CN114264755B - Gas chromatography-triple quadrupole mass spectrometry detection method for residual amount of sulfonepyraflufen in plant-derived food - Google Patents
Gas chromatography-triple quadrupole mass spectrometry detection method for residual amount of sulfonepyraflufen in plant-derived food Download PDFInfo
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Abstract
The invention provides a gas chromatography-triple quadrupole mass spectrometry detection method for the residual amount of sulfure pyraflufen-ethyl in plant-derived food. According to the technical scheme, ethyl acetate is used for extraction, impurities are removed through ethylenediamine-N-propylsilanized silica gel, octadecyl bonded silica gel and anhydrous magnesium sulfate, centrifugal filtration is carried out, detection is carried out through a gas chromatography-triple quadrupole mass spectrometer, and the matrix matching external standard method is used for quantification. The experiment optimizes the extraction solvent, extraction mode, purification mode and instrument condition, inspects the influence of matrix effect, and determines the optimal pretreatment method and instrument condition. Under the optimized experimental conditions, the target compound has good linear relation in the range of 0.001-0.05mg/kg, and the correlation coefficient is more than 0.99. The average recovery of the blank sample at the low, medium and high 4 addition levels was 83.8% -104.3%, the relative standard deviation (n = 6) was 2.6% -6.7%, and the process quantitation limit was 0.001mg/kg. The method is simple, rapid and sensitive to operate, and can meet the detection requirement of the pyraflufen-ethyl in the plant-derived food.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, and particularly relates to a gas chromatography-triple quadrupole mass spectrometry detection method for residual amount of sulfure pyraflufen in plant-derived food.
Background
Sulfoxantrol (pyroxasulfone, code: KIH-485) is a novel broad-spectrum, highly active herbicide for pre-emergence soil treatment developed by Nippon combinatorico chemicals. The herbicide belongs to isoxazole herbicides and is a potential inhibitor of the biosynthesis of Very Long Chain Fatty Acids (VLCFAs) in plants. The application crops of the sulfonepyrazoxazole are wide, and the sulfonepyrazoxazole can be safely used for crops such as corn, cotton, peanut, wheat, sunflower, sorghum and the like; can effectively prevent and kill gramineous weeds of setaria, crabgrass and cockspur grass and broadleaf weeds of amaranthus, stramonium, solanum and abutilon. Sulfuron pyrazoxazole is considered to be the best medicament for preventing and killing drug-resistant weeds such as ryegrass in countries such as Australia. The pyraflufen-ethyl has the excellent characteristics of wide herbicidal spectrum, high activity, low dosage, good safety and the like, so that the pyraflufen-ethyl receives more and more extensive attention, in recent years, the pyraflufen-ethyl has been registered in countries such as Australia, america, canada and the like to carry out closed weeding in crop fields such as wheat, corn, soybean, cotton and the like, wherein the Australia sets out residual limit values in plant source foods such as corn, cereals, bean seeds, soybean (dried) and sunflower seeds, the residual limit values are as low as 0.01mg/kg, and at present, the pyraflufen-ethyl is gradually registered and popularized as the latest soil treatment agent in wheat fields in China.
Research aiming at the xaflufen-sodium is mainly focused on the aspects of herbicidal activity, environmental behavior and safety evaluation, and related reports at home and abroad are few for a residue analysis method of the xaflufen-sodium. Wuwengu and the like establish a method for detecting the residue of the pyriflufen-ethyl in soil and water by using a high performance liquid chromatography, but no report is found on an analysis method of the pyriflufen-ethyl in plant-derived foods such as cereals and the like. Therefore, the method for detecting and analyzing the residue of the sulfuryl pyraoxystrobin in the plant-derived food can make up the blank that the project in China has no detection method; has extremely important effects on the evaluation and management of the influence of the compound on human health and environmental safety and the prevention of the trade input and output risks.
