Umbrella type high-speed centrifugal micro-column chromatography device

Abstract

The invention discloses an umbrella-type high-speed centrifugal micro-column chromatography device, which belongs to the technical field of sample analysis, and comprises a base, a motor is arranged in the base, a rotating main shaft is mounted at the upper part of the main shaft, the output end of the motor is butted with the rotating main shaft, and an umbrella-type centrifugal rotor assembly is assembled at the top of the rotating main shaft through a butt joint; the waste liquid disc is assembled in the middle of the rotating main shaft; the micro chromatographic column is assembled on the umbrella type centrifugal rotor assembly through a fixing buckle; according to the invention, the original centrifugal revolutions can be increased through the principle of gear change, so that the miniature chromatographic column connected to the centrifugal system performs umbrella-type centrifugal motion at a higher revolutions, complex sample separation under higher column efficiency is realized, elution substance analysis is performed by combining direct spectrum detection or embedding into other analysis systems, and the detection accuracy is improved. A direct sample injection mode can be provided for separation and purification of trace sample solutions in life science, biological detection and food and drug detection, and a more efficient mode is provided for more accurate separation and analysis.

Description

Technical Field

[0001] This invention relates to the field of sample analysis technology, and in particular to a microcolumn chromatography device with umbrella-type high-speed centrifugation. Background Technology

[0002] Sample analysis, especially the analysis of complex samples, is based on understanding the coexistence, interactions, and states of substances within the sample to deeply dissect complex sample systems and achieve a mechanistic understanding of the distribution of substances. Traditional chromatographic sample analysis typically utilizes the size, polarity, and acidity / alkalinity of substances in the sample for stepwise separation analysis to clarify the macroscopic and microscopic composition. Using linear separation models, common chromatographic mechanisms predict the separation model through the superposition of fine partitioning processes. The maturity of the model is then verified through simulation of actual samples. However, this approach relies on numerous assumptions, such as the equilibrium assumption of plate theory and the simple exponential summation of dynamic broadening. In reality, it superimposes many interferences and coherent interactions. During the chromatographic process, many states originally existing in the complex system are disrupted, failing to truly reflect the state of substances in a multiphase system. For example, mass transfer at phase interfaces cannot be explained by simple hypothetical models. Therefore, in-situ chromatography and rapid chromatography under physical influence have attracted attention in order to obtain the original state of existence or coexistence of substances, thereby achieving a true dissection of the material system. To address the aforementioned problems in accurate description, two issues need to be resolved: first, how to use faster physical mass transfer methods to quickly achieve dynamic equilibrium; and second, how to achieve the physical merging of multiphase substances in complex systems based on rapid equilibrium, thereby expressing the state of existence of substances within the complex system through simple substitution of complex phases. Summary of the Invention

[0003] The present invention aims to provide a microcolumn chromatography device for high-speed centrifugation using an umbrella-type centrifugation method to solve the problems mentioned in the background art.

[0004] To achieve the above objectives, the present invention provides the following technical solution:

[0005] A high-speed umbrella centrifugal microcolumn chromatography device includes a base, a rotating spindle, a waste liquid tray, a connector, an umbrella centrifugal rotor assembly, a fixing buckle, and a micro-chromatographic column;

[0006] A motor is installed inside the base, the rotating spindle is mounted on the upper part of the spindle, the output end of the motor is connected to the rotating spindle, the umbrella-type centrifugal rotor assembly is assembled on the top of the rotating spindle through a connector, the waste liquid tray is assembled in the middle of the rotating spindle, and the micro-chromatographic column is assembled on the umbrella-type centrifugal rotor assembly through a fixing buckle.

[0007] The connector is a collar-shaped ring with an internal toothed surface on the inside, and the top of the rotating spindle is an external toothed end. The connector is assembled onto the rotating spindle by meshing the internal toothed surface with the external toothed end.

[0008] The umbrella-shaped centrifugal rotor assembly includes an umbrella-shaped rotor liner and sleeves. The umbrella-shaped rotor liner is disposed on the outer side of the connector. The number of sleeves is several, arranged in a circumferential array on the umbrella-shaped rotor liner. The micro-chromatographic column is assembled onto the umbrella-shaped centrifugal rotor assembly through the sleeves. The umbrella-shaped rotor liner can open and close 30-80 degrees relative to the center line of the rotating main shaft.

[0009] Preferably, the micro-chromatographic column comprises a sample loading chamber, an upper fine particle sieve plate, a column body, a lower sieve plate, and an outlet. The top of the column body is connected to the bottom of the sample loading chamber, and the outlet is connected to the bottom of the column body. The upper fine particle sieve plate is disposed within the column body near the sample loading chamber, and the lower sieve plate is disposed within the column body near the outlet. The main body is filled with conventional packing material between the upper fine particle sieve plate and the lower sieve plate, and fine particle packing material is filled below the lower sieve plate and inside the outlet. The particle size of the fine particle packing material is smaller than that of the conventional packing material.

