CN212459559U - Pretreatment rapid purification column for detecting perfluorinated compounds - Google Patents
Pretreatment rapid purification column for detecting perfluorinated compounds Download PDFInfo
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- CN212459559U CN212459559U CN202020461900.7U CN202020461900U CN212459559U CN 212459559 U CN212459559 U CN 212459559U CN 202020461900 U CN202020461900 U CN 202020461900U CN 212459559 U CN212459559 U CN 212459559U
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Abstract
The utility model discloses a quick purification column of pretreatment for perfluorocompound detects belongs to fodder and agricultural product quality safety inspection technical field. The pretreatment rapid purification column for detecting the perfluorinated compounds comprises: the bottom of the column tube is provided with a liquid outlet, and a lower sieve plate, a packing layer and an upper sieve plate are sequentially arranged in the column tube from the liquid outlet end to the top; the lower sieve plate and the upper sieve plate are respectively installed with the inner wall of the column tube in an interference fit manner; the top of the column tube is provided with a liquid inlet. The utility model discloses a perfluorocompound's quick purification column of pretreatment, easy operation need not activation, drip washing, elution during the purification, crosses the post through the syringe pressurization, and purifying process is about 20 seconds, has shortened purifying time greatly, has shortened at least 30 minutes than other methods. And the purification effect is excellent, after the purification, the grease and pigment impurities in the extracting solution are greatly reduced, and the sample purification requirement of liquid chromatography-tandem mass spectrometry can be met.
Description
Technical Field
The utility model belongs to the technical field of fodder and agricultural product quality safety inspection, concretely relates to quick purification column of pretreatment for perfluor compound detects.
Background
Perfluoro compounds (PFC)S) The organic pollutant is a novel persistent organic pollutant with all hydrogen atoms on an organic carbon chain replaced by fluorine atoms, and mainly comprises perfluorocarboxylic acid (PFCAs) and perfluorosulfonic acid (PFSAs). Excellent stability and hydrophobic and oleophobic performance, which makes it widely used in electronic products, textile, food package, lubricant, surface material, fire extinguishing and personal hygiene product. The biological sample has biological accumulation and environmental persistence, can migrate along with the atmosphere for a long distance, can be biologically amplified through a food chain, is widely existed in various environmental media, is detected in environmental samples, various wild animal serums, tissue samples (including organisms in the arctic circle) and human bodies, has biological toxicity, is related to various human diseases, seriously harms organisms and human health, and arouses the attention and attention of global decision makers and scientists.
The common detection method of the perfluorinated compounds is high performance liquid chromatography-tandem mass spectrometry, and has higher requirements on sample injection liquid. The agricultural product matrix is complex and various, especially biological samples such as livestock, poultry and aquatic products contain a large amount of grease, and the grease is difficult to completely remove by using a simple adsorption purification method. At present, a perfluorinated compound is mainly purified by using a solid phase extraction column in the pre-purification treatment process, but the solid phase extraction purification method has the disadvantages of complicated operation steps, relatively high technical requirements, time waste and labor waste. Therefore, a special rapid purifying column for perfluorinated compounds, which is simple to operate and has a good purifying effect, is urgently needed to be found so as to realize synchronous and effective purification of the perfluorinated compounds and apply the perfluorinated compounds to batch detection of agricultural products, and has a wide market popularization prospect in the actual market.
Disclosure of Invention
The utility model aims at solving the defects of the prior art and providing a pretreatment rapid purification column for detecting perfluorinated compounds.
The utility model adopts the following technical scheme:
the utility model provides a quick purifying column of pretreatment for perfluor compound detects, include:
the bottom of the column tube is provided with a liquid outlet, and a lower sieve plate, a packing layer and an upper sieve plate are sequentially arranged in the column tube from the liquid outlet end to the top;
the lower sieve plate and the upper sieve plate are respectively installed with the inner wall of the column tube in an interference fit manner;
the top of the column tube is provided with a liquid inlet.
In some of these embodiments, the filler layer is composed of multi-walled carbon, C18, and EDTA.
In some embodiments, the mass ratio of the multi-wall carbon to the C18 to the EDTA in the filler layer is 1: 1-2: 1.
Ethylene Diamine Tetraacetic Acid (EDTA) is an important complexing agent, 4 carboxyl groups of the EDTA can chelate metal ions, and potential heavy metal elements in agricultural product matrixes can be removed well; the C18 filler is a filler bonded by C18 with silica gel as a matrix, and the carbon chain of C18 can remove nonpolar components in agricultural products, such as fat and the like; the nanotube of the multi-wall carbon has a large specific surface area, has good adsorption performance on impurities such as pigments and the like, and can obviously remove interference impurities such as the pigments and the like. The three fillers are filled in layers according to a specific sequence in a specific proportion, have a good purification effect on agricultural product substrates, and have a wide application prospect.
