CN213903437U - Purification filter column for measuring residue amount of fipronil and metabolites thereof in eggs - Google Patents
Purification filter column for measuring residue amount of fipronil and metabolites thereof in eggs Download PDFInfo
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- CN213903437U CN213903437U CN202022701824.5U CN202022701824U CN213903437U CN 213903437 U CN213903437 U CN 213903437U CN 202022701824 U CN202022701824 U CN 202022701824U CN 213903437 U CN213903437 U CN 213903437U
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Abstract
The utility model discloses a fipronil and metabolite residual measure are with purifying and filtering post in egg, include: syringe pipe, first sieve, purification adsorbent layer, microfiltration membrane, second sieve, filtrate export, first sieve is located the upper portion of syringe intraduct space, the purification adsorbent layer sets up between first sieve and microfiltration membrane, the microfiltration membrane sets up in the lower part of purification adsorbent layer, the second sieve sets up in the lower part of microfiltration membrane, the filtrate export sets up in the bottom of syringe pipe. The utility model discloses a principle of purifying and filtering the post adopts the impurity that the adsorbent can effectively adsorb in the sample extract and does not adsorb the component that awaits measuring to effectual impurity of getting rid of the sample extract reaches purification and filterable purpose. The utility model discloses a purify the filtration post and be applicable to the remaining survey of fipronil and metabolite in the egg, it is easy and simple to handle quick, purifying effect is good.
Description
[ technical field ] A method for producing a semiconductor device
The utility model relates to a material technical field for the chemical analysis relates to the purification and filtration technology field, in particular to fipronil and its metabolite residual measure in egg are with purifying and filtering post.
[ background of the invention ]
Fipronil is an insecticide used for killing fleas, mites and lice, is used for preventing and controlling pests in a farm, can cause pollution to eggs when being used improperly, and has certain toxicity to human bodies after being eaten for a long time. The european union specifies: fipronil can not be used in the livestock and poultry breeding process of the human food industry chain. China GB2763-2019 defines the maximum residue of fipronil (the sum of fipronil, fipronil sulfone and fipronil sulfoxide, expressed as fipronil) in eggs to be 0.02mg/kg, and a detection method GB 23200.115-2018 liquid chromatogram-mass spectrum combination method for determining the residue of fipronil and its metabolite in eggs, which is suitable for determining the residue of fipronil and its metabolite in eggs, is issued in 6.21.2018.6.2018. The dispersed solid phase extraction purification process needs the steps of vortex adsorption and then centrifugation to obtain supernatant, so that the operation steps are multiple, the time is consumed, and the purification effect is not ideal.
[ Utility model ] content
The utility model aims at overcoming the defects existing in the prior art and providing a purification filter column for detecting fipronil and metabolites thereof in eggs with simple, convenient and quick operation and good purification effect.
For solving the technical problem, the utility model adopts the following technical scheme.
A purification filter column for measuring the residual quantity of fipronil and its metabolites in eggs comprises: syringe pipe, first sieve, purification adsorbent layer, microfiltration membrane, second sieve, filtrate export, first sieve is located the upper portion of syringe intraduct space, the purification adsorbent layer sets up between first sieve and microfiltration membrane, the microfiltration membrane sets up in the lower part of purification adsorbent layer, the second sieve sets up in the lower part of microfiltration membrane, the filtrate export sets up in the bottom of syringe pipe.
Further, the syringe tube was a tube having an inner diameter of 12.9mm, a tube length of 67.6mm, and a volume of 6 ml.
Further, the syringe barrel is made of polypropylene.
Further, the first sieve plate and the second sieve plate are sieve plates with the diameter of 13.0mm and the thickness of 1.2mm and the pore diameter of 20 mu m.
Further, the first screen deck and the second screen deck are both made of polypropylene.
Furthermore, the particle size of the adsorbent in the purification adsorbent layer is larger than the pore size of the first sieve plate 2 and the second sieve plate 5.
Further, the microfiltration membrane is a microfiltration membrane with a pore size of 0.2 μm.