Disclosure of Invention
The invention aims to provide a gas chromatography-triple quadrupole mass spectrometry detection method for the residual amount of the pyriftalid in plant-derived foods in order to solve the technical problem that an analysis method for the pyriftalid in plant-derived foods such as cereals is not established.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the gas chromatography-triple quadrupole mass spectrometry detection method for the residual amount of the sulfuryl pyraflufen in the plant-derived food comprises the following steps: crushing a plant source sample to be detected, and fully and uniformly mixing; weighing 5g of crushed sample, putting the sample into a 50mL polypropylene centrifuge tube, adding 3g of sodium chloride, 10mL of ethyl acetate and ceramic homogenous protons, and performing vortex oscillation extraction for 5min; centrifuging at 4000r/min for 3min; pipette 1.5mL of supernatant into a 2mL polypropylene centrifuge tube, add 20mg of PSA and 20mg of C 18 And 50mg anhydrous magnesium sulfate; vortex mixing for 1min, centrifuging at 12000r/min for 3min, and filtering the supernatant with 0.22 μm organic filter membrane; the test was then performed with the following instrument conditions:
DB-17MS capillary chromatographic column; column box temperature program: keeping the temperature at 70 ℃ for 0min, then heating to 230 ℃ at a speed of 20 ℃/min, and keeping the temperature for 0min; finally, heating to 310 ℃ at a speed of 30 ℃/min, and keeping for 1min; carrier gas: helium with purity not less than 99.999%, and flow rate of 1.0mL/min in constant flow mode; sample inlet temperature: 280 ℃; sample introduction amount: 1L; and (3) sample introduction mode: no shunt sampling; electron bombardment source: 70eV; ion source temperature: 230 ℃; transmission line temperature: 280 ℃; solvent retardation: 3min; multiple reaction monitoring mode.
Preferably, the retention time during the detection process is 8.71min, the quantitative ion pair and the collision energy thereof are 228.6/179.1 and 15eV respectively, the qualitative ion pair and the collision energy thereof are 178.6/159.0 and 15eV respectively, the regression equation is Y =3038.846525X-1470.727423, the correlation coefficient is 0.9997, the linear range is 0.001-0.05mg/kg, and the detection limit is 0.001mg/kg.
Preferably, the plant-derived sample to be tested is selected from one or several of the following components: rice, wheat, sorghum, corn, soybean, peanut, sweet potato, potato and sunflower seed.
Preferably, the DB-17MS capillary chromatographic column has a specification of 30m × 0.25mm × 0.25 μm.
Preferably, the method further comprises the following steps: several known matrix mix standard working solutions of the concentration of sulfonepyrazoxazole were prepared and standard curves were plotted.
Preferably, the matrix mixing standard working solution is prepared by the following method: sucking 100mg/L standard stock solution, preparing 1mg/L mixed standard solution by using ethyl acetate, storing at 0-4 ℃ in a dark place, and having the validity period of 1 month; sucking the mixed standard solution, and preparing matrix mixed standard working solutions with the concentrations of 0.5. Mu.g/L, 2. Mu.g/L, 5. Mu.g/L, 10. Mu.g/L and 25. Mu.g/L by using the blank sample extracting solution.
The invention provides a gas chromatography-triple quadrupole mass spectrometry detection method for the residual amount of sulfure pyraflufen-ethyl in plant-derived food. According to the technical scheme, the residue of the sulfure pyraoxystrobin in the rice, the wheat, the sorghum, the corn, the soybean, the peanut, the sweet potato, the potato and the sunflower seed is extracted by ethyl acetate, impurities are removed by ethylenediamine-N-propyl silanized silica gel, octadecyl bonded silica gel and anhydrous magnesium sulfate, the centrifugal filtration is carried out, the detection is carried out by a gas chromatography-triple quadrupole mass spectrometer, and the matrix matching external standard method is used for quantification. The experiment optimizes the extraction solvent, the extraction mode, the purification mode and the instrument condition, inspects the influence of the matrix effect and determines the optimal pretreatment method and the instrument condition. Under the optimized experimental conditions, the target compound has good linear relation in the range of 0.001-0.05mg/kg, and the correlation coefficient is larger than 0.99. The average recovery of the blank sample at the low, medium and high 4 addition levels was 83.8% -104.3%, the relative standard deviation (n = 6) was 2.6% -6.7%, and the method quantitation limit was 0.001mg/kg. The method is simple, rapid and sensitive to operate, and can meet the detection requirement of the sulfuryl pyraoxystrobin in the plant-derived food. According to the invention, by optimizing chromatographic conditions, the influence of the effects of extraction solvent types, purifying agents and matrix on the recovery rate is investigated, the QuEChERS-gas chromatography triple quadrupole mass spectrometry detection method of the pyriftalid is established, and a solid technical guarantee is provided for the detection of the pyriftalid residue in plant-derived products.
