Furthermore, in the stationary phase 7, the upper section of 7-1 filler is C8 with a particle size of 10 μm, and the lower section of 7-2 filler is C8 with a particle size of 5 μm.
Example 2
As shown in fig. 4, the specific structure is different from that of embodiment 1 in that: the upper section 5-1 and the lower section 5-2 are respectively filled with different fillers, and the two fillers are separated by a stainless steel sieve sheet. The upper section of the filler 7-1 is filled with SCX ion filler with strong adsorbability, the grain diameter is 5 μm, and the lower section of the filler 7-2 can be filled with C8 filler, the grain diameter is 3.5 μm.
Comparative example 1
The specific structure is different from that of example 1 in that: the upper and lower sections are of equal diameter and are respectively filled with the same filler, the type of the filler is C8, and the grain diameter is 5 mu m.
Extraction columns of 3.5X 25mm were prepared according to example 1, example 2 and comparative example 1. Testing in a two-dimensional liquid chromatography system, wherein a test sample is a valproic acid biological sample, the sample injection volume is 500 mu L, the detector is Shimadzu SPD-20A, the wavelength is 215nm, the mobile phase is 30% acetonitrile, the flow rate is 1.0mL/min, the auxiliary mobile phase is water, the auxiliary flow rate is 2.0mL/min, the auxiliary time is 0.6min, and the column temperature is 40 ℃.
And (3) testing: FIG. 5 is a graph showing the peak formation of a large volume sample in which the upper and lower sections of a non-equal-diameter extraction column are filled with the same packing; FIG. 6 is a peak-appearing diagram of a large-volume sample filled with different fillers at the upper and lower sections of a non-equal-diameter extraction column; FIG. 7 is a graph showing the peak formation of a large volume sample when the same packing is packed in an equal-diameter extraction column; FIG. 8 is a comparison chart of examples 1 and 2 and a comparative example; FIG. 9 is a comparison of the performance of examples 1 and 2 and comparative examples.
And (4) conclusion: when the extraction column with the non-equal diameter is used for testing valproic acid, the focusing capacity is obvious when the sample injection amount is 500 mu L, and when the extraction column with the equal diameter is used for testing valproic acid, the focusing capacity is poor; and the non-equal diameter different packing extraction column has better focusing capability. The better the focusing ability, the larger the theoretical plate number, the more normal the peak shape and the smaller the peak width.
The above description is for the specific implementation of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art should be able to replace or change the technical solution and the design of the present invention within the technical scope of the present invention.
Claims (10)
1. A non-isodiametric extraction column comprises a column tube (5) with a cylindrical inner cavity, and is characterized in that the inflow end of a mobile phase is taken as the upper end, the column tube (5) is divided into an upper section (5-1) and a lower section (5-2), and the inner diameter of the upper section (5-1) is larger than that of the lower section (5-2).
2. The non-constant diameter extraction column as claimed in claim 1, wherein the length of the upper section (5-1) is 1/5-3/10 of the total length of the extraction column of the column tube (5).
3. The non-constant diameter extraction column as claimed in claim 1, wherein the ratio of the inner diameter of the upper section (5-1) to the inner diameter of the lower section (5-2) is 1.2 to 1.5.
4. The extraction column according to any one of claims 1 to 3, wherein the extraction column comprises a column head (1), a front end column cap (4), a column tube (5), a tail end column cap (6) and a column head which are connected in sequence from top to bottom.
5. The extraction column as claimed in claim 4, wherein the column head (1) is provided with an inflow hole (2) for inflow of the mobile phase or an outflow hole (3) for outflow of the mobile phase.
6. A non-isopipe extraction column according to any of claims 1-3, wherein the column tube (5) is filled with stationary phase (7) inside.
7. A non-isometric extraction column as claimed in any one of claims 1 to 3, wherein the inlet end of the column tube (5) is provided with a front end cap (4), the outlet end of the column tube (5) is provided with a rear end cap (6), the inlet end and the outlet end of the column tube (5) are arranged in the column head (1), the column head (1) is internally provided with internal threads, and the column tube (5) and the column head (1) are connected through threads.
8. A non-isometric extraction column according to any one of claims 1-3, characterized in that the upper section (5-1) and the lower section (5-2) can be filled with the same packing or with different packings.
9. The non-constant diameter extraction column according to claim 8, wherein any one of an ion-based packing, a C18, a C8, a phenyl and a naphthalene-based packing is filled in the upper section (5-1) and the lower section (5-2), respectively.
10. The non-isometric extraction column of claim 9 wherein the upper section has a larger particle size than the lower section, and further wherein the upper section has a particle size of between 5 μm and 50 μm and the lower section has a particle size of between 2 μm and 10 μm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116585752A (en) * | 2023-07-18 | 2023-08-15 | 成都百泉生物医药科技有限公司 | Chromatographic column and oscillating device for chromatographic column |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116585752A (en) * | 2023-07-18 | 2023-08-15 | 成都百泉生物医药科技有限公司 | Chromatographic column and oscillating device for chromatographic column |
| CN116585752B (en) * | 2023-07-18 | 2023-10-20 | 成都百泉生物医药科技有限公司 | Chromatographic column and oscillating device for chromatographic column |
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