CN112285254B - Method for determining residual quantity of sulfonylurea herbicide in aquatic product - Google Patents
Method for determining residual quantity of sulfonylurea herbicide in aquatic product Download PDFInfo
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- CN112285254B CN112285254B CN202011202474.6A CN202011202474A CN112285254B CN 112285254 B CN112285254 B CN 112285254B CN 202011202474 A CN202011202474 A CN 202011202474A CN 112285254 B CN112285254 B CN 112285254B
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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
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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Abstract
The invention discloses a method for measuring residual quantity of sulfonylurea herbicide in aquatic products, which comprises the following steps: A. crushing the hard sample; B. adding 35wt% of acetonitrile water solution into the crushed sample, and stirring to obtain a suspension, wherein the mass ratio of the sample to the acetonitrile water solution is 1; C. injecting the suspension into an extractor through a pressure pump to extract effective components in the sample; D. drying the extract, and dissolving the dried residue with acetonitrile to obtain a sample to be detected; E. performing isocratic elution on a sample to be detected by using a liquid chromatographic column; F. and (4) performing mass spectrometry on the eluate by using a mass spectrometer to obtain a detection result. The invention can improve the defects of the prior art and improve the dissolution efficiency of the extraction solution on the effective substances in the hard sample powder.
Description
Technical Field
The invention relates to the technical field of pesticide residue detection, in particular to a method for determining residual quantity of sulfonylurea herbicide in aquatic products.
Background
The detection of the residual amount of the sulfonylurea herbicide in the aquatic products usually adopts a mass spectrometry mode, and in order to ensure the accuracy of the mass spectrometry, a detected substance needs to be fully dissolved in an extraction solution. When the sample to be detected is a hard sample (such as a shell, a scale and the like), the extraction solution still cannot rapidly and sufficiently dissolve out the effective substances in the hard sample powder, so that the detection error is large.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for measuring the residual quantity of sulfonylurea herbicides in aquatic products, which can solve the defects of the prior art and improve the dissolution efficiency of an extraction solution on effective substances in hard sample powder.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
A method for measuring residual quantity of sulfonylurea herbicide in aquatic products comprises the following steps:
A. crushing a hard sample;
B. adding 35wt% of acetonitrile water solution into the crushed sample, and stirring to obtain a suspension, wherein the mass ratio of the sample to the acetonitrile water solution is 1;
C. injecting the suspension into an extractor through a pressure pump, and extracting effective components in the sample;
D. drying the extract, and dissolving the dried residue by using acetonitrile to prepare a sample to be detected;
E. performing isocratic elution on a sample to be detected by using a liquid chromatographic column;
F. and (4) carrying out mass spectrum analysis on the eluate by using a mass spectrometer to obtain a detection result.
Preferably, the extractor includes a jar body, rotating electrical machines is installed to jar body bottom, rotating electrical machines's rotation axis is connected with the rotary disk, jar body top is fixed with the fixed disk, rotary disk and fixed disk sliding contact cooperation, the heart is provided with a plurality of annular groove on the rotary disk, be provided with down the grinding bed between the adjacent annular groove, the center of fixed disk is provided with the feed liquor pipe, be provided with the last grinding bed that contacts with lower grinding bed on the fixed disk, be provided with the filter screen with the annular groove one-to-one on the fixed disk, the filter screen is laminated with the lateral wall slip that corresponds the annular groove, the mesh number of different filter screens is increased by the inboard outside gradually.
Preferably, the inner edge of the upper polishing layer is provided with a bevel portion.
Preferably, the height of the contact surface between the upper polishing layer and the lower polishing layer gradually decreases from the inside to the outside.
Preferably, the bottom surface of the annular groove is provided with a V-shaped guide plate, the top end of the V-shaped guide plate faces the rotating direction of the lower grinding layer, two sides of the V-shaped guide plate are respectively provided with a first through hole, and the axes of the two first through holes are not parallel to each other.
Preferably, the height of one side of the V-shaped guide plate close to the inner side of the annular groove is smaller than that of the other side of the V-shaped guide plate.
