CN114487221A - Detection apparatus for clenbuterol residual quantity in survey animal food - Google Patents
Detection apparatus for clenbuterol residual quantity in survey animal food Download PDFInfo
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- CN114487221A CN114487221A CN202011530626.5A CN202011530626A CN114487221A CN 114487221 A CN114487221 A CN 114487221A CN 202011530626 A CN202011530626 A CN 202011530626A CN 114487221 A CN114487221 A CN 114487221A
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- 238000001514 detection method Methods 0.000 title claims abstract description 41
- 229960001117 clenbuterol Drugs 0.000 title claims abstract description 38
- STJMRWALKKWQGH-UHFFFAOYSA-N clenbuterol Chemical compound CC(C)(C)NCC(O)C1=CC(Cl)=C(N)C(Cl)=C1 STJMRWALKKWQGH-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 241001465754 Metazoa Species 0.000 title claims abstract description 31
- 235000013305 food Nutrition 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 67
- 230000007246 mechanism Effects 0.000 claims abstract description 53
- 238000000926 separation method Methods 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 238000001179 sorption measurement Methods 0.000 claims abstract description 12
- 238000012784 weak cation exchange Methods 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 23
- 239000003480 eluent Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 238000010586 diagram Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
- 238000001212 derivatisation Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000012074 organic phase Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- 239000007787 solid Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XCOBLONWWXQEBS-KPKJPENVSA-N N,O-bis(trimethylsilyl)trifluoroacetamide Chemical compound C[Si](C)(C)O\C(C(F)(F)F)=N\[Si](C)(C)C XCOBLONWWXQEBS-KPKJPENVSA-N 0.000 description 2
- 229940125388 beta agonist Drugs 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 206010006458 Bronchitis chronic Diseases 0.000 description 1
- 238000002965 ELISA Methods 0.000 description 1
- 206010014561 Emphysema Diseases 0.000 description 1
- 241000282887 Suidae Species 0.000 description 1
- 210000004100 adrenal gland Anatomy 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 206010006451 bronchitis Diseases 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 208000007451 chronic bronchitis Diseases 0.000 description 1
- 229960001399 clenbuterol hydrochloride Drugs 0.000 description 1
- OPXKTCUYRHXSBK-UHFFFAOYSA-N clenbuterol hydrochloride Chemical compound Cl.CC(C)(C)NCC(O)C1=CC(Cl)=C(N)C(Cl)=C1 OPXKTCUYRHXSBK-UHFFFAOYSA-N 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 208000030603 inherited susceptibility to asthma Diseases 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- IUBSYMUCCVWXPE-UHFFFAOYSA-N metoprolol Chemical compound COCCC1=CC=C(OCC(O)CNC(C)C)C=C1 IUBSYMUCCVWXPE-UHFFFAOYSA-N 0.000 description 1
- 229960002237 metoprolol Drugs 0.000 description 1
- 235000015277 pork Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to the technical field of chemical detection devices, in particular to a detection device for determining the residual quantity of clenbuterol in animal food, which comprises a gas chromatograph-mass spectrometer and a plurality of sample preparation mechanisms; the sample preparation mechanism comprises an ultrasonic processor, a liquid separation mechanism, a first concentrator, an adsorption mechanism and a second concentrator. The invention solves the problems of complex sample pretreatment operation and long treatment time when the residual quantity of clenbuterol in animal food is determined by a GC-MS method in the prior art. Above-mentioned detection device will make appearance mechanism and detection mechanism (gas chromatography-mass spectrometer) and use jointly, will await measuring the sample and put into the system appearance mechanism and can make the appearance, need not operating personnel and take to the system appearance in the treater of difference many times, can reduce the pollution rate on the one hand, thereby on the other hand can save personnel's operating time raise the efficiency.
Description
Technical Field
The invention relates to the technical field of chemical detection devices, in particular to a detection device for determining the residual quantity of clenbuterol in animal food.
Background
Clenbuterol is known as clenbuterol hydrochloride, or clenbuterol, ammonia-Xiao-Min, and amitutol, and is white crystalline powder with slightly bitter taste.
Clenbuterol is a general name of a class of drugs, mainly adrenal glands, beta agonists and beta-agonists (beta-agonst), and is used for treating diseases such as bronchial asthma, chronic bronchitis, emphysema and the like.
