CN201522480U - Spherical high-performance liquid chromatogram preparation column - Google Patents
Spherical high-performance liquid chromatogram preparation column Download PDFInfo
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- CN201522480U CN201522480U CN2009202099247U CN200920209924U CN201522480U CN 201522480 U CN201522480 U CN 201522480U CN 2009202099247 U CN2009202099247 U CN 2009202099247U CN 200920209924 U CN200920209924 U CN 200920209924U CN 201522480 U CN201522480 U CN 201522480U
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Abstract
The utility model relates to a spherical high-performance liquid chromatogram preparation column which comprises a column head, an adjustable pre-column, a spherical column body and a column tail; the column head and the column tail are respectively matched at the upper end of the adjustable pre-column and an outlet pipe at the lower end of the spherical column body by nut caps and threads; and the specific points are as follows: the inner diameter R of the column body is 50 to 2000mm, the inner diameter r of the adjustable pre-column is 0.1R to 0.2R, the column length L is 0.2R to 0.3R, and the inner diameter of the column outlet is 5mm. The column has the advantages that: the adjustable pre-column and the spherical column body are connected and adjustable, the mending technology of the chromatographic column can be simplified, and the service life of the column can be prolonged; the shape of the upper half column body of the spherical column can overcome the 'column wall effect', thus effectively improving column efficiency; the inner diameter of the lower half spherical column body is reduced gradually, thus having certain enriching effect to samples; the column head and the column tail use sieve plates with small diameters, thus greatly reducing preparation cost; furthermore, the spherical liquid chromatogram preparation column has simple filling and convenient operation.
Description
[technical field]
The utility model relates to the liquid-phase chromatographic column technical field, specifically, is a kind of spherical high performance liquid chromatography preparative column.
[background technology]
Since Tswett in 1906 founded chromatography, analytic type chromatogram and preparative scale chromatography had all obtained tremendous development, extensively apply to the every field in the productive life.First preparative liquid chromatography truly separate be in the thirties in 20th century to plant metabolites---the separation of pigment.The main effect of preparative scale chromatography is the separation to secondary class metabolic product and natural products, for macromolecular separation and purification, chromatographic resolution also is used to separate some important medicinal organism activated protein, biological therapy product and diagnostic reagent, to meet requirement of high purity.In order to satisfy the demand of high-purity, high yield, people are in the preparative chromatography pattern of seeking a kind of high separating efficiency.For the requirement of high separating efficiency, the research of new packing and the development of new column packing technique have been promoted.In recent years, the post that how to improve preparative liquid chromatography is imitated and selectivity, reduces production costs, and obtains the focus that high-purity sample becomes research.
In order to take into account sample size and separation efficiency simultaneously, people once considered a large diameter post is connected with a little internal diameter post, provided big column capacity by front large diameter post, and the little internal diameter post in back provides effective separation.But experiment finds that series connection can not effectively improve post and imitate.1981, Said had better effect by Theoretical Calculation proof tapered pole.Nineteen ninety, the Moerker Theophile of Switzerland has invented the tapered pole that a kind of internal diameter enlarges gradually, because cylindricality has met the trend that spreads to tube wall gradually when sample flows in bamboo, solute band can not be diffused into tube wall, thereby overcome " wall effect ", present " infinite diameter effect ", improved the post effect greatly.2005, Guan Yafeng etc. invented the diminishing tapered pole of a kind of internal diameter, because the opening internal diameter is greater than the outlet internal diameter, thereby applied sample amount is big, and the diluted sample effect is diminished, and has also effectively improved the post effect.But so far, less than report about spherical preparative chromatography post.
[utility model content]
The purpose of this utility model is to overcome the deficiencies in the prior art, and a kind of spherical high performance liquid preparative chromatography post is provided.
