SU1402927A1 - Apparatus for centrifugal liquid chromatograpy - Google Patents

Abstract

The invention relates to the field of analytical instrumentation and can be used in the medical, biological, chemical and other industries in the analysis of substances by the method of liquid chromatography. The purpose of the invention is the possibility of analyzing the quantitative and qualitative composition of mixtures in the process of their separation. A device for centrifugal liquid chromatography includes a housing and a disk rotor mounted on the motor shaft. Several chromatographic columns are fixed on the rotor, at the output of which detector cells are installed, equipped with optical filters with different radiation transmission wavelengths. The eluent reservoir is located in the central part of the rotor, and the device for introducing samples into the column is made in the form of a channel in the rotor located perpendicular to the plane of its rotation and equipped with a rod with a calibrated transverse bore. One of the columns can be connected directly to the eluent tank. Optical filters can be mounted on a swivel disk connected to the rotor. A laser or a source causing the fluorescence of the analyzed substances can be used as a radiation source. 5 hp f-ly, 5 ill. with (L with go with Nd sl

Description

The invention relates to analytical instrumentation and can be used in medical, biological, chemical and other industrial fields in the analysis of mixtures of substances by liquid chromatography.

The purpose of the invention is to provide the possibility of analyzing quantitative: And qualitative composition; mixtures in the process of their separation.

I Fig. 1 shows a device, a cross section in Fig. 2, the same IB plan; Fig. 3 is a schematic diagram of a device with an additional rotating disc with filters: fit; 4 is a schematic diagram of the device using a laser as a measurement source; Fig. 5 shows the sample carrier of the sample introduction device into the chromatographic column.

The device contains a cylindrical body 1 with a removable lid 2. Inside the body 1 there is a centrifuge motor 3, on the shaft 4 of which a disk rotor is fixed; In the central part of the disk rotor 5, a reservoir 6 is installed for eluent, made removable or at the same time as the disk rotor S. In the disk rotor 5 several radial channels 7 were made, in which chromatographic columns 8 and cells 9 of the detector were installed sequentially from the axis to the periphery of the rotor. Each cell 9 is separated from the corresponding column 8 by means of a filter 10 of solid material, like a porous cermet-JCOPC material. Under the rotor 5, one or more radiation sources 11 are installed, the distance of which from the axis of rotation of the rotor 5 is equal to the distance from the center of cell 9 of the detector to the axis of rotation of the rotor 5. Radiation sources 11 are rigidly connected to device co-section 1. deuterium or mercury lamp can be used. On Kryshka 2 one or several radiation detectors 12 are installed with filters 13, with different wavelengths of radiation transmission bandwidths, filters 13 can be installed directly on cells 9 (by dashed lines). The radiation receivers 12 are located around the circumference.

the radius of which is equal to the distance from the center of the cell 9 of the detector to the axis of rotation of the rotor 5. The output of each cell is equipped with a bent tube 14 for draining the mobile phase (eluent) and the substances to be separated into the collection 15 of eluent, which is filled in the form of an annular tank, fitted in the upper part with a funnel-shaped annular receiver 16 of eluent, and in the lower part with a ring reservoir 17, Collection of eluent 15 is equipped with a device 18 for cooling it, made in the form of a tubular coil, covering the cylindrical outer surface of collection 15 o yuenta and having the channels 19 and 20 for inlet and outlet of refrigerant, e.g. tap water. The rotor 5 has an annular protrusion 21, which, together with the reservoir 6 for eluent, is led out through an annular central notch 22 in the lid 2 to the outside of the housing 1. Vertical protrusions 21 are provided with vertical channels 23 which are circumferentially oriented with respect to the rotation axis of the rotor 5 7, in which chromatographic columns 8 are installed. Vertical channels 23 serve to place sample carriers 24 in them. Each sample carrier 24 (see Fig. 5) is a metallic cylindrical rod 25, in which a calibrated transverse hole 26 is made, designed to fill the sample with the substance being analyzed. It also has a handle 27 with a marker, its position (not shown), and an ultrasound conical ring 28 made of Teflon, designed to seal the vertical channel 23 when the sample carrier 24 is installed in it. The distance between the calibrated cross hole 26 and the handle 27 of the sample carrier 24 is chosen such that when the sample carrier 24 is installed in a vertical channel 23, a calibrated cross opening 26, filled with the sample of the analyte, is set opposite the entrance to the column 8, This axis of the hole 26 and channel 7 are the same. The eluent tank 6 is provided with a lid 29 with a central opening 30. The device body 1 is provided with channels 31 and 32 for supplying and discharging an inert gas intended to purge the upper internal volume of the body 1 in the zone adjacent to the optical elements of the device. The outer surface of the rotor 5, the inner surfaces of the housing 1 and the cover 2, as well as the surfaces of the eluent collector 15, facing the optical elements of the device, are blackened. Columns 8, installed in the radial channels 7 of the rotor 5, are filled with the same or different sorbent. The device is equipped with a microcomputer 33 for processing the results of chromatographic analysis and connected to the radiation receiver 12.