Drawings
FIG. 1 is a total ion flow diagram of sulfonepyrazoxazole.
FIG. 2 is an extracted ion MRM chromatogram of xaflufen.
FIG. 3 is a graph of extraction solution type versus average recovery.
FIG. 4 is a graph of the effect of different adsorbents on the extraction recovery of a spiked blank sample.
FIG. 5 is the matrix effect ME values for methyl isothiocyanate and dazomet in different samples.
FIG. 6 is the MRM chromatogram of a rice blank sample and a sample with a limit of quantitation (0.001 mg/kg) added with a standard.
FIG. 7 is the MRM chromatogram of a wheat blank sample and a limit of quantitation (0.001 mg/kg) spiked sample.
FIG. 8 is an MRM chromatogram of a sorghum blank sample and a limit of quantitation (0.001 mg/kg) spiked sample.
FIG. 9 is an MRM chromatogram of a corn blank sample and a limit of quantitation (0.001 mg/kg) spiked sample.
FIG. 10 is an MRM chromatogram of a soybean blank sample and a limit of quantitation (0.001 mg/kg) spiked sample.
FIG. 11 is an MRM chromatogram of a peanut blank sample and a limit of quantitation (0.001 mg/kg) spiked sample.
FIG. 12 is the MRM chromatogram of a sweet potato blank sample and a standard sample with a limit of quantitation (0.001 mg/kg).
FIG. 13 is an MRM chromatogram of a potato blank sample and a limit of quantitation (0.001 mg/kg) spiked sample.
FIG. 14 is an MRM chromatogram of a sunflower seed blank sample and a limit of quantitation (0.001 mg/kg) spiked sample.
Detailed Description
Hereinafter, specific embodiments of the present invention will be described in detail. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details. Approximating language, as used herein in the following examples, may be applied to represent quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
1. Reagent and apparatus
1.1 reagents
Anhydrous magnesium sulfate (analytically pure, calcined at 650 ℃ for 4h before use, for later use) and sodium chloride were purchased from national pharmaceutical group chemical reagents, inc.; hexane, acetone and ethyl acetate were chromatographically pure and available from TEDIA, USA. ethylenediamine-N-propylsilanized silica gel (PSA: 40-60 μm) and octadecyl-bonded silica gel (C) 18 : 40-60 μm) was purchased from Shanghai' an spectral laboratory science and technology Co., ltd. Microporous filter membrane: 0.22 μm, organic phase type, ceramic homogenous proton: 2cm (long) × 1cm (outer diameter). Sulfoxaden (C) 12 H 14 F 5 N 3 O 4 S, cas No. 447399-55-5), 100 μ g/mL, uncertainty ± 3% (k = 2) was purchased from Bepure corporation. Gas chromatography-triple quadrupole mass spectrometer (agilent 7000B, usa): equipped with electron bombardment source (EI), analytical balance: sensates 0.01g and 0.0001g (sydoris germany), disintegrator (shanghai jiading grain and oil instruments ltd.), vortex shaker (Talboys, usa), centrifuge: the rotating speed is not lower than 4000r/min (Ridgeon analytical instruments, inc. of Wuxi city), and the centrifugal machine: the rotating speed is not lower than 12000r/min (Hunan instrument centrifuge Co., ltd.).
1.2 Experimental methods
1.2.1 Standard solution preparation Standard solution: sucking a proper amount of 100mg/L standard stock solution, preparing 1mg/L mixed standard stock solution by using ethyl acetate, storing at 0-4 ℃ in a dark place, and keeping the effective period for 1 month.
