WO2011069289A1

WO2011069289A1 - Visible fluorescent chromatography column

Info

Publication number: WO2011069289A1
Application number: PCT/CN2009/075450
Authority: WO
Inventors: 周胜
Original assignee: 利穗科技(苏州)有限公司
Priority date: 2009-12-10
Filing date: 2009-12-10
Publication date: 2011-06-16

Abstract

A visible fluorescent chromatography column which comprises a column body and a connector disposed at the end of the column body is provided. The said column body is constructed from ultraviolet transmitting quartz glass, and fluorescent fillers or light emissive fillers are filled in the column body. The said column body has filter board at two ends which can prevent the said fluorescent fillers or light emissive fillers from leaking. The preset fluorescent fillers in the column body can get the visual identity without the instrumentation under the ultraviolet irradiation during the chromatography by using the ultraviolet transmitting quartz glass as the material of column body. It can be widely used in the rapid analysis or preparation for chemical synthesis products and natural products etc. It is rapid and convenient, which makes it possible to get observation and analysis of the separation process inside the column and study the result and the method of separation at the same time.

Description

Description of the book visible fluorescent chromatography column

Technical field

The invention relates to a separation device in the chemical and pharmaceutical fields, in particular to a chromatography column for chromatographic separation of chemical synthesis products, natural products and the like. Background technique

The column is mainly separated according to the degree of affinity of the substances to be separated (plant active ingredients, chemical intermediates, compounds, etc.) and the fillers (resin, silica gel, gel, etc.) contained in the column. Category or different ingredients, and get the effective composition or ingredients that are planned. Chromatography is an important refining method for the preparation of high-efficiency medicines, low-dose Chinese medicines, plant active ingredients, and chemical intermediates.

The current column structure of the column is generally made of glass tube or plexiglass tube. It is usually confirmed by the detection of the ultraviolet detector when it is necessary to confirm the separation, and the detector is expensive, which is not conducive to the laboratory and The promotion of factory enterprises. Summary of the invention

The technical problem to be solved by the present invention is to provide a visible fluorescent chromatography column which can clearly observe the chromatographic effect of the substance in the column under the irradiation of a common ultraviolet lamp to make a judgment.

The technical problem to be solved can be implemented by the following technical solutions.

A visible fluorescent chromatography column comprising a cylinder and a joint disposed at an end of the cylinder, the cylinder being It is composed of quartz glass which transmits ultraviolet spectrum, and the column body is filled with a fluorescent or luminescent filler, and both ends of the column are provided with a filter plate for preventing leakage of the fluorescent or luminescent filler.

Further, the joint is a luer joint.

In the present invention, the joint and the cylinder are connected in two ways: by compression or clamping.

The pressing manner is: one end of the upper joint protrudes from the middle hole of the upper pressing head, and the other end is stuck in the upper pressing head; one end of the lower joint protrudes from the middle hole of the lower pressing head The other end is fastened in the lower pressing head; the two pressing bolts respectively pass through the two side holes of the upper pressing head and are inserted into the corresponding two side holes of the lower pressing head, Inserting the two ends of the column into the middle hole of the upper pressing head and the lower pressing head respectively and abutting the upper and lower joints respectively, the cylinder is tightened by screwing the nut onto the two pressing bolts Fixed connection to the joint.

As a further improvement of the pressing method, the cylinder is formed by joining at least two sub-columns through an intermediate joint.

The clamping mode is: one end of the joint is provided with an external thread, the end of the column is inserted into a top tube for supporting the filter plate, one end of the top tube is inserted into the joint, and the column passes through A lock ring abuts the joint, and a clamping nut screwed to the external thread of the joint is sleeved on the cylinder, and the lock ring is locked by tightening the clamp nut to the joint.

Further, the lock ring is in the shape of a tapered top.

The visible fluorescent chromatography column involved in the invention is a novel chromatography column. The quartz glass which is transparent to the ultraviolet spectrum is used as a column, so that the fluorescent filler previously placed in the column space can be in the ultraviolet during the chromatography process. It can be used for rapid analysis or preparation of chemical synthesis products, natural products, etc. under the illumination of lamps. It can be used for rapid analysis and preparation. Study separation effects and methods. Visible fluorescence chromatography The column unit can be visually observed or automatically recorded by the camera system without the need for an expensive UV detection system, which greatly reduces the cost of chromatography. DRAWINGS

The specific embodiments of the present invention are described in detail below with reference to the accompanying drawings.