In some embodiments, an adapter is disposed on the liquid inlet, the liquid inlet of the adapter is matched with a liquid outlet of the booster syringe, and the liquid outlet is cylindrical and disposed in the center of the bottom of the column tube.
In some embodiments, the column tube has an inner diameter of 1cm, a length of 10cm and a capacity of 5mL, the column tube is a polypropylene column tube, and the lower sieve plate and the upper sieve plate are both polyethylene plates.
The utility model also provides a manufacturing method for a quick purification column of pretreatment for perfluor compound detects, the step is as follows: and mounting a lower sieve plate at the liquid outlet end in the column pipe, filling the filler into the column pipe sequentially from the liquid inlet layer by layer, mounting the upper sieve plate into the column pipe, and flattening and compressing to obtain the composite material.
In some embodiments, EDTA, C18 and multi-wall carbon are sequentially filled into the column tube from the liquid inlet in a layered mode.
The utility model also provides a method that is arranged in the quick purification column of pretreatment that perfluor compound detected and purifies perfluor compound in the agricultural product, the step is as follows:
the method comprises the following steps: accurately weighing a freeze-dried agricultural product sample, adding acetonitrile, performing vortex oscillation and centrifugation, and taking supernate as an agricultural product extracting solution;
step two: and transferring the agricultural product sample extracting solution to a pressurizing injector, and pushing the agricultural product sample extracting solution into the rapid purification column through the pressurizing injector to obtain the agricultural product matrix purifying solution.
In some of these examples, 1.0g of the freeze-dried agricultural product sample was added to 10mL of acetonitrile in step one, vortexed for 1 h, and centrifuged at 4500rpm for 10 min.
Compared with the prior art, the utility model, its beneficial effect does:
firstly, the method comprises the following steps: the utility model has simple manufacturing method of the perfluorinated compound pretreatment rapid purification column, is convenient for large-scale production, can be automatically filled by detection personnel, and has strong practical significance;
secondly, the method comprises the following steps: the utility model discloses a perfluorocompound's quick purification column of pretreatment, easy operation need not activation, drip washing, elution during the purification, crosses the post through the syringe pressurization, and purifying process is about 20 seconds, has shortened purifying time greatly, has shortened at least 30 minutes than other methods.
Thirdly, the method comprises the following steps: the utility model discloses a perfluorocompound's quick purification column of pretreatment, purifying effect is fabulous, through its purification back, grease, pigment impurity significantly reduce in the extract, can reach the sample purification requirement of liquid chromatogram-tandem mass spectrum.
Drawings
FIG. 1 is a schematic structural view of a perfluorinated compound pretreatment rapid purification column of the present invention;
FIG. 2 is a bar graph of the matrix effect of perfluorochemicals (PFDA, PFUnDA) under 6 columns;
FIG. 3 is a bar graph of fractional column recovery of a perfluorinated compound standard;
FIG. 4 is a graph comparing the purification effect of the pre-treatment purification column on crab matrix;
wherein, 1, a column tube; 2. pressurizing the injector; 3. a liquid outlet; 4. a lower sieve plate; 5. a filler; 6. an upper sieve plate; 7. and (4) a liquid inlet.
Detailed Description
The present invention will be further clarified by the following specific examples, which are intended to be only illustrative and not limiting of the scope of the invention, which after reading the present invention, all modifications that may be made by a person skilled in the art to the various equivalent forms of the invention fall within the scope of the claims appended hereto.
The utility model provides a quick purifying column of pretreatment for perfluor compound detects, include:
the device comprises a column tube 1, wherein a liquid outlet 3 is formed in the bottom of the column tube 1, and a lower sieve plate 4, a packing layer 5 and an upper sieve plate 6 are sequentially arranged in the column tube 1 from the liquid outlet end to the top;
the lower sieve plate 4 and the upper sieve plate 6 are respectively installed on the inner wall of the column tube 1 in an interference fit manner;
the top of the column tube 1 is provided with a liquid inlet 7.
In one embodiment, the filler layer 5 is composed of multi-walled carbon, C18, and EDTA.
In one embodiment, the mass ratio of the multi-wall carbon to the C18 to the EDTA in the filler layer 5 is 1: 1-2: 1.
