CN210448175U - Push rod type filtering purification column - Google Patents
Push rod type filtering purification column Download PDFInfo
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- CN210448175U CN210448175U CN201920261816.8U CN201920261816U CN210448175U CN 210448175 U CN210448175 U CN 210448175U CN 201920261816 U CN201920261816 U CN 201920261816U CN 210448175 U CN210448175 U CN 210448175U
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Abstract
The application discloses type purification column is filtered to push-down includes: the device comprises a piston, a cylindrical pipe and a filtering material layer, wherein a cavity is arranged in a first end of the cylindrical pipe, and a liquid outlet is arranged in a second end of the cylindrical pipe; the piston is accommodated and slides in the cavity along the column body pipe; a filter material layer is arranged in the second end of the cylindrical pipe; the furthest end of the piston sliding stroke is the end face of the filter material layer. The purifying column can realize direct sample loading without using a solid phase extraction device.
Description
Technical Field
The application relates to a push-rod filtering type purification column, belonging to the field of solid-phase extraction and purification.
Background
With the rapid development of economy, the material life of people is continuously improved, the types of foods related in daily life are greatly enriched, and higher requirements are provided for the quality safety detection of the foods. The traditional filtering type purifying column comprises a purifying column hollow pipe and two porous sieve plates, wherein the two porous sieve plates are placed in the purifying column hollow pipe, and a purifying filler is placed between the two porous sieve plates. At present, the process of analyzing and detecting drug residues in foods such as vegetables and aquatic products is generally divided into three steps.
Firstly, extracting a target analyte from food to obtain an extracting solution;
secondly, purifying by using a purification column, and removing impurities by adopting a physical adsorption mode of a purification filler;
and finally, adopting nitrogen (air) blowing or rotary evaporation for concentration, and rotating a proper redissolution for redissolution to obtain a solution which can be detected on a machine.
During purification, the filtration type purification column is connected with the solid phase extraction device, and the extract to be purified is transferred into the filtration type purification column. Under the vacuum pumping action of the solid phase extraction device, the purified extracting solution flows out to realize purification.
The operation process is complicated, the purification process can be completed only by relying on the solid-phase extraction device, the efficiency is low, and the purification cost is high.
SUMMERY OF THE UTILITY MODEL
According to one aspect of the present application, a push-rod filtration-type purification column is provided that allows for direct loading without the use of a solid phase extraction device.
The push-rod filtering type purification column is characterized by comprising: the device comprises a piston, a cylindrical pipe and a filtering material layer, wherein a cavity is arranged in a first end of the cylindrical pipe, and a liquid outlet is arranged in a second end of the cylindrical pipe; the piston is accommodated and slides in the cavity along the cylindrical barrel;
the second end of the cylindrical pipe is internally provided with the filter material layer;
the farthest end of the sliding stroke of the piston is the end surface of the filter material layer.
Optionally, the periphery of the filter material layer is fixedly connected with the inner wall of the trunk tube.
Optionally, the filtering material layer includes at least one pair of porous sieve plates and a purifying filler, the pair of porous sieve plates are arranged at intervals, and the purifying filler is filled between the porous sieve plates.
Optionally, the push-rod filter type purification column comprises a push rod, and one end of the push rod is provided with the piston.
Optionally, the push-rod filtration-type purification column comprises an upper cover, and the upper cover is mounted on the other end of the push rod.
Optionally, the side wall of the cavity of the shaft tube is provided with a pressure discharge hole and a sample injection hole at intervals.
Optionally, the pressure discharge holes are round or square; the sampling hole is round or square.
Optionally, the purification packing is C18, PSA, or N-propyl ethylenediamine bonded solid phase adsorbent.
Optionally, the liquid outflow port is in communication with a collection bottle.
The beneficial effects that this application can produce include:
1) the push-rod filtering type purifying column provided by the application has the advantages of simple structure, convenience in use and lower manufacturing and using cost. The sample extracting solution to be purified can be moved into the purifying column through the sample adding hole, and the extracting solution can be purified only by pushing the piston.
Drawings
Fig. 1 is a schematic front cross-sectional view of a push-rod filtration type purification column according to an embodiment of the present disclosure.