The clenbuterol can promote the growth of pigs, reduce fat content and improve the clenbuterol rate when being used in the feed in a large dose, but the eating of pork containing the clenbuterol is harmful to human bodies, and the clenbuterol is forbidden in China.
In the prior art, the clenbuterol residual quantity in animal food is mainly determined as follows: gas chromatography-mass spectrometry, high performance liquid chromatography, enzyme-linked immunosorbent assay, and liquid chromatography-mass spectrometry/mass spectrometry.
The GC-MS method has the advantages of combining the efficient and rapid separation effect of the chromatogram with the qualitative analysis of the mass spectrum with high sensitivity, being capable of carrying out qualitative and quantitative analysis on a certain specific residue under the condition that a plurality of residues exist simultaneously, and having higher detection limit. The GC-MS method has good specificity, strong selectivity, higher detection accuracy and low false positive rate; the defects are that the sample pretreatment operation is complicated, the treatment time is long, the detection process is complicated and the operation is difficult.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a detection device for determining residual clenbuterol content in animal food, which is used for solving the problems of complicated sample pretreatment operation and long treatment time when determining residual clenbuterol content in animal food by GC-MS method in the prior art. Above-mentioned detection device will make appearance mechanism and detection mechanism (gas chromatography-mass spectrometer) and use jointly, will await measuring the sample and put into the system appearance mechanism and can make the appearance, need not operating personnel and take to the system appearance in the treater of difference many times, can reduce the pollution rate on the one hand, thereby on the other hand can save personnel's operating time raise the efficiency.
In order to achieve the above objects and other related objects, the present invention provides a detection device for determining residual clenbuterol content in animal food, comprising a GC-MS and a plurality of sample preparation mechanisms; the sample preparation mechanism comprises an ultrasonic processor, a liquid separation mechanism, a first concentrator, an adsorption mechanism and a second concentrator;
the ultrasonic processor is internally provided with a plurality of sample processing tanks, and the sample processing tanks are provided with extracting agent adding pipes;
the liquid separating mechanism comprises a liquid separating bottle, and the liquid separating bottle is connected with the super sample processing tank through a first pipeline; the liquid separation bottle is connected with the first support frame through a rotating shaft, and the rotating shaft is connected with a first motor;
the first concentrator is connected with the liquid separation bottle through a second pipeline;
the adsorption mechanism comprises a weak cation exchange column, and the weak cation exchange column is connected with the first concentrator through a third pipeline; the weak cation exchange column is connected with the second support frame, and an eluent adding pipe is installed at the inlet end of the weak cation exchange column; a liquid collecting tank is arranged at the outlet end of the weak cation exchange column;
the second concentrator is connected with the liquid collecting tank through a fourth pipeline, and a derivative adding pipe is installed on the second concentrator; the second concentrator is connected with the gas chromatograph-mass spectrometer through a fifth pipeline;
wherein, first concentrator and second concentrator all are connected with the blast pipe.
Above-mentioned detection device will make appearance mechanism and detection mechanism (gas chromatography-mass spectrometer) and use jointly, will await measuring the sample and put into the system appearance mechanism and can make the appearance, need not operating personnel and take to the system appearance in the treater of difference many times, can reduce the pollution rate on the one hand, thereby on the other hand can save personnel's operating time raise the efficiency.
The detection device comprises a plurality of sample preparation mechanisms, so that a plurality of samples can be prepared in batch, the sample preparation efficiency is improved, and the detection efficiency is improved.
The sample preparation mechanism comprises an ultrasonic processor, a liquid separation mechanism, a first concentrator, an adsorption mechanism and a second concentrator, the whole sample preparation process is reasonable in design, a sample is subjected to homogenate ultrasonic treatment by the ultrasonic processor, then an extracting agent is added for extraction, then an organic phase is obtained by liquid separation, the organic phase is added into a weak cation exchange column after being concentrated by the first concentrator, an eluent is concentrated by the second concentrator after being separated by the weak cation exchange column, and a derivatization agent is added for derivatization after concentration, so that the sample preparation mechanism can be used for sample loading detection of a gas chromatograph-mass spectrometer.
The liquid separating mechanism comprises a liquid separating bottle, the liquid separating bottle can rock under the driving of a motor, and the function of uniformly shaking and separating liquid can be realized without the operation of an operator.
