CN201522480U - A spherical high performance liquid chromatography preparative column - Google Patents

A spherical high performance liquid chromatography preparative column Download PDF

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Publication number
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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column
spherical
cylinder
adjustable pre
liquid chromatography
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CN2009202099247U
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万昊
刘翻
张维冰
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East China University of Science and Technology
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East China University of Science and Technology
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Abstract

本实用新型涉及一种球形高效液相色谱制备柱,包含柱头、可调预柱、球形柱体和柱尾;柱头和柱尾以螺帽和螺纹分别配于可调预柱的上端与球形柱体下端出口管;具体是:柱体内径R=50~2000mm,可调预柱内径r=0.1R~0.2R,柱长L=0.2R~0.3R,柱出口内径为5mm。本实用新型优点为:可调预柱与球形柱体连接可调,能简化色谱柱修补技术,延长柱使用寿命;球形柱体上半柱体形状能克服“柱壁效应”,有效提高柱效;下半球形柱体内径逐渐减小,对样品有一定量的富集效应,柱头与柱尾使用小直径筛板,可大幅度降低制备成本;而且该球形液相制备色谱柱装填简单,操作方便。

The utility model relates to a spherical high-performance liquid chromatography preparation column, which comprises a column head, an adjustable pre-column, a spherical column body and a column tail; The outlet pipe at the lower end of the body; specifically: the inner diameter of the column is R=50-2000mm, the inner diameter of the adjustable pre-column is r=0.1R-0.2R, the length of the column is L=0.2R-0.3R, and the inner diameter of the column outlet is 5mm. The utility model has the advantages of: the adjustable pre-column and the spherical cylinder can be connected and adjusted, which can simplify the repair technology of the chromatographic column and prolong the service life of the column; the shape of the upper half of the spherical cylinder can overcome the "column wall effect" and effectively improve the column efficiency. ;The inner diameter of the lower hemispherical column gradually decreases, which has a certain enrichment effect on the sample. The use of small-diameter sieve plates at the column head and column tail can greatly reduce the preparation cost; moreover, the spherical liquid phase preparation chromatographic column is easy to fill and easy to operate .

Description

A kind of spherical high performance liquid chromatography preparative column
[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.
Embodiment 1
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)