The purpose of this utility model is achieved through the following technical solutions:
A kind of spherical high performance liquid chromatography preparative column comprises column cap, adjustable pre-column, spherical cylinder and post tail; Column cap and post tail are assigned in the outlet of the upper end and the spherical cylinder lower end of adjustable pre-column respectively with nut and screw thread;
Described column cap comprises nut, screw thread, gathering sill, O-ring seal, distribution plate and porous sieve plate; Column cap is assigned in the upper end of adjustable pre-column with nut and screw thread, under the gathering sill that the column cap inner face is recessed into O-ring seal is arranged, distribution plate and the porous sieve plate that is complementary with adjustable pre-column internal diameter;
Described adjustable pre-column is cylindrical adjustable pre-column, and its internal diameter r is less than spherical column diameter R, r=0.1R～0.2R, and column length L=0.2R～0.3R, all there is screw thread adjustable pre-column upper/lower terminal outside, links to each other with cylinder with column cap respectively;
Described spherical cylinder comprises induction pipe, first spherical cylinder, ring flange, second O-ring seal, bolt, second spherical cylinder and outlet; Ring flange and second the spherical cylinder that forms protruded in ring flange, second O-ring seal, bolt, second outside, spherical cylinder upper edge of having its outside, lower edge protrusion to form under first spherical cylinder; Upper and lower semisphere cylinder is with ring flange, bolt seal; An import is opened at the top of described first spherical cylinder, and the post jamb outside is outwards protruded and formed a 20mm elongated cylindrical induction pipe; Induction pipe internal diameter and adjustable pre-column coupling, its inner face has screw thread, is connected with adjustable pre-column by screw thread; First outside, spherical cylinder lower edge post jamb outwards protrudes, and forms 4 equally distributed ring flanges; Described second outside, spherical cylinder upper edge post jamb outwards protrudes, and forms 4 ring flanges corresponding with the ring flange of first spherical cylinder; One diameter is arranged at its bottom is the opening of 5mm, and the cylindrical outlet pipe that forms a long 10mm, internal diameter 5mm is outwards protruded in the opening outside; This outlet inner face has screw thread, and second spherical column jecket links to each other with the post tail with screw thread by this outlet;
Column diameter R=50～the 2000mm of described spherical cylinder;
Described post tail comprises porous sieve plate, O-ring seal, screw thread, gathering sill and nut; The gathering sill, the O-ring seal that have post tail inner face to be recessed on the spiral shell tail reach the porous sieve plate that is complementary with the outlet internal diameter, and the post tail is assigned in the outlet lower end with nut and screw thread.
The cylinder that the utility model uses is spherical cylinder, and in the spheroid, distance is equal everywhere apart from sphere for the centre of sphere; By fluid dynamics as can be known, the stressed everywhere size of this spherical cylinder tube wall is consistent; Thereby use simple column packing technique, and can fill out chromatographic column even in the cylinder, Gao Zhuxiao everywhere, simplified dress post process; This cylinder episphere part is the cylindricality that column internal diameter enlarges gradually, the diffusion tendency when meeting sample and in cylinder, flowing, and solute band can not be diffused into tube wall, thereby has overcome " wall effect ", presents " infinite diameter effect ", can improve post greatly and imitate; Cylinder lower semisphere part, it is the cylindricality that column internal diameter reduces gradually, have and the tapered pole identity function, make amplitude that tube wall district moving phase linear velocity increases greater than the post center, and the moving phase linear velocity progressively reduces to the post center from post inner tubal wall district, thereby make chromatogram bands of a spectrum flow pattern be parabolic shape down, thereby can effectively improve the post effect; And internal diameter reduces gradually, and sample is had certain concentration effect, and the solvent that therefore only needs to handle still less in preparation is produced just can obtain the same product, can reduce solvent consumption, reduces production costs.
Spherical liquid chromatography preparative column of the present utility model can be filled two kinds of particle diameter fillers; The bulky grain filler of particle diameter greater than packing material size in the cylinder can be filled in adjustable pre-column and spherical cylinder porch in this chromatographic column; This fills bulky grain filler part, and effect is equivalent to a fluid distribution plate, and sample and moving phase are carried out secondary distribution, makes them evenly enter cylinder, makes full use of filler in the cylinder, improves separation efficiency; The filler contact area has increased inlet area indirectly greater than adjustable pre-column cross-sectional area in bulky grain filler and the cylinder, thereby has increased the sample charge capacity.