List of parts and reference numerals:
| name of component | Reference numerals | Name of component | Reference numerals |
| 1 | |
6 | Piston |
| 2 | |
71 | First perforated |
| 3 | |
72 | Second perforated screen plate |
| 4 | |
8 | |
| 5 | |
9 | Collecting bottle |
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Referring to fig. 1, the present application provides a push-rod 2-type filtration purification column, comprising: push rod 2, piston 6, shaft pipe 5, filtering material layer. One end of the push rod 2 is provided with a piston 6, and the piston 6 is accommodated in the cylindrical tube 5 and slides along the inner wall of the cylindrical tube 5. The first end of the cylindrical tube 5 is open, and the second end is provided with a liquid outflow port. A layer of filter material is provided within the second end of the shaft tube 5.
When the device is used, after liquid to be purified is added into the cavity in the column tube 5, the piston 6 extends into the cavity from the open end of the column tube 5, the liquid to be purified is extruded, and the liquid to be purified flows out from the outlet of the second end of the column tube 5 after passing through the filter material layer under the action of pressure. The pressure of the liquid to be purified is manually adjusted by adopting the piston 6, so that the liquid can be quickly, simply and conveniently purified. The device cost is reduced, a solid phase extraction device is not used, and the purification efficiency is improved.
Optionally, the periphery of the filter material layer is fixedly connected with the inner wall of the shaft tube 5.
Optionally, the filtering material layer comprises at least one pair of porous sieve plates and the purifying filler 8, the porous sieve plates are arranged at intervals, and the purifying filler 8 is filled between the porous sieve plates arranged in pairs.
Optionally, the cavity side wall of the shaft tube 5 is provided with a pressure discharge hole 3 and a sample injection hole 4 at intervals, and the pressure discharge hole 3 is used for connecting the inside and the outside of the cavity to adjust pressure. The sample inlet 4 is used for adding the liquid to be purified, and the material can be added without pulling out the piston 6.
Optionally, the other end of the push rod 2 is provided with an upper cover 1. Through installing upper cover 1, be convenient for the user when using treat that the purification liquid carries out pressurization treatment.
Alternatively, the pressure discharge hole 3 and the sampling hole 4 may be holes having various shapes such as a circle or a square.
Alternatively, the purification packing 8 may be various types of commonly used materials, such as C18, PSA, and the like. Preferably N-propyl ethylenediamine bonded solid phase adsorbent with particle size of 40-63 μm and specific pore diameter
Example push rod filtration type purification column
Referring to fig. 1, the push-rod filtration type purification cartridge of the present embodiment includes: the device comprises an upper cover 1, a push rod 2, a pressure discharge hole 3, a sample inlet hole 4, a column body pipe 5, a piston 6, a first porous sieve plate 71, a purifying filler 8, a second porous sieve plate 72 and a collecting bottle 9. The top of shaft pipe 5 is equipped with upper cover 1, and the one end of push rod 2 is worn to establish in upper cover 1, and piston 6 is connected to the other end of push rod 1, and piston 6 slides and sets up in 5 cavities of shaft pipe, and the inner wall laminating setting of piston 6 and shaft pipe 5.
The inside bottom of shaft pipe 5 is equipped with first porous sieve 71, purifies packing 8 and second porous sieve 72, purifies packing 8 up end and lower terminal surface and is equipped with first porous sieve 71 and second porous sieve 72 respectively. The first porous sieve plate 71 is positioned below the piston 6, the isolating porous sieve plate 7 is fixedly connected on the inner wall of the column tube 5, and the cavity side wall above the purifying filler 8 is provided with a pressure discharge hole 3 and a sample inlet hole 4. A collecting bottle 9 is arranged at the liquid outlet at the bottom end of the cylindrical tube 5. The pressure discharge hole and the sample inlet hole are circular.
The working principle is as follows: outwards stimulate piston 6 to the pressure vent 3 tops, will wait to purify the sample through advancing in the hole 4 moves into shaft pipe 5 through the liquid-transfering gun, promote piston 6 with the sample extract extrusion through purifying packing 8 and realize that the absorption of interference material with getting rid of, the extract after the purification flows into receiving flask 9 from the liquid outlet under the continuous promotion of piston 6.
Examples of the applications
The push-rod filtration type purification column provided in the above embodiment of the present application is used for detecting ethyl 3-aminobenzoate in different aquatic products, and comprises:
1. material method
1.1 instruments
20At high performance liquid chromatography (Shimadzu), 8060 triple quadrupole mass spectrometer (Shimadzu), and the like.