In an embodiment of the present invention, a stirring blade is installed in the sample processing tank, the stirring blade is connected to a stirring shaft, and the stirring shaft is connected to the second motor. Through setting up stirring vane, play the effect of mixing stirring on the one hand, on the other hand can play the effect of stirring to the solid sample.
In an embodiment of the present invention, the sample processing tank includes a tank body and a cover body, the tank body and the cover body are detachably connected, the extractant adding pipe and the first pipeline are both connected to the tank body, the stirring shaft penetrates through the cover body, and the second motor is mounted on the cover body.
In an embodiment of the present invention, the liquid-separating bottle is a liquid-separating device with a large top and a small bottom, and the large top and the small bottom are separated into layers.
In an embodiment of the present invention, a liquid outlet pipe is disposed at the bottom of the liquid separation bottle, and a valve is disposed on the liquid outlet pipe; the top of the liquid separation bottle is provided with a liquid inlet pipe. The liquid inlet pipe can be filled with solvent or pure water, so that the washing can be carried out for multiple times, and the separation effect is better.
In an embodiment of the present invention, the weak cation exchange column is detachably connected to the second support frame.
In an embodiment of the invention, the first concentrator and the second concentrator are both provided with heating plates. The heat patch provides energy to concentrate the liquid in the first and second concentrators.
In one embodiment of the present invention, the first concentrator is installed above the weak cation exchange column. Since the first concentrator is installed above the weak cation exchange column, the third conduit is short and therefore there is little loss of concentrate.
As described above, the detection device for determining the residual amount of clenbuterol in animal food according to the present invention has the following beneficial effects: above-mentioned detection device will make appearance mechanism and detection mechanism (gas chromatography-mass spectrometer) and use jointly, will await measuring the sample and put into the system appearance mechanism and can make the appearance, need not operating personnel and take to the system appearance in the treater of difference many times, can reduce the pollution rate on the one hand, thereby on the other hand can save personnel's operating time raise the efficiency. The detection device comprises a plurality of sample preparation mechanisms, so that a plurality of samples can be prepared in batch, the sample preparation efficiency is improved, and the detection efficiency is improved.
Drawings
Fig. 1 is a schematic overall view of a detection device for determining the residual amount of clenbuterol in animal food according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of a sample preparation mechanism of a detection device for determining residual clenbuterol content in animal food in the embodiment of the invention.
Fig. 3 is a schematic connection diagram of a sample treatment tank, a liquid separation mechanism, a first concentrator, an adsorption mechanism and a second concentrator of a detection device for determining the residual amount of clenbuterol in animal food according to an embodiment of the present invention.
Fig. 4 is a schematic view showing a sample treatment tank of a detection device for determining residual clenbuterol content in animal food according to an embodiment of the present invention (a cover and a tank are connected).
Fig. 5 is a schematic diagram of a sample treatment tank of a detection device for determining residual clenbuterol content in animal food according to an embodiment of the present invention (the cover and the tank are in a separated state).
Fig. 6 is a schematic diagram of a liquid separating mechanism of a detection device for determining clenbuterol residual quantity in animal food in the embodiment of the invention.
Fig. 7 is a schematic diagram of a first concentrator of a detection device for determining residual clenbuterol content in animal food according to an embodiment of the present invention.
Fig. 8 is a schematic diagram showing an adsorption mechanism of a detection device for determining residual clenbuterol content in animal food in an embodiment of the present invention.
Fig. 9 is a schematic diagram of a second concentrator of a detection device for determining residual clenbuterol content in animal food according to an embodiment of the present invention.
Description of the element reference numerals
1-gas chromatography-mass spectrometry;
2-a sample preparation mechanism; 201-ultrasonic processor, 2011-sample treatment tank, 20111-tank, 20112-cover, 2012-extractant adding pipe, 2013-stirring blade, 2014-stirring shaft, 2015-second motor; 202-liquid separating mechanism, 2021-liquid separating bottle, 2022-rotating shaft, 2023-first supporting frame, 2024-first motor, 2025-liquid outlet pipe, 2026-valve, 2027-liquid inlet pipe; 203-a first concentrator; 204-adsorption mechanism, 2041-weak cation exchange column, 2042-second support frame, 2043-eluent addition tube and 2044-liquid collecting tank; 205-second concentrator, 2051-derivitization agent addition tube;
3-a first conduit; 4-a second conduit; 5-a third conduit; 6-a fourth conduit; 7-a fifth pipeline; 8-an exhaust pipe; 9-heating plate.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Please refer to fig. 1 to 9. It should be understood that the structures, ratios, sizes, and the like shown in the drawings and described in the specification are only used for matching with the disclosure of the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions under which the present invention can be implemented, so that the present invention has no technical significance, and any structural modification, ratio relationship change, or size adjustment should still fall within the scope of the present invention without affecting the efficacy and the achievable purpose of the present invention. In addition, the terms "upper", "lower", "left", "right", "middle" and "one" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the terms is not to be construed as a scope of the present invention.