Matrix mix standard working solution: sucking a proper amount of mixed standard solution, and preparing matrix mixed standard working solution with the concentration of 0.5 mu g/L, 2 mu g/L, 5 mu g/L, 10 mu g/L and 25 mu g/L by using the blank sample extracting solution, wherein the matrix mixed standard working solution is prepared for use.
1.2.2 QuEChERS pretreatment
Pulverizing plant-derived samples such as rice, wheat, corn and peanut, and mixing. Weighing 5g (accurate to 0.01 g) of crushed sample, putting the crushed sample into a 50mL polypropylene centrifuge tube, adding 3g of sodium chloride, 10mL of ethyl acetate and one ceramic homogeneous proton, and performing vortex oscillation extraction for 5min; n; centrifuging at 4000r/min for 3min. Accurately sucking 1.5mL of supernatant into a 2mL polypropylene centrifuge tube, adding 20mg of PSA and 20mg of C 18 And 50mg of anhydrous magnesium sulfate. Vortex mixing for 1min, centrifuging at 12000r/min for 3min, and filtering the supernatant with 0.22 μm organic filter membrane for determination.
1.2.3 apparatus conditions
DB-17MS capillary chromatography column (30 m × 0.25mm × 0.25 μm) column or equivalent; column box temperature program: keeping the temperature at 70 ℃ for 0min, then heating to 230 ℃ at a speed of 20 ℃/min, and keeping the temperature for 0min; finally, heating to 310 ℃ at a speed of 30 ℃/min, and keeping the temperature for 1min; carrier gas: helium with purity not less than 99.999%, and flow rate of 1.0mL/min in constant flow mode; sample inlet temperature: 280 ℃; sample introduction amount: 1 mu L of the solution; and (3) sample introduction mode: no shunt sampling; electron bombardment source: 70eV; ion source temperature: 230 ℃; transmission line temperature: 280 ℃; solvent retardation: 3min; multiple reaction monitoring mode: a pair of quantitative ions, a pair of qualitative ions, their retention times, their quantitative ion pairs, their qualitative ion pairs and their collision energies were selected, see table 1.
TABLE 1 Retention time, quantitative ion pair, qualitative ion pair, collision energy, regression equation, correlation coefficient, linear range, and quantitative limits for Sulfoxaden
2 results and discussion
2.1 conditions of the apparatus
2.1.1 selection of instruments
The research aims to establish a detection method for detecting and confirming the sulfonepyraflufen-ethyl, a gas chromatograph and a liquid chromatograph are abandoned when a detection instrument is selected, and only a high performance liquid chromatograph-tandem mass spectrometer and a triple quadrupole gas chromatograph-mass spectrometer with stronger qualitative ability are selected and tried. Firstly, carrying out parent ion scanning and daughter ion scanning on dazomet and methyl isothiocyanate according to a high performance liquid chromatography-tandem mass spectrometer method development program, and finding out that the parent ion 391.2 response of the sulfonepyrazoxazole is good through experiments, but the general response of the optimized column analysis peak type is poor, and the detection limit is high and cannot meet the requirements of related regulations; and finally, the high performance liquid chromatography-tandem mass spectrometry is abandoned for detecting the sulfuryl pyraflufen-ethyl, the triple quadrupole gas chromatograph-mass spectrometer can obtain a good peak pattern, the method sensitivity is high, and the triple quadrupole gas chromatograph-mass spectrometer is finally determined to be used for determining the residual quantity of the sulfuryl pyraflufen-ethyl in the plant-derived food.
2.1.2 Mass Spectrometry Condition optimization
Selecting 5mg/L standard solution of the sulfonepyrazoxazole for MS1 full scanning, selecting ions with higher response as parent ions, determining the parent ions 228.6 and 178.6 of the sulfonepyrazoxazole, then scanning the product ions of the corresponding parent ions, and selecting two groups with best signals as MRM quantitative and qualitative ion pairs. The total ion flow chart and the MRM chromatogram of the extraction ions of the sufonazole in the 0.01mg/L matrix standard solution are shown in figures 1 and 2.