Adopt the beneficial effect that above-mentioned technical scheme brought to lie in: the invention adopts a detection mode of combining a chromatographic column and a mass spectrometer to detect pesticide residues on a sample. In order to ensure the full dissolution of the active ingredients in the suspension, the extractor is provided with the rotating disc and the fixed disc which can rotate relatively, a grinding type extraction mode is adopted, and the sample particles are secondarily crushed by the grinding process during extraction, so that the sample particles can generate a new contact surface which is contacted with the extraction liquid, and the dissolution efficiency of the active ingredients is greatly accelerated. The extraction device adopts multi-stage grinding in the extraction process, and each stage of grinding mechanism is separated by a filter screen, so that the grinding efficiency can be effectively improved. The annular groove is used for mixing the suspension subjected to the previous grinding for the second time, so that the treatment effect of the next grinding is ensured. The inclined plane part at the inner edge of the upper grinding layer is used for guiding suspension, and the inclined grinding contact surface is matched, so that the ground particles can uniformly move to the outer side of the grinding area, and the aggregation of sample particles in the grinding area is avoided. The V-shaped guide plate can push and guide the mixed suspension to two sides of the annular groove in the rotating process of the rotating disk, and the mixed suspension is blocked by the side wall of the annular groove, so that the mixed suspension generates an inner vertical circulation area and an outer vertical circulation area in the annular groove. Meanwhile, the first through hole can form a turbulent flow area at the bottom of the V-shaped guide plate, so that the mixing uniformity of the sample particles in the suspension is improved. The V-shaped guide plate adopts the design of unequal height, so that the interference of the whole outward flowing trend of the suspension on the vertical circulation of the suspension can be reduced.
Drawings
FIG. 1 is a block diagram of an extractor according to one embodiment of the present invention.
FIG. 2 is an enlarged partial view of the interface of the upper abrasive layer and the lower abrasive layer in accordance with one embodiment of the present invention.
Fig. 3 is a top view of a V-shaped baffle in an embodiment of the present invention.
In the figure: 1. a tank body; 2. a rotating electric machine; 3. rotating the disc; 4. fixing the disc; 5. an annular groove; 6. a lower polishing layer; 7. a liquid inlet pipe; 8. an upper polishing layer; 9. filtering with a screen; 10. an inclined plane part; 11. a V-shaped guide plate; 12. a first through hole; 13. a second through hole; 14. and (4) sealing plugs.
Detailed Description
The standard parts used in the invention can be purchased from the market, the special-shaped parts can be customized according to the description and the description of the attached drawings, and the specific connection mode of each part adopts the conventional means of mature bolts, rivets, welding, sticking and the like in the prior art, and the detailed description is not repeated.
A method for measuring residual quantity of sulfonylurea herbicide in aquatic products comprises the following steps:
A. crushing a hard sample;
B. adding 35wt% of acetonitrile water solution into the crushed sample, and stirring to obtain a suspension, wherein the mass ratio of the sample to the acetonitrile water solution is 1;
C. injecting the suspension into an extractor through a pressure pump, and extracting effective components in the sample;
D. drying the extract, and dissolving the dried residue by using acetonitrile to prepare a sample to be detected;
E. performing isocratic elution on a sample to be detected by using a liquid chromatographic column;
F. and (4) carrying out mass spectrum analysis on the eluate by using a mass spectrometer to obtain a detection result.
Referring to fig. 1-3, the extractor includes a jar body 1, rotating electrical machines 2 are installed to jar body 1 bottom, rotating electrical machines 2's rotation axis is connected with rotary disk 3, jar body 1 top is fixed with fixed disk 4, rotary disk 3 and the cooperation of fixed disk 4 sliding contact, be provided with a plurality of annular groove 5 on the rotary disk 3 with the heart, be provided with down grinding coat 6 between the adjacent annular groove 5, the center of fixed disk 4 is provided with feed liquor pipe 7, be provided with the last grinding coat 8 that contacts with lower grinding coat 6 on the fixed disk 4, be provided with the filter screen 9 with annular groove 5 one-to-one on the fixed disk 4, filter screen 9 and the lateral wall that corresponds annular groove 5 slide the laminating, the mesh number of different filter screens is increased outside by inboard gradually. The inner edge of the upper polishing layer 8 is provided with a bevel 10. The height of the contact surface between the upper polishing layer 8 and the lower polishing layer 6 gradually decreases from the inside to the outside. The bottom surface of the annular groove 5 is provided with a V-shaped guide plate 11, the top end of the V-shaped guide plate 11 faces the rotating direction of the lower grinding layer 6, two sides of the V-shaped guide plate 11 are respectively provided with a first through hole 12, and the axes of the two first through holes 12 are not parallel to each other. The height of one side of the V-shaped guide plate 11 close to the inner side of the annular groove 5 is less than that of the other side.
In addition, a plurality of second through holes 13 are also arranged on the fixed disk 4, and the tops of the second through holes 13 are inserted with sealing plugs 14. When the effective substances cannot be fully dissolved out through liquid inlet grinding extraction, the sealing plug 14 can be taken down, the rotating motor 2 is restarted, and the suspension is circularly ground and extracted.
In the embodiment, the liquid chromatographic column adopts Shimadzurintsil ods-3, the mobile phase of the elution process adopts eluent with the molar ratio of acetonitrile to formic acid being 1. The specific operation of liquid chromatography columns and mass spectrometers is well known in the art and will not be described in detail herein.
The invention can effectively extract various types of hard sample particles and has wide application range.