Compared with prior art, good effect of the present utility model is:
The adjustable pre-column that the utility model uses, itself and cylinder are connected to flexible connection, can move up and down by rotation, adjust the length that it enters induction pipe, summarized chromatogram post repairing technique; When reasons such as chromatographic column is long because of service time, on-stream pressure is excessive, chromatographic condition is improper cause filler to subside, cavity appears in the cylinder, post is pressed significantly and is descended, post is imitated when sharply reducing: general repairing method is to pull down column cap, replenish chromatograph packing material of the same race at column cap, this repairing method needs certain operation skill, and often causes the chromatographic column post to imitate decline, so many times need to refill chromatographic column; The design of adjustable pre-column in the utility model makes chromatographic column subside afterwards to repair and becomes extremely simple, only needs adjustable pre-column is down screwed, extruding cylinder filler, replenish the cylinder cavity filler, thereby make chromatographic column arrive the complete filling state again, reach the repairing effect of post; Therefore, this design can prolong post serviceable life, and then provides cost savings greatly.
It has simplified the adjustable pre-column that the utility model uses and has mixed the sample operation; In preparative chromatography, a lot of samples all are the slightly solubility samples, take to mix the sample input mode in the mesolow preparative chromatography; It is that column cap is pulled down that routine is mixed the sample operation, digs out a certain amount of filler from post head, with after filler and the sample mix oven dry, inserts in the chromatographic column more then; And this mode is often infeasible in the high pressure preparation, and is very high because the filling of high pressure preparative column requires, and mixes sample loading mode and can cause high pressure preparative column post to imitate significantly decline; Spherical chromatographic column of the present utility model can adopt mixes the sample input mode, and it is simple to operate: at first adjustable pre-column is pulled down, got required filler from adjustable pre-column, mix the adjustable pre-column of packing into behind the sample, then adjustable pre-column is connected with cylinder, screws adjustable pre-column, filling compaction is got final product; Thereby the design provides a kind of new input mode to high pressure preparation, expanded the range of application of high pressure preparative chromatography.
Spherical chromatographic column of the present utility model is used little internal diameter sieve plate; The adjustable pre-column of this chromatographic column and outlet internal diameter be all less than column diameter, and the sieve plate that is complementary with them that therefore uses all is minor diameter sieve plates, and this has very important meaning for the preparative chromatography post; Because the major diameter sieve plate price of using in the preparative chromatography post is higher, the utility model only uses the minor diameter sieve plate, can reduce the cost of sieve plate, thereby reduces preparative chromatography post cost.
[description of drawings]
The spherical high performance liquid chromatography preparative column of Fig. 1 the utility model synoptic diagram;
Mark in the accompanying drawing is respectively: 1, column cap, 2, nut, 3, gathering sill, 4, distribution plate, 5, sieve plate, 6, O-ring seal, 7, adjustable pre-column, 8, induction pipe, 9, spherical cylinder, 10, first spherical cylinder, 11, ring flange, 12, second O-ring seal, 13, bolt, 14, second spherical cylinder, 15, the post tail, 16, granule filler, 17, the bulky grain filler, 18, outlet.
[embodiment]
The embodiment of a kind of spherical high performance liquid chromatography preparative column of the utility model below is provided.