2.2 optimization of the pretreatment method
2.2.1 selection of extraction mode and extraction solvent
In the experiment, n-hexane-acetone (9: 1, V/V), n-hexane-acetone (2: 1, V/V), n-hexane-acetone (7: 3, V/V) and ethyl acetate are selected as extraction solvents, a wheat sample added with 0.01mg/kg of sulfoxaflor is processed and put on a machine according to an experimental method of 1.2, the result is measured for 3 times in parallel, the type-average recovery rate relation graph of the obtained extraction solution is shown in figure 3, the result shows that the five extraction solvents have good extraction efficiency on the sulfoxaflor, the color of the extraction solution is seen, the color of the mixed solvent extraction solution containing acetone is slightly dark, the extraction efficiency is increased along with the increase of the content of the acetone, and the ethyl acetate is finally selected as the extraction solvent from the aspects of environmental protection, cost reduction and simple and convenient operation.
2.2.2 selection of purification mode
Ethylene diamine-N-propyl silanized silica gel (PSA) is a weak anion exchange adsorbent and can effectively remove organic acid in a samplePolar pigments, fatty acids, sugars and other components capable of forming hydrogen bonds; octadecylsilane chemically bonded silica (C) 18 ) Can remove nonpolar compounds such as volatile oil, terpenes, lignin, lipids, carotenoid, etc., and anhydrous magnesium sulfate can remove water in the sample solution. The QuEChERS method typically uses a combination of PSA, C18 and anhydrous magnesium sulfate for pre-treatment decontamination of grain and oil samples to remove impurities and moisture from the sample solution. In order to make the experimental process as simple and rapid as possible, the pretreatment process is carried out by adopting a mode of one-time extraction without concentration and QuEChERS purification. Experiment researches PSA and C 18 And anhydrous MgSO 4 The recovery rate of the three substances after adsorbing the standard solution of the sulfuryl pyraflufen-ethyl. Weighing 50mg of different adsorbents in a 1.5mL bullet centrifuge tube, adding 1mL of 0.01mg/L mixed standard solution, performing vortex oscillation for 2min, centrifuging for 2min at 12000r/min, filtering the supernate with a 0.22 mu m organic filter membrane, and performing detection on the supernate on a machine. Three parallel adsorbents are made, the average recovery rate is calculated, and the experimental result shows that the PSA and the C are 18 Anhydrous MgSO (MgSO) 4 The adsorption recovery rate of the pyraflufen-ethyl to the pyraflufen-ethyl is between 95 and 105 percent; shows that none of the three substances can cause the adsorption of the sulfuryl pyraflufen-ethyl.
2.2.3 determination of the Combined amounts of adsorbents
When a plant-derived sample is extracted and purified by the QuEChERS method, two or more adsorption purifiers are usually used to better remove impurities which interfere with the analysis of an instrument, such as organic acids, lipids, saccharides and the like in the sample. Three groups of adsorbents (I: 10mgPSA + 10mgC) are compounded in the experiment 18 +50mg of anhydrous MgSO 4 ，II：20mgPSA+20mgC 18 +50mg of anhydrous MgSO 4 ，III：50mgPSA+50mgC 18 +50mg of anhydrous MgSO 4 ) A0.02 mg/kg standard addition recovery experiment is carried out on a wheat blank sample, the combined purification effect of different adsorbents is inspected, and the experiment result is shown in figure 4. The experimental result shows that the three groups of compounded adsorbent combinations can meet the requirement of experimental recovery rate, and the recovery rate ranges from 90% to 110%; from the actual purification effect, after impurity removal and purification by the combination of II and III type adsorbents, the purification effect is better, and the influence on target pesticides is smaller. Comprehensively considering the purifying effect, cost, convenience and appearanceThe interfering impurities and the baseline are selected to be 20mgPSA +20mgC during analysis by the analyzer 18 +50mg of anhydrous MgSO 4 And determining the type and the dosage of the compound adsorption purifying agent for the final experiment.