Referring to fig. 1, the present invention provides a detection apparatus for determining clenbuterol residual quantity in animal food, the detection apparatus includes a gas chromatograph-mass spectrometer 1 and a plurality of sample preparation mechanisms 2 (refer to fig. 1); the sample preparation mechanism 2 comprises an ultrasonic processor 201, a liquid separation mechanism 202, a first concentrator 203, an adsorption mechanism 204 and a second concentrator 205;
an ultrasonic processor 201, wherein a plurality of sample processing tanks 2011 (see fig. 2 and 3) are installed in the ultrasonic processor 201, and an extractant adding pipe 2012 is installed on the sample processing tanks 2011; a stirring blade 2013 (please refer to fig. 5) is installed in the sample processing tank 2011, the stirring blade 2013 is connected with a stirring shaft 2014, and the stirring shaft 2014 is connected with a second motor 2015; the sample processing tank 2011 includes a tank 20111 and a cover 20112, the tank 20111 and the cover 20112 are detachably connected (please refer to fig. 4 and 5), the extractant adding pipe 2012 and the first pipeline 3 are both connected with the tank 20111, the stirring shaft 2014 penetrates through the cover 20112, and the second motor 2015 is installed on the cover 20112;
referring to fig. 6, the liquid separating mechanism 202 includes a liquid separating bottle 2021 (a liquid separating bottle 2021 with a large top and a small bottom), and the liquid separating bottle 2021 is connected to the ultra-sample processing tank 2011 through a first pipe 3; the liquid separation bottle 2021 is connected with the first support 2023 through a rotating shaft 2022, and the rotating shaft 2022 is connected with a first motor 2024; a liquid outlet pipe 2025 is arranged at the bottom of the liquid separation bottle 2021, and a valve 2026 is arranged on the liquid outlet pipe 2025; the top of the liquid separation bottle 2021 is provided with a liquid inlet pipe 2027;
referring to fig. 7, a first concentrator 203, the first concentrator 203 is connected to the liquid separation bottle 2021 through a second pipe 4;
referring to fig. 8, the adsorption mechanism 204 comprises a weak cation exchange column 2041, the weak cation exchange column 2041 is connected with the first concentrator 203 through a third pipe 5, and the first concentrator 203 is installed above the weak cation exchange column 2041; the weak cation exchange column 2041 is connected to a second support frame 2042, and an eluent addition pipe 2043 is installed at the inlet end of the weak cation exchange column 2041; a liquid collecting tank 2044 is installed at the outlet end of the weak cation exchange column 2041;
referring to fig. 9, the second concentrator 205 is connected to the sump 2044 through a fourth pipe 6, and a derivative adding pipe 2051 is installed on the second concentrator 205; the second concentrator 205 is connected with the gas chromatograph-mass spectrometer 1 through a fifth pipeline 7;
wherein, the first concentrator 203 and the second concentrator 205 are both connected with the exhaust pipe 8; the weak cation exchange column 2041 is detachably connected to the second support 2042; the first concentrator 203 and the second concentrator 205 are both provided with heating plates 9; in order to adapt to the shaking of the liquid separation bottle 2021, the pipelines arranged on the liquid separation bottle are hoses, mainly comprising a first pipeline 3, a second pipeline 4 and a liquid inlet pipe 2027.