FIG. 1, a dashed line shows an embodiment of the device in which the radiation sources 11 are mounted opposite the respective cells 9 and are rigidly connected to the rotor 5. The difference of this version of the device from that described above is that the cell 9 is constantly illuminated by a beam of light from the corresponding radiation source 11, and the radiation receivers 12 installed on the cover 2 periodically receive the radiation transmitted through the corresponding cells (at constant intervals). In this case, the light signals arriving at the receivers 12 are simulated with a frequency equal to the frequency of rotation of the rotor 5, i.e. the rotor 5 performs the functions of the obturator. This mode of operation provides a higher accuracy of measurements due to filtering most of the noise of the optical system.

FIG. 2, a dashed line shows an embodiment of the device, in which the source 11 and the radiation receiver 12 are mounted on the device cover 2 and placed ejaculated by centrifugal elements adjacent to one ok-.g.

rigor Such an arrangement of the source 11 and the radiation receiver 12 is most appropriate when implementing the fluorimetric detection principle. When cell 9 is suitable for rotating the rotor into a beam emitted by radiation source 11, in the case of cell 9 fluorescent substances (aromatic compounds, metabolites and other biologically important compounds), fluorescent radiation is excited in it, which is fixed at that moment ( after 0.01 s and less) receiver 12

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forces in the direction of the funnel receiver 16 eluent. At the same time, there is no special cell in the device for detecting the separation of substances. Its role is played by a stream of eluent ejected from the outlet of column 8 through the conical flow guide 38. When a stream of eluent crosses a narrow focused laser beam of radiation from a laser, the fluorescent substances in the eluent are awakened by the action of laser radiation and excitation) the long-term fluorescent radiation is sensed by the receiver.

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radiation, also mounted on the cover 2 of the device. A fluorimetric detection system can be used in the proposed device in conjunction with a photometric detection system.

A version of the device is also provided, according to which the source 11 and the radiation receiver 12 are fixed against each other and rigidly connected respectively to the housing 1 and the cover 2 (FIG. 3). Between them, a rotary disk 34 mounted on the axis 35 connected to the cover 2 is installed above the rotor 5. The disk 34 has windows 36 in which filters are installed around the disk 34 and having different radiation transmission wavelengths. The edges of the disk 34 have teeth that engage with the teeth of gear 37, which is rigidly connected to a 6-dp tank of gluten. Thanks to the use of a rotating disk 34 with filters, whose rotational speed differs from that of the rotor 5 and is synchronized with it rigidly, the substances of the sample are scanned, sequentially entering cell 9, at different radiation wavelengths, which ensures reliable identification of these substances.

Another embodiment of the proposed device (see Fig. 4) is characterized in that a laser is used as the radiation source 11, which, together with the radiation receiver 12, is mounted on the key 2 of the device. With this, the output end of each chromatographic column 8 is provided with a conical flow guide 38 with a capillary outlet opening, forming a flow eluent.

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forces in the direction of the funnel receiver 16 eluent. At the same time, there is no special cell in the device for detecting the substances to be separated. Its role is played by a stream of eluent ejected from the outlet of column 8 through a conical flow guide 38. When a stream of eluent crosses a narrow focused laser beam, the fluorescent substances in the eluent are excited by laser radiation and excitation), the long-term fluorescent radiation is sensed by the receiver.