2.2.4 Effect of the matrix Effect
Matrix Effects (ME) are the co-extraction of a sample of a substance to be detected, which can enhance or inhibit the detection response of the substance to be detected, thereby affecting the accuracy and precision of the detection result. The matrix effect is mainly expressed as a matrix-induced chromatographic response enhancement phenomenon in a gas phase system, namely, a matrix enhancement effect. When the Matrix effect is greatly influenced, the sensitivity of the method is reduced, the accuracy of the method is influenced, and errors are brought to measurement, so Matrix Effects (ME) need to be evaluated in the process of developing and confirming the method. The matrix effect is related to the types of matrixes, the content of matrix interferents, the characteristics of analytes, chromatographic separation conditions, ion source designs of different instruments and the like, and can be quantitatively evaluated according to the following formula: matrix effect (ME,%) = [ (slope of matrix matching calibration curve/slope of pure solvent standard curve) -1] × 100. The weak substrate effect is that less than 20 percent of ME, and can be ignored without adopting compensation measures; medium substrate effect is obtained when ME is more than or equal to 20% and less than or equal to 50%, strong substrate effect is obtained when ME is more than 50%, and measures are taken to compensate the substrate effect. Test A blank matrix solution was prepared according to the pretreatment method of 1.2.2, and a standard working solution and a matrix matching standard working solution were prepared according to the method of 1.2.1. The calculation of the matrix effect in different matrices according to the above formula is shown in figure 5.
As can be seen from FIG. 5, the matrix effect of the xaflufen in 8 matrices is moderate and it should be considered to take measures to compensate the matrix effect. In the pesticide residue analysis and detection process, the influence of matrix effect on the quantitative result can be overcome by adopting the matrix matching standard solution for quantitative analysis. National standards GB/T20769-2008 and GB 23200.113-2018 and the like for detecting pesticide residues in plant-derived foods in China all stipulate a quantitative method for a matrix matching standard solution, and the European Union recommends the use of the matrix matching standard solution for quantitative analysis in an instructive document SANTE/12682/2019 of a method for analyzing pesticide residues in foods. However, for a wide variety of sample matrices, the detection efficiency is greatly reduced during the process of preparing a matrix-matched standard solution. As can be seen from FIG. 5, the matrix effect difference among different types of samples is small, so in practical operation, wheat can be selected as a representative matrix to prepare a matrix matching standard working solution, the matrix effect is overcome, and the detection efficiency is improved on the premise of ensuring the quantitative accuracy and stability.
2.3 methodological validation
2.3.1 Linear Range, correlation coefficient and method detection Limit
Preparing a series of sulphone pyrazoxazole matching standard working solutions with the concentrations of 0.5 mu g/L, 2 mu g/L, 5 mu g/L, 10 mu g/L, 20 mu g/L and 25 mu g/L by using a blank substrate solution, detecting according to 1.2.3 sample injection, and drawing a substrate standard working curve by taking the concentration (X, ng/mL) of the sulphone pyrazoxazole as a horizontal coordinate and taking the peak area of the sulphone pyrazoxazole as a vertical coordinate to obtain a linear equation and a correlation coefficient; the appropriate amount of standard solution was added to the blank sample solution and the limit of quantitation (LOQ) was determined as S/N =10, and the data is shown in table 1.
2.3.2 recovery
Standard addition and recovery experiments with different concentrations are respectively carried out on blank samples of rice, wheat, sorghum, corn, soybean, peanut, sweet potato, potato and sunflower seed, the standard addition and recovery experiments cover the limit of quantitation, the main MRL value is obtained, each standard addition level is measured for 6 times, the parallel results are obtained, and the experimental data of the addition concentration and the recovery rate of the pyraflufen-ethyl in the plant source samples are shown in a table 2.
Table 2 normalized recovery and relative standard deviation of xaflufen in different samples (n = 6)
2.4 actual sample detection
The method is used for detecting 50 rice, wheat, sorghum, corn, soybean, peanut, sweet potato, potato and sunflower seeds, and the detection results are all undetected.
3 conclusion
The method for detecting the residual quantity of the sulfure pyraflufen in the plant source food by the gas chromatography triple quadrupole mass spectrometry is established for the first time, under the optimized experimental condition, the linear relation of a target compound in the range of 0.001-0.05mg/kg is good, and the correlation coefficient is larger than 0.99. The average recovery rate of the blank sample under 4 addition levels of low, medium and high levels is 83.8% -104.3%, the relative standard deviation (n = 6) is 2.6% -6.7%, the quantitative limit of the method is 0.001mg/kg, the method has high sensitivity, simple operation, rapidness, accuracy and low cost, and can meet the detection requirement of the residual sulfuryl pyraoxystrobin in the plant-derived food.