The detection device for determining the residual quantity of the clenbuterol in the animal food adopts a GB/T5009.193-2003' determination of the residual quantity of the clenbuterol in the animal food-GC/MS method, and the basic principle is as follows: shearing a solid sample, homogenizing with a perchloric acid solution, performing ultrasonic extraction, extracting with isopropanol + ethyl acetate (40+60), concentrating an organic phase after extraction, separating by using a weak cation exchange column 2041, eluting with an ethanol + concentrated ammonia water (98+2) solution, concentrating an eluent, reducing the polarity of a compound containing hydroxyl groups by using an N, O-bis (trimethylsilyl) trifluoroacetamide (hydroxyl derivatization reagent, increasing the volatility of the compound, and making the sample more suitable for GC analysis), then feeding the sample to a gas chromatograph-mass spectrometer 1 for determination, and quantifying by using metoprolol as an internal standard.
The working process of the detection device for determining the residual quantity of the clenbuterol in the animal food comprises the following steps:
s1, adding the solid sample into a sample processing tank 2011, adding a perchloric acid solution into the sample processing tank 2011, starting a second motor 2015, driving a stirring shaft 2014 to rotate by the second motor 2015, driving stirring blades 2013 to rotate by the stirring shaft 2014, and stirring and homogenizing by the stirring blades 2013;
s2, adding an extractant (i.e., isopropyl alcohol + ethyl acetate (40+60)) into the sample processing tank 2011 through the extractant adding pipe 2012, stirring and extracting, and then inputting the liquid from the first pipeline 3 into the liquid separation bottle 2021;
s3, start the first motor 2024, the first motor 2024 drives the rotation axis 2022 to rotate forward and backward, the rotation axis 2022 drives the liquid separation bottle 2021 to rotate forward and backward, the included angle between the highest point of rotation and the vertical line is 45 °, then the water phase is discharged through the liquid outlet pipe 2025 (the water phase is below because the ethyl acetate is lighter than water), then purified water is added through the liquid inlet pipe 2027 for washing for many times, and finally the organic phase is transported to the first concentrator 203 through the second pipeline 4;
s4, heating the heating plate 9 of the first concentrator 203 to volatilize the solvent in the organic phase and discharge the solvent from the exhaust pipe 8;
s5, the concentrated solution in the first concentrator 203 enters the weak cation exchange column 2041 through the third pipe 5, the concentrated solution is separated in the weak cation exchange column 2041, and an eluent (ethanol + concentrated ammonia (98+2)) is added to the weak cation exchange column 2041 through the eluent addition pipe 2043 and enters the liquid collection tank 2044;
s6, the eluent enters the second concentrator 205 from the liquid collecting tank 2044 through the fourth pipeline 6, and the heating sheet 9 of the second concentrator 205 heats the eluent to volatilize the solvent in the eluent, so that the solvent is discharged from the exhaust pipe 8;
s7, adding a derivatization agent (N, O-bis (trimethylsilyl) trifluoroacetamide) to the concentrated solution of the second concentrator 205 through a derivatization agent addition pipe 2051;
and S8, conveying the derived sample to a sample tray of the gas chromatograph-mass spectrometer 1 through a fifth pipeline 7.
In summary, the detection device of the invention combines the sample preparation mechanism 2 and the detection mechanism (gas chromatograph-mass spectrometer 1) for use, and samples can be prepared by putting samples to be detected into the sample preparation mechanism 2 without taking the samples to different processors for multiple times by operators, so that on one hand, the pollution rate can be reduced, and on the other hand, the operation time of the operators can be saved, thereby improving the efficiency. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. A detection device for determining the residual quantity of clenbuterol in animal food is characterized by comprising a gas chromatograph-mass spectrometer (1) and a plurality of sample preparation mechanisms (2); the sample preparation mechanism (2) comprises an ultrasonic processor (201), a liquid separation mechanism (202), a first concentrator (203), an adsorption mechanism (204) and a second concentrator (205);
the ultrasonic treatment device comprises an ultrasonic processor (201), wherein a plurality of sample treatment tanks (2011) are installed in the ultrasonic processor (201), and extracting agent adding pipes (2012) are installed on the sample treatment tanks (2011);
the liquid separating mechanism (202) comprises a liquid separating bottle (2021), and the liquid separating bottle (2021) is connected with the ultra-sample processing tank (2011) through a first pipeline (3); the liquid separation bottle (2021) is connected with the first support frame (2023) through a rotating shaft (2022), and the rotating shaft (2022) is connected with the first motor (2024);
the first concentrator (203), the first concentrator (203) is connected with the liquid separation bottle (2021) through a second pipeline (4);
an adsorption mechanism (204), the adsorption mechanism (204) comprising a weak cation exchange column (2041), the weak cation exchange column (2041) being connected to the first concentrator (203) by a third conduit (5); the weak cation exchange column (2041) is connected with a second support frame (2042), and an eluent addition pipe (2043) is installed at the inlet end of the weak cation exchange column (2041); a liquid collecting tank (2044) is arranged at the outlet end of the weak cation exchange column (2041);
a second concentrator (205), wherein the second concentrator (205) is connected with the liquid collecting tank (2044) through a fourth pipeline (6), and a derivative adding pipe (2051) is installed on the second concentrator (205); the second concentrator (205) is connected with the gas chromatograph-mass spectrometer (1) through a fifth pipeline (7);
wherein the first concentrator (203) and the second concentrator (205) are both connected with an exhaust pipe (8).