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12 radiation at the next point in time, i.e. when a stream of eluent with a fluorescent substance excited in it crosses the optical axis of the radiation receiver 12.

In a preferred embodiment of the device, optical filters 13 having different proFormula wavelengths.

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1. A device for centrifugal liquid chromatography containing

the housing, the disk rotor mounted on the motor shaft in the housing, the eluent reservoir installed in the central part of the rotor, the radiation adjustment device, are not installed, and the Q input is installed for introducing samples into chromatography directly on the windows of the cells 9 (Fig. 1 , chesky column, compilation of brute, us-dashed lines). In this embodiment, installed in the housing, and a detector cell with a source and a radiation receiver, installed at the output

one source of radiation 11 is used,

mounted under the rotor 5 and rigidly connected to the device body 1, and one radiation receiver 12 mounted on the cover 2 of the body 1.

Samples of the same analyzed mixture are introduced to the input simultaneously of several chromatographic columns 8–20 with the help of corresponding carriers of 24 samples. The separated components of the sample in the eluent stream are successively exiting the columns 8 into the corresponding cells 9, equipped with optical filters 13 with different radiation transmission bands. In addition, each sample cocktail that comes from different columns 8 having the same separation properties (the same sorbent, the same permeability and efficiency, etc.) is detected at different wavelengths. Treated using a microcomputer 33 signals from the receiver

12 radiations coming to printer15

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plotter or display (not shown) and are recorded as several (by the number of separation 8) chromatograms corresponding to different wavelengths of absorption, i.e. multiwave detection of the separated components of the analyzed mixture is carried out. This provides a definition not only quantitatively, but also the qualitative composition of the mixture.

In all embodiments of the device in order to avoid condensation of solvent vapors on the optical elements of the detecting system (cell windows 9, filter surfaces 13, receiving windows of the radiation receiver 12 AND DR), cooling of the eluent 15 by the refrigerant supplied to the coil 18 through channel 19 is provided and purging the upper internal volume of the core- Jaus 1 with inert gas (nitrogen, air, etc.).

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Claims (5)

1. A device for centrifugal liquid chromatography containing housing, a disk rotor mounted on the motor shaft in the housing, an eluent reservoir mounted in the central part of the rotor, a device for introducing samples into the chromatographic column, a collection of solvent; housing, a disk rotor mounted on the motor shaft in the housing, an eluent reservoir mounted in the central part of the rotor, a device for introducing samples into the chromatographic column, a collection of solvent; mounted in the housing, and a detector cell with a radiation source and receiver installed at the exit chromatographic column, characterized in that, in order to enable analysis of the quantitative and qualitative composition of the mixtures in the process of their separation, it is equipped with several chromatographic columns mounted on the rotor, radially with respect to its axis of rotation, and several detector cells equipped with optical filters with different lengths radiation transmission waves, and the device for introducing samples is made in the form of a channel in the rotor located perpendicular to the plane of its rotation and provided with a rod with a calibrated transverse bore. 2. The device according to claim. 1, about t l and alone so that input one from the columns, 2g is directly connected to the reservoir for the solvent, and the inputs other columns are connected to an eluent reservoir through a sample inlet. 3 "Device according to claim 1, 40 and 40 - that the optical filters are mounted on a rotary disk connected through a transmission system to the rotor shaft and installed between the radiation receiver and the rotor 4. Device on PP. 1 to 3, characterized in that the outer surface of the rotor and the inner surfaces of the housing and the solid reservoir facing the radiation source and receiver are blackened. 5. A device according to claim 1, characterized in that a source is used as a radiation source, which causes the fluorescence of the analytes in the detector cell, the source and receiver of the excited fluorescence radiation being mounted around the rotor circumferentially. the radius of which is equal to the distance from the axis of rotation of the rotor to the detector cell, 6, the apparatus according to claim 5, characterized in that tTX 29 11 „V / a laser source was used for the radiation source, and an eluent jet former crossing the laser beam was installed at the exit of the chromatographic column. L № hro 3BN J2  2 f1 n gjuf.ff. W 29 srig.5