A rapid filtration and purification device for sample extraction fluid

Abstract

The patent application discloses a kind of sample extraction liquid rapid filtration purification device, specifically relates to the technical field of sample processing device.It includes sample centrifugal tube, purification pipe and conical barrel, the purification pipe is threadedly connected with sample centrifugal tube, the purification pipe adopts upper and lower opening design, the pipe opening at the bottom of the purification pipe is equipped with sieve plate, the purification pipe is sequentially filled with fine particle filler, medium particle filler and coarse particle filler from bottom to top, the pipe opening at the top of the purification pipe is equipped with purification ball, the conical barrel is connected on the purification pipe, the conical barrel is equipped with push liquid barrel, and the push liquid rod is slidably and sealingly connected in the push liquid barrel.The technical scheme of the present application solves the problem of complex operation of existing purification device, which leads to large deviation of test results, and can improve the purification efficiency of sample extraction liquid.

Description

Technical Field

[0001] This invention relates to the technical field of sample processing devices, and in particular to a rapid filtration and purification device for sample extracts. Background Technology

[0002] In the testing and detection of samples such as food, agricultural products, pharmaceuticals, environmental samples, clinical samples, and biological samples, the samples are mixed, crushed, and extracted to obtain the analytical solution present in the extract. The purification of the extract is achieved by reducing the coexisting matrix and enriching the analyte. The purification of the extract is a key step to improve the sensitivity and accuracy of detection.

[0003] Existing purification methods involve multiple steps, such as solid-liquid, liquid-liquid, solid extraction, solid dispersion, countercurrent separation, and turbulent separation, which have led to the development of related experimental devices, such as the commonly used solid-phase extraction device. This device can rapidly extract and purify samples to obtain sample test solutions that can be used for chromatographic or chromatographic-mass spectrometry detection. The steps are as follows: after the sample is pulverized and homogenized, inorganic salts and extraction solutions are added for extraction. After centrifugation, purification materials or solid-phase extraction are added to the supernatant to remove impurities. The solution obtained after centrifugation or concentration and reconstitution is the sample test solution. However, for complex matrix samples, existing purification methods require multiple operations to separate the analyte from the matrix. During these multiple operations, steps such as adsorption, transfer, and dilution lead to the loss of the analyte, resulting in uncertainty in the detection. Furthermore, many separation and purification processes involve matrix replacement and dilution to some extent. For residual detection, the low concentration can cause a decrease in the overall sensitivity of the method. Therefore, methods such as concentration and solid-phase enrichment can be used to further increase the concentration of the analyte. However, the uncertainty caused by repeated steps will inevitably lead to uncertainty in the detection results, resulting in significant deviations. Summary of the Invention

[0004] The present invention aims to provide a rapid filtration and purification device for sample extracts, which solves the problem that existing purification devices are complex to operate and lead to large deviations in test results.

[0005] To achieve the above objectives, the technical solution of the present invention is as follows: A rapid filtration and purification device for sample extract includes a sample centrifuge tube, a purification tube, and a conical barrel. The purification tube is threadedly connected to the sample centrifuge tube. The purification tube has an opening at both the top and bottom. A sieve plate is provided at the bottom opening of the purification tube. The purification tube is filled with fine particle packing, medium particle packing, and coarse particle packing in sequence from bottom to top. A purification ball is provided at the top opening of the purification tube. The conical barrel is connected to the purification tube. A liquid pushing barrel is provided inside the conical barrel. A liquid pushing rod is slidably and sealed inside the liquid pushing barrel.

[0006] Furthermore, the liquid-pushing bucket uses a disposable plastic cylindrical pipe.

[0007] Using the above setup, the liquid sample is pushed into the purification tube.

[0008] Furthermore, the upper part of the purification tube is cylindrical, and the lower part of the purification tube is conical.

[0009] By using the above setup and filling with purification materials of different particle sizes, the downstream liquid can achieve central aggregation without dispersion.

[0010] Furthermore, the purification ball is elliptical in shape and is made of porous ceramic, stainless steel, or nylon material. The purification ball contains PSA, activated carbon, alumina, or cellulose.

[0011] The above settings enable uniform dispersion of the liquid during sample loading and preliminary filtration.