Further, the microfiltration membrane is made of polytetrafluoroethylene.
Through this technical scheme, can realize following effect:
(1) the utility model provides a purify and filter post is applicable to fipronil and metabolite residual assay in the egg, and the post is directly crossed to the sample extract, can reach purification and filterable purpose.
(2) Compared with the dispersed solid phase extraction method of the national standard method, the purification filter column provided by the utility model uses the adsorption capacity and the column capacity which are better than C18The polystyrene/divinylbenzene (PEP) has better purification effect. Meanwhile, the purification column is prepared, purification and filtration are combined, the operation is simpler and quicker, and the sample pretreatment time is greatly saved.
[ description of the drawings ]
FIG. 1 is a schematic structural diagram of a purification filter column for measuring the residual quantity of fipronil and its metabolites in eggs.
[ detailed description ] embodiments
The present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following embodiments. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
As shown in figure 1, a purification filter column for measuring the residual quantity of fipronil and its metabolites in eggs comprises: the injection device comprises an injection tube 1, a first sieve plate 2, a purification adsorbent layer 3, a microporous filter membrane 4, a second sieve plate 5 and a filtrate outlet 6, wherein the first sieve plate 2 is positioned at the upper part of the inner space of the injection tube 1, the purification adsorbent layer 3 is arranged between the first sieve plate 2 and the microporous filter membrane 4, the microporous filter membrane 4 is arranged at the lower part of the purification adsorbent layer 3, the second sieve plate 5 is arranged at the lower part of the microporous filter membrane 4, and the filtrate outlet 6 is arranged at the bottom of the injection tube 1.
The syringe tube 1 is a polypropylene tube with the inner diameter of 12.9mm, the length of 67.6mm and the volume of 6ml and is used as a purifying filter columnThe housing of (1). The first sieve plate 2 and the second sieve plate 5 are polypropylene sieve plates with the diameter of 13.0mm and the thickness of 1.2mm and the aperture of 20 mu m, and mainly play roles in fixing the purifying adsorbent layer 3 and the microporous filter membrane 4 and controlling the flow rate of the column. The purifying adsorbent layer 3 comprises the following raw materials: 45-55mg of PSA powder with particle size of 40-60 μm, 45-55mg of PEP powder with particle size of 40-60 μm, and 45-55mg of C powder with particle size of 40-60 μm18The powder and 135-165mg anhydrous magnesium sulfate are uniformly mixed to form the extract, impurities in the extract can be selectively adsorbed without adsorbing the component to be detected, and the component to be detected is left in the purified filtrate to achieve the purpose of separating the impurities. The microporous filter membrane 4 is a Polytetrafluoroethylene (PTFE) microporous filter membrane with a pore diameter of 0.2 μm, and can filter purified liquid and prevent solution particles from blocking an instrument.
The utility model discloses an among the purification filtration column, purification adsorbent layer 3 is located the upper portion of millipore filtration 4, will guarantee to purify the adsorbent and load closely knit, can not be too loose, and first sieve 2 and second sieve 5 will be tight firm fixed purification adsorbent layer 3 and millipore filtration 4.
The use of the purification filter column of the present invention is further described in detail below in conjunction with practical applications:
example 1
Sample preparation: egg
The target object to be detected: fipronil and its metabolites (fluoronitrile, fipronil sulfone, fipronil sulfoxide)
Preparing a purifying and filtering column: the bottom of the injector tube 1 is arranged with a second sieve plate 5, and a filtrate outlet 6 is arranged under the second sieve plate 5, then the microporous filter membrane 4 is laid on the second sieve plate 5, the purifying adsorbent layer 3 is filled, and then the first sieve plate 2 is arranged to fix the purifying adsorbent layer 3 and the microporous filter membrane 4. The purifying adsorbent layer 3 comprises the following raw materials: 50mg of PSA powder with a particle size of 42-58 μm, 50mg of PEP powder with a particle size of 40-56 μm, and 50mg of C with a particle size of 41-55 μm18Powder and 160mg of anhydrous magnesium sulfate are uniformly mixed.