See also accompanying drawing 1, a kind of spherical high performance liquid chromatography preparative column comprises column cap 1, adjustable pre-column 7, spherical cylinder 9 and post tail 15; Column cap 1 and post tail 15 are assigned in adjustable pre-column 7 upper ends and spherical cylinder 9 lower end outlets 18 with nut 2 and screw thread respectively;
Described column cap comprises nut 2, screw thread, gathering sill 3, O-ring seal 6, distribution plate 4 and porous sieve plate; Column cap 1 is assigned in adjustable pre-column upper end with nut and screw thread, under the gathering sill that column cap 1 inner face is recessed into O-ring seal 6 is arranged, distribution plate 4 and the porous sieve plate that is complementary with adjustable pre-column internal diameter;
Described adjustable pre-column 7 is cylindrical adjustable pre-column, and its internal diameter r is less than spherical column diameter R, r=0.1R～0.2R, and column length L=0.2R～0.3R, all there is screw thread adjustable pre-column upper/lower terminal outside, links to each other with spherical cylinder 9 respectively at column cap 1;
Described spherical cylinder 9 comprises induction pipe 8, first spherical cylinder 10, ring flange 11, second O-ring seal 12, bolt, second spherical cylinder and outlet 18; Ring flange and second the spherical cylinder that forms protruded in ring flange 11, second O-ring seal 12, bolt 13, second outside, spherical cylinder upper edge of having its outside, lower edge protrusion to form under first spherical cylinder; Upper and lower semisphere cylinder is with ring flange 11, bolt 13 sealings; An import is opened at first spherical cylinder top, and the post jamb outside is outwards protruded and formed a 20mm elongated cylindrical induction pipe; Induction pipe internal diameter and adjustable pre-column coupling, its inner face has screw thread, is connected with adjustable pre-column by screw thread; Outwards protrude first outside, spherical cylinder lower edge, forms 4 equally distributed ring flanges; Outwards protrude second outside, spherical cylinder upper edge, forms 4 ring flanges corresponding with the ring flange of first spherical column jecket; One diameter is arranged at its bottom is the 5mm opening, and the cylindrical outlet pipe that forms a long 10mm, internal diameter 5mm is outwards protruded in the opening outside; This outlet inner face has screw thread, and second spherical column jecket links to each other with the post tail with screw thread by this outlet 18;
Described post tail 15 comprises porous sieve plate, O-ring seal 6, screw thread, gathering sill and nut; The gathering sill, the O-ring seal that have post tail inner face to be recessed on the spiral shell tail reach the porous sieve plate that is complementary with the outlet internal diameter, and the post tail is assigned in the outlet lower end with nut and screw thread;
Concrete parameter is: a kind of adjustable pre-column internal diameter 12mm of spherical liquid chromatography preparative column, and column length 40mm, induction pipe internal diameter 15mm, spherical cylinder internal diameter is 120mm, outlet internal diameter 5mm.By shown in Figure 1, post top is column cap 1, down gathering sill 3, O-ring seal 6, distribution plate 4 and porous sieve plate is arranged, and links to each other with adjustable pre-column 7 with screw thread with nut 2; Adjustable pre-column 7 is assigned in induction pipe 8 by screw thread; Spherical cylinder 9 is made up of first spherical cylinder 10 and second spherical cylinder 14, and they link to each other with bolt 13 with flange 11, second O-ring seal 12; There is outlet 18 second spherical cylinder 11 bottoms, lower joint pin tail 15; Nut 2, gathering sill 3, O-ring seal 6 and sieve plate 5 are arranged under it, link to each other with outlet 18 with screw thread with nut 2.
Fill the C18 filler in the post, be granule filler 16 and bulky grain filler 17, with methyl alcohol: water=50: 50 be moving phase, and toluene and n-proplbenzene are sample, the detection of UV detecting device 260nm wavelength.Experimental result shows that this chromatographic column is simple to operate, and has very high post effect.
The above only is a preferred implementation of the present utility model; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the utility model design; can also make some improvements and modifications, these improvements and modifications also should be considered as in the protection domain of the present utility model.
Claims (8)
1. a spherical high performance liquid chromatography preparative column comprises column cap, adjustable pre-column, spherical cylinder and post tail; It is characterized in that column cap and post tail are assigned in the outlet of the upper end and the spherical cylinder lower end of adjustable pre-column respectively with nut and screw thread.
2. a kind of spherical high performance liquid chromatography preparative column as claimed in claim 1 is characterized in that described column cap comprises nut, screw thread, gathering sill, O-ring seal, distribution plate and porous sieve plate; Column cap is assigned in the upper end of adjustable pre-column with nut and screw thread, under the gathering sill that the column cap inner face is recessed into O-ring seal is arranged, distribution plate and the porous sieve plate that is complementary with adjustable pre-column internal diameter.