[0012] Furthermore, the fine particle packing is a chromatographic packing with a particle size of 5-10 μm, the medium particle packing is a chromatographic packing with a particle size of 20-30 μm, and the coarse particle packing is a chromatographic packing with a particle size of 30-50 μm or a mesoporous fiber with a pore size of 2-5 μm.

[0013] The above setup enables rapid filtration of the sample liquid. The resulting slight damping, combined with the lower and middle packing bed, allows for horizontal correction of the arc-shaped liquid surface flowing down the purification ball, while simultaneously focusing the sample, reducing longitudinal liquid surface diffusion, and filtration and purification of the sample.

[0014] Furthermore, the sieve plate is a nylon or stainless steel sieve plate with an aperture between 0.45μm and 1.25μm.

[0015] Furthermore, the outlet cone at the lower part of the purification tube is 1 / 4 to 1 / 5 of the inner diameter of the upper part of the sample centrifuge tube.

[0016] The above settings prevent the leakage of fine particle packing.

[0017] Compared with existing technologies, the beneficial effects of this solution are:

[0018] This solution can be applied to the testing of food, agricultural products, pharmaceuticals, environmental samples, clinical samples, biological samples, etc. It is particularly suitable for the detection of hazardous substance residues. It is highly practical and can be combined with different extraction modes such as pulverization and homogenization or ultrasonic homogenization. It utilizes the combination of pulverization, homogenization, extraction and purification to achieve rapid extraction and purification of samples. Furthermore, it can achieve rapid processing of batch samples. The method is simple and economical. Attached Figure Description

[0019] Figure 1This is a schematic diagram of the structure of a rapid filtration and purification device for sample extract of the present invention. Detailed Implementation

[0020] The present invention will be further described in detail below through specific embodiments:

[0021] The reference numerals in the accompanying drawings of the instruction manual include: 1. Sample centrifuge tube; 2. Purification tube; 3. Purification ball; 4. Conical barrel; 5. Pushing barrel; 6. Pushing rod; 7. Coarse particle packing; 8. Medium particle packing; 9. Fine particle packing; 10. Sieve plate.

[0022] Example

[0023] As attached Figure 1 As shown, a rapid filtration and purification device for sample extract includes a sample centrifuge tube 1, a purification tube 2, and a conical barrel 4. The sample centrifuge tube 1 has a volume of 2-5 mL, and its opening is tapped with an internal thread. The outer wall of the purification tube 2 is tapped with an external thread that mates with the internal thread, and the purification tube 2 is threadedly connected to the sample centrifuge tube 1. The upper part of the purification tube 2 is cylindrical, and the lower part is conical. The purification tube 2 features an open-top and closed-bottom design. A sieve plate 10 is fitted at the bottom of the tube. The purification tube 2 is filled from bottom to top with fine-particle packing 9, medium-particle packing 8, and coarse-particle packing 7. The fine-particle packing 9 consists of chromatographic packing material with a particle size of 5-10 μm, the medium-particle packing 8 consists of chromatographic packing material with a particle size of 20-30 μm, and the coarse-particle packing 7 consists of chromatographic packing material with a particle size of 30-50 μm or mesoporous fibers with a pore size of 2-5 μm. The resulting downward flow damping of the liquid allows for the horizontal correction of the arc-shaped liquid surface flowing down the purification ball 3, ensuring a horizontal sample propulsion surface. The outlet sieve plate 10 of the purification tube 2 is made of nylon or stainless steel with a pore size between 0.45 μm and 1.25 μm. The outlet cone at the bottom of the purification tube 2 is 1 / 4 to 1 / 5 of the upper inner diameter of the sample centrifuge tube 1, effectively preventing leakage of the fine-particle packing 9.

[0024] A purification ball 3 is installed at the top of the purification tube 2. The purification ball 3 is elliptical and made of porous ceramic, stainless steel, or nylon. It contains PSA, activated carbon, alumina, cellulose, or other materials for removing impurities from the sample extract. A conical barrel 4 is connected to the purification tube 2. A liquid-pushing barrel 5 is installed inside the conical barrel 4, and a liquid-pushing rod 6 is slidably and sealed inside the liquid-pushing barrel 5. The conical barrel 4, liquid-pushing barrel 5, and liquid-pushing rod 6 serve as channels for adding the extract and solvent. The lower middle part of the conical barrel 4 has an inner groove for fixing and sealing the liquid-pushing barrel 5. The liquid-pushing rod 6 is mainly used for liquid propulsion. The liquid-pushing barrel 5 is a disposable plastic cylindrical pipe.