1.2 reagents
Acetonitrile (chromatographically pure, from merck, germany), sodium chloride and anhydrous magnesium sulfate (analytically pure, from beijing chemical plant), PSA (40-63 μm,
purchased from Shanghai' an spectral laboratory science and technology Co., Ltd.), and ethyl 3-aminobenzoate (imported, pure)>98%), ethyl 3-aminobenzoate standard solution in methanol.
1.3 solid phase extraction column conditions
a) The push-rod filtration type purification column provided in the above embodiment: the cavity is 2.5mL in specification;
b) solid-phase extraction purification filler: n-propyl ethylenediamine bonded solid phase adsorbent (particle diameter of 40-63 μm, pore diameter is specifically
Purchased from Shanghai' an spectral laboratory science and technology Co., Ltd.), 100 mg.
1.4 chromatographic conditions
a) A chromatographic column: kromasil C18Reverse phase chromatography column ((2.1 mm. times.50 mm,3.5 μm);
b) mobile phase and gradient elution conditions:
at the end of 0-1.5min, the volume percentage of the mobile phase 0.1% formic acid aqueous solution is from 60% to 10%, and the volume percentage of the mobile phase 0.1% formic acid methanol solution is from 40% to 90%;
at the end of-2.0 min from 1.51min, the volume percentage of the mobile phase 0.1% formic acid aqueous solution is 10%, and the volume percentage of the mobile phase 0.1% formic acid methanol solution is 90%;
at the end of-2.01 min from 2.01min, the volume percentage of the mobile phase 0.1% formic acid aqueous solution is from 10% to 60%, and the volume percentage of the mobile phase 0.1% formic acid methanol solution is from 90% to 40%;
at the end of-3.51 min from 2.02min, the volume percentage of the mobile phase 0.1% formic acid aqueous solution is 60%, and the volume percentage of the mobile phase 0.1% formic acid methanol solution is 40%;
the mobile phase is 0.1% of formic acid water, and 0.1% of the mobile phase represents the mass percentage concentration of formic acid in the formic acid water solution;
in the 0.1% formic acid methanol solution, 0.1% represents the mass percentage concentration of formic acid in the formic acid methanol solution;
c) sample introduction amount: 5 mu L of the solution;
d) column temperature: 40 ℃;
e) flow rate of mobile phase: 0.3 mL/min.
1.4 Mass Spectrometry conditions
The ionization mode is ESI ionization; the parameters of the multiple reaction monitoring mode are shown in table 1; atomizing gas pressure: 2.0 mL/min; pressure of drying gas: 10 mL/min; heating air pressure: 10 mL/min; temperature of the heating block: 400 ℃; the temperature of the curved desolventizing tube is 250 ℃.
1.5 sample pretreatment
Dissecting and homogenizing the fish body to obtain a minced fillet sample, and storing at low temperature in a refrigerator at-20 ℃; weighing 2.0g of minced fillet sample, melting at room temperature, adding 100 mu L of isotope labeled internal standard 3-ethyl aminobenzoate-D into a 50mL centrifugal test tube with a cover5The solution (0.2mg/mL) was thoroughly soaked at room temperatureWarming for 2 min;
adding 10mL of mixed solution (volume ratio is 7: 3) of acetonitrile and sodium acetate buffer solution (pH4.0), extracting, and performing vortex oscillation at 500rpm for 5 min; adding 3g of anhydrous magnesium sulfate and 1g of sodium chloride, performing vortex oscillation at 500rpm for 1min, and performing ultrasonic extraction (200W) for 10 min; freezing at-20 deg.C for 30min, and centrifuging at 10000rpm for 10 min; pulling the piston 6 outwards to the upper surface of the pressure discharge hole 3, moving 1mL of sample extracting solution to be purified into the trunk tube 5 through the sample inlet 4 by a pipette, pushing the piston 6 to realize the adsorption and removal of interfering substances by the sample extracting solution through the purification filler 8, enabling the purified extracting solution to flow into the collection bottle 9 through the liquid outlet under the continuous pushing of the piston 6, blowing nitrogen to dry, redissolving 1mL of mobile phase (methanol: water is 1: 1V/V, and contains 0.1% formic acid), filtering through a 0.22 mu m organic phase filter membrane, and performing HPLC-MS analysis.