1.一种球形高效液相色谱制备柱,包含柱头、可调预柱、球形柱体和柱尾;其特征在于,柱头和柱尾分别以螺帽和螺纹配于可调预柱的上端和球形柱体下端的出口管。1. A spherical high-performance liquid chromatography preparative column comprises a column head, an adjustable pre-column, a spherical cylinder and a column tail; it is characterized in that the column head and the column tail are respectively arranged on the upper end and the adjustable pre-column with nuts and threads Outlet tube at the lower end of the spherical cylinder. 2.如权利要求1所述的一种球形高效液相色谱制备柱,其特征在于,所述的柱头包含螺帽、螺纹、导向槽、密封圈、分配盘和多孔筛板;柱头以螺帽和螺纹配于可调预柱的上端,柱头内面凹成的导向槽下有密封圈,分配盘及与可调预柱内径相匹配的多孔筛板。2. a kind of spherical high performance liquid chromatography preparative column as claimed in claim 1, is characterized in that, described stigma comprises nut, screw thread, guide groove, seal ring, distribution plate and porous sieve plate; stigma is with nut The screw thread is arranged on the upper end of the adjustable pre-column. There is a sealing ring, a distribution plate and a porous sieve plate matching the inner diameter of the adjustable pre-column. 3.如权利要求1所述的一种球形高效液相色谱制备柱,其特征在于,所述的可调预柱为圆柱形可调预柱,其内径r小于球形柱体直径R,r=0.1R~0.2R,柱长L=0.2R~0.3R,可调预柱上、下两端外面均有螺纹,分别与柱头和柱体相连。3. a kind of spherical HPLC preparative column as claimed in claim 1, is characterized in that, described adjustable pre-column is cylindrical adjustable pre-column, and its internal diameter r is less than spherical cylinder diameter R, and r= 0.1R~0.2R, column length L=0.2R~0.3R, the upper and lower ends of the adjustable pre-column are threaded, respectively connected with the column head and the column body. 4.如权利要求1所述的一种球形高效液相色谱制备柱,其特征在于,所述的球形柱体,包含进口管、上半球形柱体、法兰盘、第二密封圈、螺栓、下半球形柱体和出口管;上半球形柱体下有其下沿外面凸出形成的法兰盘、第二密封圈、螺栓、下半球形柱体上沿外面凸出形成的法兰盘和下半球形柱体;上、下半球形柱体以法兰盘、螺栓密封。4. A kind of spherical HPLC preparative column as claimed in claim 1, is characterized in that, described spherical cylinder comprises inlet pipe, upper hemispherical cylinder, flange plate, second sealing ring, bolt , lower hemispherical cylinder and outlet pipe; under the upper hemispherical cylinder, there is a flange formed by protruding from the lower edge of the upper hemispherical cylinder, a second sealing ring, bolts, and a flange formed by protruding from the upper edge of the lower hemispherical cylinder The plate and the lower hemispherical cylinder; the upper and lower hemispherical cylinders are sealed with flanges and bolts. 5.如权利要求4所述的一种球形高效液相色谱制备柱,其特征在于,所述的球形柱体的柱体直径R=50~2000mm。5. A spherical high performance liquid chromatography preparative column as claimed in claim 4, characterized in that, the column diameter R of the spherical column is 50-2000 mm. 6.如权利要求4所述的一种球形高效液相色谱制备柱,其特征在于,所述的上半球形柱体的顶部开一进口,柱壁外面向外凸出形成一20mm长圆柱形进口管;进口管内径与可调预柱匹配,其内面有螺纹,通过螺纹与可调预柱连接;上半球形柱体下沿外面柱壁向外凸出,形成4个均匀分布的法兰盘。6. A kind of spherical HPLC preparative column as claimed in claim 4, it is characterized in that, the top of described upper hemispherical cylinder has an inlet, and the outside of the column wall protrudes outwards to form a 20mm long cylindrical shape Inlet pipe; the inner diameter of the inlet pipe matches the adjustable pre-column, and the inner surface is threaded, and is connected with the adjustable pre-column through the thread; the upper hemispherical cylinder protrudes outward along the outer column wall to form four evenly distributed flanges plate. 7.如权利要求4所述的一种球形高效液相色谱制备柱,其特征在于,所述的下半球形柱体上沿外面柱壁向外凸出,形成与上半球形柱体的法兰盘对应的4个法兰盘;其底部有一直径为5mm的开口,开口外面向外凸出形成一长10mm、内径5mm的圆柱形出口管;该出口管内面有螺纹,下半球形柱管通过此出口管以螺纹与柱尾相连。7. a kind of spherical high performance liquid chromatography preparative column as claimed in claim 4, is characterized in that, on described lower hemispherical cylinder, protrudes outwards along the outer column wall, forms the method with upper hemispherical cylinder There are 4 flanges corresponding to the blue plate; there is an opening with a diameter of 5mm at the bottom, and the outside of the opening protrudes outward to form a cylindrical outlet pipe with a length of 10mm and an inner diameter of 5mm; the inner surface of the outlet pipe is threaded, and the lower hemispherical column pipe The outlet pipe is threaded to the end of the column through this outlet. 8.如权利要求1所述的一种球形高效液相色谱制备柱,其特征在于,所述的柱尾包含多孔筛板、密封圈、螺纹、导向槽和螺帽;螺尾上有柱尾内面凹成的导向槽、密封圈及与出口管内径相匹配的多孔筛板,柱尾以螺帽和螺纹配于出口管下端。8. A kind of spherical high-performance liquid chromatography preparative column as claimed in claim 1, is characterized in that, described column tail comprises porous sieve plate, sealing ring, screw thread, guide groove and nut; Column tail inner surface is arranged on screw tail A concave guide groove, a sealing ring and a porous sieve plate matching the inner diameter of the outlet pipe, and the end of the column is equipped with a nut and thread at the lower end of the outlet pipe.
CN2009202099247U 2009-09-23 2009-09-23 A spherical high performance liquid chromatography preparative column Expired - Fee Related CN201522480U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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

Cited By (4)

* Cited by examiner, † Cited by third party
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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