[0025] The purification method of the purification device is as follows: push the liquid into or not push it into the lower purification tube 2, add solvent, put the sealing cap on the upper part of the device, put the whole device into the centrifuge or push it in through the push rod 6, and perform purification filtration at a speed of 8000-12000 rpm in the centrifuge.

[0026] Application Example 1

[0027] In this application example, the purification device eliminates the conical barrel 4, the liquid-pushing barrel 5, and the liquid-pushing rod 6. Taking the detection of pyrethroid pesticide residues in tea as an example, after the sample is crushed, 2g of the sample is taken, and extracted with 10mL of water using ultrasound. Then, 5mL of acetonitrile, 2g of sodium chloride, and 0.5g of magnesium sulfate are added. After vortex centrifugation, the supernatant is taken for purification. The supernatant is placed in the conical barrel 4. The purification tube 2 is a purification ball 3 filled with activated carbon. The lower part of the purification tube 2 is made of 30μm and 5μm C18 packing material. After adding the solution, the purification tube 2 of this device is capped and placed in a centrifuge at 8000 rpm for 5 minutes. It can be seen that the upper solution is filtered into the centrifuge tube. After removing the centrifuge tube, liquid chromatography-mass analysis is performed. Using cypermethrin as an indicator, the concentration linear range is 0.2μg / kg-50μg / kg, and the recovery rate is greater than 85%.

[0028] Application Example 2

[0029] Taking the detection of vomitoxin in rice as an example, after crushing the sample, 2g of the sample was extracted with 5mL of water using ultrasound. Then, 5mL of acetonitrile, 1g of sodium chloride, and 0.5g of magnesium sulfate were added. After vortex centrifugation, the supernatant was purified and placed in the pusher 5 on the conical barrel 4. The purification tube 2 is a purification ball 3 filled with activated carbon. The lower part of the purification tube 2 is made of 30μm and 5μm C18 packing material. After adding the solution, the solution was pushed forward using the pusher rod. It can be seen that the upper solution is filtered into the centrifuge tube. After removing the centrifuge tube, liquid chromatography-mass spectrometry was used. Using vomitoxin as an indicator, the linear range of concentration was 0.05μg / kg-30μg / kg, and the recovery rate was greater than 90%.

[0030] The above are merely embodiments of the present invention, and common knowledge such as specific structures and / or characteristics in the solutions 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 structure 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 rapid filtration and purification device for sample extract, characterized in that: The device includes a sample centrifuge tube, a purification tube, and a conical barrel. The purification tube is threadedly connected to the sample centrifuge tube and has an open design at both ends. A sieve plate is provided at the bottom of the purification tube. The purification tube is filled with fine-particle packing, medium-particle packing, and coarse-particle packing in sequence from bottom to top. A purification ball is provided at the top of the purification tube. The conical barrel is connected to the purification tube and has a liquid-pushing barrel inside. A liquid-pushing rod is slidably and sealed inside the liquid-pushing barrel. The upper part of the purification tube is cylindrical, and the lower part of the purification tube is conical. The purification ball is elliptical and made of porous ceramic, stainless steel, or nylon material. The purification ball contains PSA, activated carbon, or alumina and cellulose. The fine particle packing is a chromatographic packing with a particle size of 5-10 μm, the medium particle packing is a chromatographic packing with a particle size of 20-30 μm, and the coarse particle packing is a chromatographic packing with a particle size of 30-50 μm or a mesoporous fiber with a pore size of 2-5 μm.

2. The rapid filtration and purification device for sample extract according to claim 1, characterized in that: The liquid-pushing tank uses a disposable plastic cylindrical pipe.

3. The rapid filtration and purification device for sample extract according to claim 1, characterized in that: The sieve plate is a nylon or stainless steel sieve plate with an aperture between 0.45μm and 1.25μm.

4. The rapid filtration and purification device for sample extract according to claim 1, characterized in that: The outlet cone at the bottom of the purification tube is 1 / 4 to 1 / 5 of the inner diameter of the upper part of the sample centrifuge tube.

Images