[0010] Compared with the prior art, the present invention has the following beneficial effects:

[0011] This invention can be implemented in various microcolumn packing modes and sizes, and can be embedded in analytical detection devices. With its higher extraction and separation efficiency, it can provide a direct injection method for the separation and purification of trace sample solutions in life sciences, biological detection, and food and drug detection, and provide a more efficient way for more accurate separation and analysis. Attached Figure Description

[0012] Figure 1 A schematic diagram of the main structure of a microcolumn chromatography device for high-speed centrifugation using an umbrella-type centrifugation method;

[0013] Figure 2 This is a partial structural schematic diagram of a microcolumn chromatography device for high-speed centrifugation using an umbrella-type centrifuge.

[0014] Figure 3 This is a schematic diagram of the structure of a micro-column in a high-speed umbrella centrifugal microcolumn chromatography device.

[0015] The reference numerals in the accompanying drawings include:

[0016] 1. Base; 101. Motor; 2. Rotating spindle; 201. External tooth end; 3. Waste liquid tray; 4. Connector; 401. Internal tooth surface; 5. Umbrella-type centrifugal rotor assembly; 501. Umbrella-type rotor liner; 502. Sleeve position; 6. Fixing buckle; 7. Miniature chromatographic column; 701. Sample loading chamber; 702. Upper fine particle sieve plate; 703. Column body; 704. Lower sieve plate; 705. Outlet. Detailed Implementation

[0017] The present invention will now be described in further detail with reference to the accompanying drawings and embodiments:

[0018] This invention utilizes the principle of gear transmission to increase the original centrifugal speed, enabling the micro-chromatographic column connected to the centrifugal system to undergo umbrella-shaped centrifugation at a higher speed. This achieves the separation of complex samples at a higher column efficiency. Combined with direct spectral detection or embedding in other analytical systems, it provides a direct injection method for the separation and purification of trace sample solutions in life sciences, biological detection, and food and drug testing, offering a more efficient approach for more precise separation and analysis.

[0019] In order to achieve the above objective, such as Figure 1-3 The umbrella-type high-speed centrifugal microcolumn chromatography device shown includes a base 1, a rotating spindle 2, a waste liquid tray 3, a connector 4, an umbrella-type centrifugal rotor assembly 5, a fixing buckle 6, and a micro-chromatographic column 7.

[0020] A motor 101 is installed inside the base 1. The rotating spindle 2 is installed on the upper part of the spindle. The output end of the motor 101 is connected to the rotating spindle 2. The umbrella centrifugal rotor assembly 5 is assembled on the top of the rotating spindle 2 through the connector 4. The waste liquid tray 3 is assembled in the middle of the rotating spindle 2. The micro chromatography column 7 is assembled on the umbrella centrifugal rotor assembly 5 through the fixing buckle 6.

[0021] The coupling 4 is a collar-shaped ring with an inner toothed surface 401 on the inside and an outer toothed end 201 on the top of the rotating spindle 2. The coupling 4 is assembled onto the rotating spindle 2 by meshing the inner toothed surface 401 with the outer toothed end 201.

[0022] The umbrella-type centrifugal rotor assembly 5 includes an umbrella-type rotor liner 501 and a sleeve 502. The umbrella-type rotor liner 501 is disposed on the outer side of the connector 4. There are several sleeves 502 arranged in a circumferential array on the umbrella-type rotor liner 501. The micro-chromatographic column 7 is assembled on the umbrella-type centrifugal rotor assembly 5 through the sleeves 502. The umbrella-type rotor liner 501 can open and close 30-80 degrees relative to the centerline of the main shaft 2.

[0023] The micro-chromatographic column 7 consists of a sample loading chamber 701, an upper fine particle sieve plate 702, a column body 703, a lower sieve plate 704, and an outlet 705. The top of the column body 703 is connected to the bottom of the sample loading chamber 701, and the outlet 705 is connected to the bottom of the column body 703. The upper fine particle sieve plate 702 is located inside the column body 703 near the sample loading chamber 701, and the lower sieve plate 704 is located inside the column body 703 near the outlet 705. The main body is filled with conventional packing material between the upper fine particle sieve plate 702 and the lower sieve plate 704. The area below the lower sieve plate 704 and inside the outlet 705 is filled with fine particle packing material, the particle size of which is smaller than that of conventional packing material.

[0024] In actual operation, the micro-column 7 is approximately the size of a blood collection capillary tube and is filled with 1.7-5μm chromatographic packing material, which serves as a sieve plate to remove fine particles and prevent packing material loss. It consists of packing material with a smaller particle size than the main chromatographic packing material. In actual loading, the corresponding packing material is suspended and the suspension is added to the sample loading chamber 701 of the empty column on the rotor. The motor 101 is turned on to centrifuge and rotate at a low speed followed by a high speed to load the chromatographic column. After the required column length 703 is reached, it is moistened with a small amount of chromatographic solvent for later use. During the separation operation, the sample solution is added to the sample loading chamber 701, followed by the addition of elution buffer for elution. After the overall separation, the micro-column can be removed and embedded in the mass spectrometry tubing for further analysis.