Ethylene Diamine Tetraacetic Acid (EDTA) is an important complexing agent, 4 carboxyl groups of the EDTA can chelate metal ions, and potential heavy metal elements in agricultural product matrixes can be removed well; the C18 filler is a filler bonded by C18 with silica gel as a matrix, and the carbon chain of C18 can remove nonpolar components in agricultural products, such as fat and the like; the nanotube of the multi-wall carbon has a large specific surface area, has good adsorption performance on impurities such as pigments and the like, and can obviously remove interference impurities such as the pigments and the like. The three fillers are filled in layers according to a specific sequence in a specific proportion, have a good purification effect on agricultural product substrates, and have a wide application prospect.
In one embodiment, the liquid inlet 7 is provided with an adapter 8, the liquid inlet of the adapter 8 is matched with the liquid outlet of the booster syringe 2, and the liquid outlet 3 is cylindrical and is arranged at the center of the bottom of the column tube 1.
In one embodiment, the column tube 1 has an inner diameter of 1cm, a length of 10cm and a capacity of 5mL, the column tube 1 is a polypropylene column tube, and the lower sieve plate 4 and the upper sieve plate 6 are both polyethylene plates.
The utility model also provides a manufacturing method for a quick purification column of pretreatment for perfluor compound detects, the step is as follows: and (3) mounting a lower sieve plate 4 at the liquid outlet end in the column tube 1, sequentially filling the filler into the column tube 1 from a liquid inlet 7 in a layering manner, mounting an upper sieve plate 6 into the column tube 1, and flattening and compressing to obtain the composite material.
In one embodiment, EDTA, C18, and multi-walled carbon are sequentially layered from loading port 7 into column tube 1.
The utility model also provides a method that is arranged in the quick purification column of pretreatment that perfluor compound detected and purifies perfluor compound in the agricultural product, the step is as follows:
the method comprises the following steps: accurately weighing a freeze-dried agricultural product sample, adding acetonitrile, performing vortex oscillation and centrifugation, and taking supernate as an agricultural product extracting solution;
step two: and transferring the agricultural product sample extracting solution to a pressurizing injector 2, and pushing the agricultural product sample extracting solution into the rapid purification column through the pressurizing injector 2 to obtain the agricultural product matrix purifying solution.
In one example, 1.0g of a freeze-dried sample of agricultural product is added to 10mL of acetonitrile in step one, vortexed for 1 h, and centrifuged at 4500rpm for 10 min.
The size of the adapter 8 used in the utility model is matched with the column tube, which plays the role of connecting the injector and the column tube; the utility model discloses can use Shanghai clever biotechnology limited, the model: 6mL adapter.
The utility model discloses raw materials and reagent that well use as follows:
95% of multi-wall carbon, 3-5 nm of inner diameter, 8-5 nm of outer diameter and 50um of length, and is purchased from alatin.
C18: diameter of 40-60 μm, carbon content of 18%, available from Aijier.
EDTA: 99.5% from Solibao.
The present invention will be described in further detail with reference to several embodiments.
Examples
Screening of purification column packing
Selecting 7 common purifying materials (NH)2C18, MgSO4, PSA, GCB, multiwall carbon, EDTA) in different combinations, each NH2；C18/NH2(ii) a MgSO 4/PSA; MgSO 4/PSA/C18; MgSO 4/PSA/C18/GCB; multi-wall carbon/C18/EDTA, which are respectively layered and loaded into a hollow column tube with a lower sieve plate at the bottom, and an upper sieve plate is loaded on a purifying material, and the purifying material is properly compacted to prepare 6 kinds of purifying columns and combinations. 10mL of the extract was taken, and after passing through a column under pressure by means of a syringe, all the effluent was collected.
The tested purifying column multi-wall carbon/C18/EDTA purifying column has a good purifying effect, the other 5 purifying columns with combined fillers have no obvious purifying effect, and especially, a large amount of grease in column passing liquid is not removed, so that serious interference is caused to a chromatographic column and a liquid instrument.
And blowing the effluent to 1mL of the solution at 40 ℃ by using nitrogen, passing through a 0.22 mu m filter membrane as a solvent to prepare a matrix standard sample, detecting the liquid quality, taking another 10mL of the perfluorinated compound standard substance, pressurizing the perfluorinated compound standard substance by using a syringe, passing through a multi-wall carbon/C18/EDTA purification column, and collecting the effluent in sections.