3. a kind of spherical high performance liquid chromatography preparative column as claimed in claim 1, it is characterized in that, described adjustable pre-column is cylindrical adjustable pre-column, its internal diameter r is less than spherical column diameter R, r=0.1R～0.2R, column length L=0.2R～0.3R, all there is screw thread adjustable pre-column upper/lower terminal outside, links to each other with cylinder with column cap respectively.
4. a kind of spherical high performance liquid chromatography preparative column as claimed in claim 1 is characterized in that, described spherical cylinder comprises induction pipe, first spherical cylinder, ring flange, second O-ring seal, bolt, second spherical cylinder and outlet; Ring flange and second the spherical cylinder that forms protruded in ring flange, second O-ring seal, bolt, second outside, spherical cylinder upper edge of having its outside, lower edge protrusion to form under first spherical cylinder; Upper and lower semisphere cylinder is with ring flange, bolt seal.
5. a kind of spherical high performance liquid chromatography preparative column as claimed in claim 4 is characterized in that the column diameter R=50～2000mm of described spherical cylinder.
6. a kind of spherical high performance liquid chromatography preparative column as claimed in claim 4 is characterized in that an import is opened at the top of described first spherical cylinder, and the post jamb outside is outwards protruded and formed a 20mm elongated cylindrical induction pipe; Induction pipe internal diameter and adjustable pre-column coupling, its inner face has screw thread, is connected with adjustable pre-column by screw thread; First outside, spherical cylinder lower edge post jamb outwards protrudes, and forms 4 equally distributed ring flanges.
7. a kind of spherical high performance liquid chromatography preparative column as claimed in claim 4 is characterized in that, described second outside, spherical cylinder upper edge post jamb outwards protrudes, and forms 4 ring flanges corresponding with the ring flange of first spherical cylinder; One diameter is arranged at its bottom is the opening of 5mm, and the cylindrical outlet pipe that forms a long 10mm, internal diameter 5mm is outwards protruded in the opening outside; This outlet inner face has screw thread, and second spherical column jecket links to each other with the post tail with screw thread by this outlet.
8. a kind of spherical high performance liquid chromatography preparative column as claimed in claim 1 is characterized in that described post tail comprises porous sieve plate, O-ring seal, screw thread, gathering sill and nut; The gathering sill, the O-ring seal that have post tail inner face to be recessed on the spiral shell tail reach the porous sieve plate that is complementary with the outlet internal diameter, and the post tail is assigned in the outlet lower end with nut and screw thread.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202099247U CN201522480U (en) | 2009-09-23 | 2009-09-23 | Spherical high-performance liquid chromatogram preparation column |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202099247U CN201522480U (en) | 2009-09-23 | 2009-09-23 | Spherical high-performance liquid chromatogram preparation column |
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| CN201522480U true CN201522480U (en) | 2010-07-07 |
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| CN2009202099247U Expired - Fee Related CN201522480U (en) | 2009-09-23 | 2009-09-23 | Spherical high-performance liquid chromatogram preparation column |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569232A (en) * | 2014-12-11 | 2015-04-29 | 首都师范大学 | High-performance liquid chromatographic ball |
| CN105327524A (en) * | 2014-08-08 | 2016-02-17 | 苏州汇通色谱分离纯化有限公司 | Smooth joint type medium-and-high pressure chromatographic column with two contracting ends |
-
2009
- 2009-09-23 CN CN2009202099247U patent/CN201522480U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105327524A (en) * | 2014-08-08 | 2016-02-17 | 苏州汇通色谱分离纯化有限公司 | Smooth joint type medium-and-high pressure chromatographic column with two contracting ends |
| CN105327524B (en) * | 2014-08-08 | 2017-10-17 | 苏州汇通色谱分离纯化有限公司 | A kind of two ends contraction type in smoothing junction is high, middle pressure chromatographic column |
| CN104569232A (en) * | 2014-12-11 | 2015-04-29 | 首都师范大学 | High-performance liquid chromatographic ball |
| CN104569232B (en) * | 2014-12-11 | 2017-01-18 | 首都师范大学 | High-performance liquid chromatographic ball |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100707 Termination date: 20150923 |
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| EXPY | Termination of patent right or utility model |