[0025] The specific implementation process is as follows:

[0026] Example 1:

[0027] The principle device uses C18 3.5μm packing material, with a column length of 5cm, an inner diameter of 1mm, and an outlet diameter of 0.1mm. The upper and lower sieve plates are filled with 1.7μm packing material. The sample loading chamber can hold a maximum of 0.2mL. During empty column packing, the column is filled by suspending the packing material in methanol using a motor speed of 8000-17000 rpm. A 0.05% melatonin methanol solution is used as the sample, and a methanol:water (70:20) mobile phase is used. 0.1mL of sample is loaded, and after the sample enters the column, 0.15mL of mobile phase is added to the sample loading chamber to test the rotation speed and perform sample separation. For separation efficiency testing, the column is inserted into the mass spectrometry flow pump system at a set time, with methanol solution used for propulsion. The separation time is calculated by subtracting the dead time from the melatonin detection result.

[0028] Example 2:

[0029] The application device operates on a similar principle. The column is packed with C18 3.5μm packing material, with a column length of 5cm, an inner diameter of 1mm, an outlet diameter of 0.1mm, and upper and lower sieve plates with 1.7μm packing material. The sample loading chamber can hold a maximum of 0.2mL. When filling an empty column, the rotation speed is 8000-17000 rpm, using methanol to suspend the packing material. The sample is a 0.05% gardenia methanol solution, and the mobile phase is methanol:water (70:20). 0.1mL of sample is loaded, and after the sample enters the column, 0.15mL of mobile phase is added to the loading chamber to test the rotation speed and perform sample separation. For separation efficiency testing, the column is embedded in the mass spectrometry flow pump system at specific intervals, propelled by methanol solution. The elution time of geniposide is recorded, and the time is adjusted by subtracting the dead time.

[0030] The above descriptions are merely embodiments of the present invention, and common knowledge such as specific technical solutions and / or characteristics are not described in detail here. It should be noted that those skilled in the art can make various modifications and improvements without departing from the technical solutions of the present invention, and these should also be considered within the scope of protection of the present invention. These modifications and improvements will not affect the effectiveness of the implementation of the present invention or the practicality of the patent. The scope of protection claimed in this application should be determined by the content of its claims, and the specific embodiments described in the specification can be used to interpret the content of the claims.

Claims

1. A microcolumn chromatography device with umbrella-type high-speed centrifugation, characterized in that: The device includes a base (1), a rotating spindle (2), a waste liquid tray (3), a connector (4), an umbrella-type centrifugal rotor assembly (5), a fixing buckle (6), and a micro-chromatographic column (7); The base (1) is equipped with a motor (101), the rotating spindle (2) is installed on the upper part of the spindle, the output end of the motor (101) is connected to the rotating spindle (2), the umbrella centrifugal rotor assembly (5) is assembled on the top of the rotating spindle (2) through the connector (4), the waste liquid tray (3) is assembled in the middle of the rotating spindle (2), and the micro chromatography column (7) is assembled on the umbrella centrifugal rotor assembly (5) through the fixing buckle (6); The connector (4) is a collar-shaped ring with an inner toothed surface (401) on the inside. The top of the rotating spindle (2) is an outer toothed end (201). The connector (4) is fitted onto the rotating spindle (2) by meshing with the outer toothed end (201) through the inner toothed surface (401). The umbrella-type centrifugal rotor assembly (5) includes an umbrella-type rotor liner (501) and a sleeve (502). The umbrella-type rotor liner (501) is disposed on the outer side of the connector (4). The sleeve (502) is a plurality of sleeves arranged in a circumferential array on the umbrella-type rotor liner (501). The micro-chromatographic column (7) is assembled on the umbrella-type centrifugal rotor assembly (5) through the sleeve (502). The umbrella-type rotor liner (501) can open and close 30-80 degrees relative to the centerline of the rotating main shaft (2).

2. The umbrella-type high-speed centrifugal microcolumn chromatography apparatus according to claim 1, characterized in that: The micro-chromatographic column (7) consists of a loading chamber (701), an upper fine particle sieve plate (702), a column body (703), a lower sieve plate (704), and an outlet (705). The top of the column body (703) is connected to the bottom of the loading chamber (701), and the outlet (705) is connected to the bottom of the column body (703). The upper fine particle sieve plate (702) is located inside the column body (703) near the loading chamber (701), and the lower sieve plate (704) is located inside the column body (703) near the outlet (705). The main body is filled with conventional packing material between the upper fine particle sieve plate (702) and the lower sieve plate (704). The area below the lower sieve plate (704) and inside the outlet (705) is filled with fine particle packing material, and the particle size of the fine particle packing material is smaller than that of the conventional packing material.

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