The application method of the purification filter column for measuring the residual quantity of fipronil and metabolites thereof in eggs comprises the following steps:
(1) preparing a sample extracting solution: taking 20ml of sample 1, 20ml of sample 2 and 20ml of sample 3 to extract the target object in the eggs;
(2) salting out and layering of the extracting solution: adding sodium chloride and anhydrous sodium sulfate into the extract, and performing vortex oscillation to separate acetonitrile and a water phase;
(3) purifying: the acetonitrile layer is taken to slowly pass through the purification filter column of the utility model, the filtrate is collected, the residue amount of fipronil in the sample 1 is 0.014mg/kg through detection, and metabolites of fipronil (such as fipronil, fipronil sulfone and fipronil sulfoxide) are not detected; the residual quantity of fipronil in the sample 2 is 0.015mg/kg, and metabolites of fipronil (fipronil, fipronil sulfone and fipronil sulfoxide) are not detected; the residual quantity of fipronil in the sample 3 is 0.017mg/kg, and metabolites of fipronil (fipronil, fipronil sulfone and fipronil sulfoxide) are not detected, which indicates that 3 samples all meet the requirement of national standard GB2763-2019 on the maximum residual quantity of fipronil (the sum of fipronil, fipronil sulfone and fipronil sulfoxide, expressed by fipronil) in eggs, and the maximum residual quantity is 0.02 mg/kg.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A fipronil and its metabolite residual amount in egg are measured and are used purification filtration post, its characterized in that includes: syringe pipe, first sieve, purification adsorbent layer, microfiltration membrane, second sieve, filtrate export, first sieve is located the upper portion of syringe intraduct space, the purification adsorbent layer sets up between first sieve and microfiltration membrane, the microfiltration membrane sets up in the lower part of purification adsorbent layer, the second sieve sets up in the lower part of microfiltration membrane, the filtrate export sets up in the bottom of syringe pipe.
2. The purifying filter column for measuring the residual quantity of fipronil and its metabolites in eggs according to claim 1, wherein the syringe tube is a tube with an inner diameter of 12.9mm, a tube length of 67.6mm and a volume of 6 ml.
3. The clean filter column for measuring the residual quantity of fipronil and its metabolites in eggs according to claim 2, wherein the syringe tube is made of polypropylene.
4. The purifying and filtering column for measuring the residual quantity of fipronil and its metabolites in eggs according to claim 1, wherein the first sieve plate and the second sieve plate are sieve plates with a diameter of 13.0mm and a thickness of 1.2mm and a pore size of 20 μm.
5. The egg fipronil and its metabolite residue amount measuring purifying filter column as claimed in claim 4, wherein the first sieve plate and the second sieve plate are made of polypropylene.
6. The purifying and filtering column for measuring the residual quantity of fipronil and its metabolites in eggs according to claim 1, wherein the particle size of the adsorbent in the purifying adsorbent layer is larger than the pore size of the first sieve plate 2 and the second sieve plate 5.
7. The purifying and filtering column for measuring the residual quantity of fipronil and its metabolites in eggs according to claim 1, wherein the microporous filter membrane is a 0.2 μm pore size microporous filter membrane.
8. The purifying and filtering column for measuring the residual quantity of fipronil and its metabolites in eggs as claimed in claim 7, wherein said microporous membrane is made of polytetrafluoroethylene.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022701824.5U CN213903437U (en) | 2020-11-20 | 2020-11-20 | Purification filter column for measuring residue amount of fipronil and metabolites thereof in eggs |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022701824.5U CN213903437U (en) | 2020-11-20 | 2020-11-20 | Purification filter column for measuring residue amount of fipronil and metabolites thereof in eggs |
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| Publication Number | Publication Date |
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| CN213903437U true CN213903437U (en) | 2021-08-06 |
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| CN202022701824.5U Active CN213903437U (en) | 2020-11-20 | 2020-11-20 | Purification filter column for measuring residue amount of fipronil and metabolites thereof in eggs |
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| CN (1) | CN213903437U (en) |
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