2. The apparatus for detecting clenbuterol residual quantity in animal food according to claim 1, wherein: install stirring vane (2013) in sample processing jar (2011), stirring vane (2013) is connected with (mixing) shaft (2014), (mixing) shaft (2014) second motor (2015) are connected.
3. The apparatus for detecting clenbuterol residual quantity in animal food according to claim 2, wherein: sample processing jar (2011) is including jar body (20111) and lid (20112), the connection can be dismantled to jar body (20111) and lid (20112), extraction agent adds pipe (2012) and first pipeline (3) and all is connected with jar body (20111), (mixing) shaft (2014) run through lid (20112), second motor (2015) is installed on lid (20112).
4. The apparatus for detecting clenbuterol residual quantity in animal food according to claim 1, wherein: the liquid separation bottle (2021) is a liquid separation bottle (2021) with a large upper part and a small lower part.
5. The apparatus for detecting clenbuterol residual quantity in animal food according to claim 4, wherein: a liquid outlet pipe (2025) is arranged at the bottom of the liquid separation bottle (2021), and a valve (2026) is arranged on the liquid outlet pipe (2025); the top of the liquid separation bottle (2021) is provided with a liquid inlet pipe (2027).
6. The apparatus for detecting clenbuterol residual quantity in animal food according to claim 1, wherein: the weak cation exchange column (2041) is detachably connected with the second support frame (2042).
7. The apparatus for detecting clenbuterol residual quantity in animal food according to claim 1, wherein: the first concentrator (203) and the second concentrator (205) are provided with heating plates (9).
8. The apparatus for detecting clenbuterol residual quantity in animal food according to claim 1, wherein: the first concentrator (203) is installed above the weak cation exchange column (2041).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011530626.5A CN114487221A (en) | 2020-12-22 | 2020-12-22 | Detection apparatus for clenbuterol residual quantity in survey animal food |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011530626.5A CN114487221A (en) | 2020-12-22 | 2020-12-22 | Detection apparatus for clenbuterol residual quantity in survey animal food |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117310157A (en) * | 2023-10-16 | 2023-12-29 | 青岛海润农大检测有限公司 | Device and method for detecting clenbuterol in animal food |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103616467A (en) * | 2013-11-25 | 2014-03-05 | 广东省中山市质量计量监督检测所 | Method for detecting residual tranquilizer medicines in meat product |
| CN205374398U (en) * | 2016-01-28 | 2016-07-06 | 甘肃国信润达分析测试中心 | Remain measurement of quantities system to clenbuterol among animal -derived food |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103616467A (en) * | 2013-11-25 | 2014-03-05 | 广东省中山市质量计量监督检测所 | Method for detecting residual tranquilizer medicines in meat product |
| CN205374398U (en) * | 2016-01-28 | 2016-07-06 | 甘肃国信润达分析测试中心 | Remain measurement of quantities system to clenbuterol among animal -derived food |
Non-Patent Citations (1)
| Title |
|---|
| 陈剑刚 等: "固相萃取-气质联用法分析肉食品中盐酸克伦特罗残留量", 《中国卫生检验杂志》, vol. 13, no. 6, 31 December 2003 (2003-12-31), pages 712 - 713 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117310157A (en) * | 2023-10-16 | 2023-12-29 | 青岛海润农大检测有限公司 | Device and method for detecting clenbuterol in animal food |
| CN117310157B (en) * | 2023-10-16 | 2024-02-13 | 青岛海润农大检测有限公司 | Device and method for detecting clenbuterol in animal food |
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