The embodiments of the present invention have been described in detail, but the description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. Any modification, equivalent replacement, and improvement made within the scope of the application of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The gas chromatography-triple quadrupole mass spectrometry detection method for the residual amount of the sulfuryl pyraflufen in the plant-derived food is characterized by comprising the following steps of: crushing a plant-derived food sample to be detected, and fully and uniformly mixing; weighing 5g of crushed sample, putting the sample into a 50mL polypropylene centrifuge tube, adding 3g of sodium chloride, 10mL of ethyl acetate and ceramic homogenous protons, and performing vortex oscillation extraction for 5min;4000 Centrifuging for 3min at r/min; pipette 1.5mL of supernatant into a 2mL polypropylene centrifuge tube, add 20mg of PSA and 20mg of C 18 And 50mg anhydrous magnesium sulfate; vortex mixing for 1min, centrifuging at 12000r/min for 3min, and filtering the supernatant with 0.22 μm organic filter membrane; the test was then performed with the following instrument conditions:
DB-17MS capillary chromatography column; column box temperature program: 70. keeping the temperature for 0min, then heating to 230 ℃ at a speed of 20 ℃/min, and keeping the temperature for 0min; finally, heating to 310 ℃ at a speed of 30 ℃/min, and keeping for 1min; carrier gas: helium with purity not less than 99.999%, and flow rate of 1.0mL/min in constant flow mode; sample inlet temperature: 280 ℃; sample injection amount: 1L; and (3) sample introduction mode: no-shunt sample introduction; electron bombardment source: 70eV; ion source temperature: 230 ℃; transmission line temperature: 280 ℃; solvent retardation: 3min; a multiple reaction monitoring mode;
the retention time in the detection process is 8.71min, the quantitative ion pair and the collision energy thereof are 228.6/179.1 and 15eV respectively, and the qualitative ion pair and the collision energy thereof are 178.6/159.0 and 15eV respectively;
the plant-derived food sample to be detected is selected from rice, wheat, sorghum, corn, soybean, peanut, sweet potato, potato and sunflower seed;
DB-17MS capillary column specification of 30m x 0.25mm x 0.25 μm.
2. The gas chromatography-triple quadrupole mass spectrometry detection method for the residual amount of sulfuryl pyraflufen in plant-derived foods as claimed in claim 1, wherein the regression equation is Y =3038.846525X-1470.727423, the correlation coefficient is 0.9997, the linear range is 0.001-0.05mg/kg, and the detection limit is 0.001mg/kg.
3. The gas chromatography-triple quadrupole mass spectrometry detection method for the residual amount of sulfuryl pyraflufen-ethyl in plant-derived food as claimed in claim 1, further comprising the steps of: several known matrix mix standard working solutions of the concentration of sulfonepyrazoxazole were prepared and standard curves were plotted.
4. The gas chromatography-triple quadrupole mass spectrometry detection method for the residual amount of sulfuryl pyraflufen in plant-derived food as claimed in claim 3, wherein the matrix mixed standard working solution is prepared by the following method: absorbing 100mg/L standard stock solution, preparing 1mg/L mixed standard solution by using ethyl acetate, storing at 0-4 ℃ in a dark place, and having the validity period of 1 month; sucking the mixed standard solution, and preparing matrix mixed standard working solution with the concentrations of 0.5. Mu.g/L, 2. Mu.g/L, 5. Mu.g/L, 10. Mu.g/L and 25. Mu.g/L by using the blank food sample extract.
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| WO2020118754A1 (en) * | 2018-12-14 | 2020-06-18 | 青岛清原化合物有限公司 | Ternary weeding composition containing pyroxasulfone and use thereof |
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| WO2020118754A1 (en) * | 2018-12-14 | 2020-06-18 | 青岛清原化合物有限公司 | Ternary weeding composition containing pyroxasulfone and use thereof |
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