In the description of the present invention, it is to be understood that the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, are merely for convenience of description of the present invention, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (1)
1. A method for determining residual quantity of sulfonylurea herbicide in aquatic products is characterized by comprising the following steps:
A. crushing the hard sample;
B. adding 35wt% of acetonitrile water solution into the crushed sample, and stirring to obtain a suspension, wherein the mass ratio of the sample to the acetonitrile water solution is 1;
C. injecting the suspension into an extractor through a pressure pump, and extracting effective components in the sample;
D. drying the extract, and dissolving the dried residue with acetonitrile to obtain a sample to be detected;
E. performing isocratic elution on a sample to be detected by using a liquid chromatographic column;
F. performing mass spectrometry on the eluate by using a mass spectrometer to obtain a detection result;
the extractor comprises a tank body (1), a rotating motor (2) is installed at the bottom of the tank body (1), a rotating shaft of the rotating motor (2) is connected with a rotating disk (3), a fixed disk (4) is fixed at the top of the tank body (1), the rotating disk (3) is in sliding contact fit with the fixed disk (4), a plurality of annular grooves (5) are concentrically arranged on the rotating disk (3), lower grinding layers (6) are arranged between adjacent annular grooves (5), a liquid inlet pipe (7) is arranged at the center of the fixed disk (4), upper grinding layers (8) which are in contact with the lower grinding layers (6) are arranged on the fixed disk (4), filter screens (9) which are in one-to-one correspondence with the annular grooves (5) are arranged on the fixed disk (4), the filter screens (9) are in sliding fit with the outer side walls of the corresponding annular grooves (5), and the mesh number of different filter screens is gradually increased from the inner side to the outer side; the inner side edge of the upper grinding layer (8) is provided with an inclined plane part (10); the height of the contact surface of the upper grinding layer (8) and the lower grinding layer (6) is gradually reduced from the inner side to the outer side; the bottom surface of the annular groove (5) is provided with a V-shaped guide plate (11), the top end of the V-shaped guide plate (11) faces the rotating direction of the lower grinding layer (6), two sides of the V-shaped guide plate (11) are respectively provided with a first through hole (12), and the axes of the two first through holes (12) are not parallel to each other; the height of one side of the V-shaped guide plate (11) close to the inner side of the annular groove (5) is smaller than that of the other side.
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| CN202011202474.6A CN112285254B (en) | 2020-11-02 | 2020-11-02 | Method for determining residual quantity of sulfonylurea herbicide in aquatic product |
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| CN202011202474.6A CN112285254B (en) | 2020-11-02 | 2020-11-02 | Method for determining residual quantity of sulfonylurea herbicide in aquatic product |
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| CN112285254A CN112285254A (en) | 2021-01-29 |
| CN112285254B true CN112285254B (en) | 2022-10-14 |
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| CN115494180B (en) * | 2022-10-08 | 2024-02-27 | 石家庄市畜产品和兽药饲料质量检测中心 | Method for measuring residual quantity of nicosulfuron in aquatic product |
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| WO2006125644A1 (en) * | 2005-05-24 | 2006-11-30 | Basf Aktiengesellschaft | Method for determining pesticide residues in soil or plant material |
| CN102128901A (en) * | 2010-12-20 | 2011-07-20 | 天津市农业科学院中心实验室 | Method for processing ginseng sample containing sulfonylurea pesticide residue before measurement |
| CN105699550A (en) * | 2016-02-26 | 2016-06-22 | 环境保护部南京环境科学研究所 | Analysis method applied to measuring residual quantity of sulfonylurea herbicide in plants |
| CN109024046A (en) * | 2018-07-04 | 2018-12-18 | 盐城康鼎机械有限公司 | A kind of centrifugal pulper of paper plastic-aluminum composite packing slurrying |
| CN209967741U (en) * | 2019-05-17 | 2020-01-21 | 山东省农业科学院农产品研究所 | Gardenoside is leached with drawing jar |
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2020
- 2020-11-02 CN CN202011202474.6A patent/CN112285254B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2006125644A1 (en) * | 2005-05-24 | 2006-11-30 | Basf Aktiengesellschaft | Method for determining pesticide residues in soil or plant material |
| CN102128901A (en) * | 2010-12-20 | 2011-07-20 | 天津市农业科学院中心实验室 | Method for processing ginseng sample containing sulfonylurea pesticide residue before measurement |
| CN105699550A (en) * | 2016-02-26 | 2016-06-22 | 环境保护部南京环境科学研究所 | Analysis method applied to measuring residual quantity of sulfonylurea herbicide in plants |
| CN109024046A (en) * | 2018-07-04 | 2018-12-18 | 盐城康鼎机械有限公司 | A kind of centrifugal pulper of paper plastic-aluminum composite packing slurrying |
| CN209967741U (en) * | 2019-05-17 | 2020-01-21 | 山东省农业科学院农产品研究所 | Gardenoside is leached with drawing jar |
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