The matrix effect and the purification column adsorption effect of the perfluorinated compounds are used as the basis for screening the purification filler, and fig. 2 is a bar chart of the matrix effect of the perfluorinated compounds (PFDA, PFUnDA). As can be seen from FIG. 2, NH2；C18/NH2；MgSO4/PSA(ii) a MgSO 4/PSA/C18; the purification column of the combination of MgSO4/PSA/C18/GCB 5 fillers has almost no purification effect, the perfluorinated compound matrix effect is more than 150%, and after the purification column of multiwall carbon/C18/EDTA, the perfluorinated compound matrix effect is about 100%. FIG. 3 is a bar graph of fractional column recovery of a perfluorinated compound standard. As can be seen from FIG. 3, the multiwall carbon/C18/EDTA filler has no adsorption effect on the perfluorinated compounds, and the segmented effluent is about 35%, which indicates that the perfluorinated compounds are not retained in the multiwall carbon/C18/EDTA purification column. Therefore, multiwall carbon/C18/EDTA is used as the rapid purification column filler in the pretreatment of the perfluorinated compounds.
Example 1: perfluor compound pre-treatment quick purifying column raw material and preparation
(1) Raw materials:
column tube: the volume is 5mL, the inner diameter is 1cm, and the length is 10 cm; the filling amount of the filler in the column tube is 300 mg;
sieve plate: polyethylene plates with a pore size of 10 μm.
(2) Preparation:
and (3) mounting a lower sieve plate at the liquid outlet end of the column tube, sequentially filling 75mg of EDTA, 150 mg of C18 and 75mg of multi-wall carbon into the column tube in a layering manner from the liquid inlet end, mounting the upper sieve plate into the column tube, mounting the upper sieve plate and the lower sieve plate in an interference fit manner, and pressing to obtain the catalyst.
Example 2: perfluor compound pre-treatment quick purifying column raw material and preparation
(1) Raw materials: same as in example 1
(2) Preparation:
and (3) mounting a lower sieve plate at the liquid outlet end of the column tube, sequentially filling 100mg of EDTA, 100mg of C18 and 100mg of multi-wall carbon into the column tube in a layering manner from the liquid inlet end, mounting the upper sieve plate into the column tube, mounting the upper sieve plate and the lower sieve plate in an interference fit manner, and pressing to obtain the composite material.
Comparing the purification columns obtained in examples 1 and 2, it was found that the purification column obtained in example 1 had a good purification effect, and it was found that the purification column prepared by filling 75mg of EDTA, 150 mg of C18, and 75mg of multi-walled carbon in layers and using the combination as a filler could achieve a good purification effect.
Application example: crab sample was purified using the perfluoro compound pretreatment rapid purification column prepared in example 1
(1) Accurately weighing 1.0g of freeze-dried crab sample into a 50mL centrifuge tube, accurately adding 10mL of acetonitrile, carrying out vortex oscillation for 1 h, centrifuging at 4500rpm for 10 min, and taking supernatant as crab extract;
(2) transferring the crab sample extract into a syringe; push into the purifying column through the syringe with the sample extract, the extract pressurizes the utility model discloses the quick purifying column of perfluor compound pretreatment who makes obtains crab matrix purifying liquid.
The comparison graph of the appearance before and after purification of the crab sample extract by using the perfluorinated compound pretreatment rapid purification column is shown in fig. 4, wherein A is the appearance before purification, and B is the appearance after purification, and the comparison shows that after purification by the purification column, yellow matrix liquid completely disappears, and the super-strong capability of removing grease and pigment of the purification column is embodied.
Although the embodiments of the present invention have been described in detail in the above examples, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the scope of knowledge possessed by those skilled in the art. The above description is only a preferred and practical embodiment of the present invention, and not intended to limit the scope of the present invention, and all structural equivalents made by using the contents of the specification and drawings are included in the scope of the present invention.
Claims (2)
1. A pretreatment rapid purification column for detecting perfluorinated compounds is characterized by comprising:
the device comprises a column tube (1), wherein a liquid outlet (3) is formed in the bottom of the column tube (1), and a lower sieve plate (4), a packing layer (5) and an upper sieve plate (6) are sequentially arranged in the column tube (1) from bottom to top from the liquid outlet end;
the lower sieve plate (4) and the upper sieve plate (6) are respectively installed on the inner wall of the column tube (1) in an interference fit manner;
a liquid inlet (7) is arranged at the top of the column tube (1);
wherein, be equipped with switching adapter (8) on inlet (7), the inlet of switching adapter (8) and the liquid outlet phase-match of booster syringe (2), liquid outlet (3) are cylindricly, and set up in the bottom center of pillar pipe (1).
2. The pretreatment rapid purification column for detecting perfluoro compounds according to claim 1, characterized in that the column tube (1) has an inner diameter of 1cm, a length of 10cm and a capacity of 5mL, the column tube (1) is a polypropylene column tube, and the lower sieve plate (4) and the upper sieve plate (6) are both polyethylene plates.
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| CN111307997A (en) * | 2020-04-01 | 2020-06-19 | 上海市农业科学院 | Pretreatment rapid purification column for detecting perfluorinated compounds and manufacturing method and application thereof |
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