2. Results and analysis
2.1 Retention time determination
The method adopts acetonitrile as an extraction solvent and a constant volume solvent, and adopts ethyl 3-aminobenzoate and ethyl 3-aminobenzoate-D5The sample was placed in an autosampler, and 5. mu.L of the sample was injected into HPLC-MS for measurement.
TABLE 1.3 Ethyl aminobenzoate and its isotopic label ethyl 3-aminobenzoate-D5Information and multi-reaction monitoring mode parameters
2.2 determination of reproducibility of ethyl 3-aminobenzoate in aquatic products
And adding ethyl 3-aminobenzoate into the aquatic product by adopting a standard addition method, and repeatedly measuring according to the conditions to investigate the reproducibility. Specific results are shown in table 2:
TABLE 2 measurement results of different concentrations of additives in different aquatic products
As can be seen from Table 2, after the purifying column provided by the application is adopted to treat a sample, the recovery rate of the standard addition determination result of the ethyl 3-aminobenzoate in the aquatic product is good, and the reproducibility is good. The purifying column has no influence on the detection result and can be applied to actual detection.
Vortex mixing and centrifugal separation can all be once only accomplished through adopting the device to realize manual operation, and have simple structure, set up reasonable, cost of manufacture low grade advantage.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (7)
1. A push-rod filtration-type purification column, comprising: the device comprises a piston, a cylindrical pipe and a filtering material layer, wherein a cavity is arranged in a first end of the cylindrical pipe, and a liquid outlet is arranged in a second end of the cylindrical pipe; the piston is accommodated and slides in the cavity along the cylindrical barrel;
the side wall of the cavity of the cylindrical pipe is provided with a pressure discharge hole and a sample inlet hole;
the second end of the column body pipe is internally provided with the filter material layer, and the periphery of the filter material layer is fixedly connected with the inner side wall of the column body;
the farthest end of the sliding stroke of the piston is the end surface of the filter material layer.
2. The rod pass filter purification column of claim 1, wherein the layer of filter material comprises at least one pair of porous sieve plates and purification packing, the pair of porous sieve plates being spaced apart and the purification packing being filled between the porous sieve plates.
3. The push-rod filtration purification column of claim 1, comprising a push rod, wherein the piston is disposed at one end of the push rod.
4. The push-rod filtration purification column of claim 3, comprising an upper cover mounted on the other end of the push rod.
5. The push-rod filtration purification column of claim 1, wherein the pressure vent is circular or square; the sampling hole is round or square.
6. The push-rod filtration purification column of claim 2, wherein the purification packing is C18, PSA, or N-propyl ethylenediamine bonded solid phase adsorbent.
7. The push-rod filtration purification column of claim 1, wherein the liquid flow outlet is in communication with a collection vial.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920261816.8U CN210448175U (en) | 2019-03-01 | 2019-03-01 | Push rod type filtering purification column |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920261816.8U CN210448175U (en) | 2019-03-01 | 2019-03-01 | Push rod type filtering purification column |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111751195A (en) * | 2020-06-29 | 2020-10-09 | 中国水产科学研究院 | Multi-channel automatic purification device |
| CN111855366A (en) * | 2020-06-29 | 2020-10-30 | 中国水产科学研究院 | Automatic filtering type purification device for sample pretreatment |
| CN111888796A (en) * | 2020-07-17 | 2020-11-06 | 中国水产科学研究院 | Reusable purification device |
| CN112973979A (en) * | 2021-02-04 | 2021-06-18 | 天津三好科技有限公司 | Extraction purifying tube and extraction system |
-
2019
- 2019-03-01 CN CN201920261816.8U patent/CN210448175U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111751195A (en) * | 2020-06-29 | 2020-10-09 | 中国水产科学研究院 | Multi-channel automatic purification device |
| CN111855366A (en) * | 2020-06-29 | 2020-10-30 | 中国水产科学研究院 | Automatic filtering type purification device for sample pretreatment |
| CN111888796A (en) * | 2020-07-17 | 2020-11-06 | 中国水产科学研究院 | Reusable purification device |
| CN112973979A (en) * | 2021-02-04 | 2021-06-18 | 天津三好科技有限公司 | Extraction purifying tube and extraction system |
| CN112973979B (en) * | 2021-02-04 | 2022-04-12 | 天津三好科技有限公司 | Extraction purifying tube and extraction system |
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