Figure 1 is a cross-sectional structural view showing a first embodiment of the present invention;

Figure 2 is a cross-sectional structural view showing a second embodiment of the present invention;

Figure 3 is a plan view of Figure 2;

Figure 4 is a plan view of Figure 1;

Figure 5 is an exploded structural view showing a first embodiment of the present invention;

Figure 6 is an exploded structural view showing a second embodiment of the present invention;

Figure 7 is an overall structural view of a first embodiment of the present invention;

Figure 8 is a view showing the entire configuration of a second embodiment of the present invention;

The label in the figure shows:

10, 11, 12, 13—fluorescent column 20, 21—intermediate connector

301, 302, 311, 312, 321, 322, 73, 74 - sieve plates 41, 43 - Luer female connector

42, 44-Ruhr male connector 51-upper head 52-lower head 61, 62-pressing bolt 70, 75-top tube 71, 76-locking ring 72, 77-clamping nut

Embodiment 1 : The visible fluorescence chromatography column of the first structure shown in FIG. 1, FIG. 4, FIG. 5, and FIG. 7 has the following main structures and components:

A visible fluorescent chromatography column comprising a cylinder and a joint disposed at an end of the cylinder, the cylinder being transparent The outer spectrum is composed of quartz glass, and the column is connected by at least two fluorescent columns through the intermediate connecting head; as shown in FIG. 1, the fluorescent columns 10, 11, 12 are connected through the intermediate connecting heads 20, 21 to form the entire column, and each The fluorescent column is filled with a fluorescent or luminescent filler, and both ends of the column are provided with filter plates for preventing leakage of fluorescent or luminescent filler. The filter plates in the first embodiment are sieve plates 301, 302, 311, 312, 321, and 322. They are respectively disposed at both ends of the fluorescent columns 10, 11, and 12. In this embodiment, the connection between the fluorescent cylinder and the joint is performed by pressing, as shown in FIG. 5, and the specific structure is as follows: One end of the upper joint (ie, the Luer female joint 41) protrudes from the middle hole of the upper pressing head 51, The other end of the Luer female connector 41 is fastened in the upper pressing head 51; one end of the lower joint (i.e., the Luer male connector 42) protrudes from the intermediate hole of the lower pressing head 52, and the other end of the Luer male connector 42 is clamped under the pressing In the head 52; two compression bolts 61, 62 are respectively passed through the two side holes of the upper pressing head 51 and inserted into the corresponding two side holes of the lower pressing head 52, and the two ends of the fluorescent cylinder are respectively inserted into The intermediate holes of the upper pressing head 51 and the lower pressing head 52 are respectively abutted against the upper and lower joints (ie, the Luer female joint 41 and the Luer male joint 42), and the nut is tightened to the two pressing bolts 61 and 62. The cylinder is fixedly connected to the joint.

The locking joints on the upper and lower ends of the cylinder can be LUER male/female joints, 1/4~28 thread or other universal joints.

The column connection of the chromatography column of the embodiment adopts a stackable design, and a plurality of fluorescent columns are connected into a monolithic column through an intermediate connector. The purpose of the design is to conveniently keep the separated substance in a short position. The inside of the column is easy to remove and separate again. Embodiment 2: The visible fluorescence chromatography column of the second structure shown in Fig. 2, Fig. 3, Fig. 6, and Fig. 8 has the following main structures and components:

A visible fluorescent chromatography column comprises a column and a joint disposed at an end of the column, the column is composed of quartz glass that transmits ultraviolet spectrum, and the fluorescent column 13 is filled with a fluorescent or luminescent filler, and the fluorescent column 13 The filter plate is provided at the end to prevent leakage of fluorescent or luminescent filler. The filter plates in the second embodiment are sieve plates 73 and 74, which are respectively disposed at both ends of the fluorescent column 13. In this embodiment, the connection between the fluorescent cylinder and the joint is in a clamping manner, as shown in FIG. 6. The specific structure is as follows: Since the upper and lower joints are connected to the fluorescent column in the same manner, the upper joint is mainly described as Luermu in this embodiment. The connection mode of the joint 43 and the fluorescent column 13 and the connection mode of the lower joint, that is, the Luer male connector 44 and the fluorescent column 13 can refer to the connection manner of the upper joint and the fluorescent column. The specific connection between the Luer female connector 43 and the fluorescent column 13 is as follows:

The 43-end end of the Luer female connector is provided with an external thread, the end of the fluorescent column 13 is inserted into a top tube 70 for supporting the sieve plate 73, and the top tube 70-end is inserted into the Luer female joint 43, and the fluorescent column 13 passes through A lock ring 71 abuts the Luer female connector 43. Since the top tube 70 is inserted into the Luer female connector 43, when the fluorescent column 13 abuts the Luer female connector 43, the top tube 70 is also connected to the Luer female connector 43. Abut, this can be seen very clearly from Figure 3. A clamping nut 72, which is screwed to the external thread of the Luer female connector 43, is sleeved on the fluorescent column 13, and the lock ring 71 is locked to the fluorescent column 13 by tightening the clamping nut 72 to the Luer female connector 43. The locking ring 71 is a tapered cone. The specific shape can be seen in FIG. 2. The clamping nut 72 is continuously tightened, so that the Luer female connector 43 is continuously moved forward along the cone of the locking ring 71, forcing the locking ring 71. The shaft is contracted so that the fluorescent column 13 sleeved in the lock ring 71 is tightly clamped. This patent adopts a column made of special UV-transparent quartz material and a unique joint design. The joint and the seal (ie the sieve plate) are separately separated, and the joint is connected to ensure that the column and the solvent transfer line can be safely connected; The piece ensures a reliable seal of the column; at the same time, the superimposed connection piece can ensure the safe superposition of the columns, and the whole system can withstand 7Bar pressure. The fluorescent filler can be filled in a tubular container, and the separation of the target sample in the tubular column can be clearly observed under the irradiation of the ultraviolet lamp. The substance having ultraviolet absorption can be directly observed.

The chromatography column device of the invention is irradiated by an ultraviolet lamp with a wavelength of about 254 nm. At the time of observation, a substance having ultraviolet absorption (black absorption band) can be observed; when irradiated with an ultraviolet lamp having a wavelength of about 365 nm, a fluorescent substance (special light band) can be observed when the sample is eluted. The column device can be observed in an intuitive form or recorded by a camera system. The design is unique and easy to operate. It is no longer necessary to use an expensive UV detection system for analysis and confirmation, which greatly reduces the performance. Product cost; and can be set to various specifications as needed, which is very suitable for quantitative analysis, small-volume preparation and process development.

At room temperature, alkali and salt are extremely corrosive to quartz glass. The column device is resistant to various organic solvents and can be used in all separations.

When using, the sample can be loaded by injection or solid injection, and the appropriate eluent can be selected after loading. It can be eluted manually by syringe syringe or pneumatic device or automatically by gradient pump. The separation process is in UV lamp ( It can be clearly observed at 254 nm or 365 nm wavelength.

A person skilled in the art should understand that the above-mentioned embodiments are merely exemplary, and are intended to enable those skilled in the art to understand the patent, and are not to be construed as limiting the scope of the patent, as long as it is according to the patent. Any equivalent changes or modifications made to reveal the spirit are within the scope of this patent.

Claims

Claim

A visible fluorescent chromatography column comprising a column and a joint disposed at an end of the column, wherein the column is composed of quartz glass that transmits ultraviolet spectrum, and the column is filled with a fluorescent or luminescent filler. The filter body is provided at both ends of the cylinder to prevent the fluorescent or luminescent filler from leaking.

2. A visible fluorescent chromatography column according to claim 1 wherein the linker is a luer connector.

3. A visible fluorescent chromatography column according to claim 1, wherein the joint is connected to the cylinder by compression.

The visible fluorescent chromatography column according to claim 3, wherein the pressing manner is: one end of the upper joint protrudes from a middle hole of the upper pressing head, and the other end is stuck at the In the upper pressing head; one end of the lower joint protrudes from the middle hole of the lower pressing head, and the other end is locked in the lower pressing head; two pressing bolts respectively from the two side holes of the upper pressing head Inserting and inserting into the corresponding two side holes of the lower pressing head, the two ends of the column are respectively inserted into the middle holes of the upper pressing head and the lower pressing head, and respectively respectively resist the upper and lower joints The post is fixedly coupled to the joint by tightening a nut onto the two compression bolts.

5. The visible fluorescent chromatography column according to claim 1, wherein the joint is connected to the cylinder by a clamping method.

The visible fluorescent chromatography column according to claim 5, wherein the clamping mode is: one end of the joint is provided with an external thread, and the end of the cylinder is inserted into a filter plate for inserting a top tube, one end of the top tube is inserted into the joint, the cylinder is abutted against the joint through a lock ring, and a clamping nut screwed to the external thread of the joint is sleeved on the cylinder , Lock the cylinder by tightening the clamping nut onto the fitting.

7. A visible fluorescent chromatography column according to claim 6, wherein the lock ring is a tapered cone.

The visible fluorescent chromatography column according to claim 4, wherein the column is formed by connecting at least two sub-columns through an intermediate connector.