CN116183766A - Method for detecting multiple residues of herb tea pesticides and adsorption purification composition used by method - Google Patents
Method for detecting multiple residues of herb tea pesticides and adsorption purification composition used by method Download PDFInfo
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- CN116183766A CN116183766A CN202310156703.2A CN202310156703A CN116183766A CN 116183766 A CN116183766 A CN 116183766A CN 202310156703 A CN202310156703 A CN 202310156703A CN 116183766 A CN116183766 A CN 116183766A
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000000575 pesticide Substances 0.000 title claims abstract description 42
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 38
- 238000000746 purification Methods 0.000 title claims abstract description 37
- 239000000203 mixture Substances 0.000 title claims abstract description 33
- 241001122767 Theaceae Species 0.000 title claims description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 30
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 30
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 30
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 21
- 235000015092 herbal tea Nutrition 0.000 claims abstract description 18
- 238000004458 analytical method Methods 0.000 claims abstract description 15
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- 239000000447 pesticide residue Substances 0.000 claims abstract description 13
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- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 10
- XBJFCYDKBDVADW-UHFFFAOYSA-N acetonitrile;formic acid Chemical compound CC#N.OC=O XBJFCYDKBDVADW-UHFFFAOYSA-N 0.000 claims description 10
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- 238000004885 tandem mass spectrometry Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 8
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- MNHVNIJQQRJYDH-UHFFFAOYSA-N 2-[2-(1-chlorocyclopropyl)-3-(2-chlorophenyl)-2-hydroxypropyl]-1,2-dihydro-1,2,4-triazole-3-thione Chemical compound N1=CNC(=S)N1CC(C1(Cl)CC1)(O)CC1=CC=CC=C1Cl MNHVNIJQQRJYDH-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
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- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 6
- 239000005825 Prothioconazole Substances 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
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- 241000628997 Flos Species 0.000 description 1
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- 125000003277 amino group Chemical group 0.000 description 1
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- 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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- 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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- 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
- G01N30/14—Preparation by elimination of some components
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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
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Abstract
A method for detecting multi-residue of herb tea pesticides and an adsorption purification composition used by the method are provided, wherein the adsorption purification composition comprises graphite-phase carbon nitride, crosslinked polyvinylpyrrolidone, octadecyl bonded silica gel, N-propylethylenediamine and anhydrous magnesium sulfate. The method solves the technical problem of serious interference of pesticide multi-residue pretreatment matrixes in complex matrixes of the herbal tea, can effectively remove impurities such as pigment, polyphenol, organic acid, aromatic oil and the like, is used for rapidly extracting, purifying and accurately qualitatively quantifying pesticide multi-residues in the herbal tea such as safflower, chrysanthemum and rose, has the advantages of less reagent consumption, good purifying effect, low matrix effect, high sensitivity, high accuracy and high analysis speed, and can meet the detection requirements of various pesticide residues in the herbal tea.
Description
Technical Field
The invention belongs to the technical field of food pesticide residue detection, and particularly relates to a method for detecting multiple residues of a flower grass tea pesticide and an adsorption purification composition used by the method.
Background
Pesticide residue analysis is an analytical technique for trace components in complex mixtures. The method has the advantages of less sample consumption, less reagent consumption, less matrix interference, high detection flux and high analysis speed, and is a development trend of pesticide chemical pollutant residue detection technology. Traditional detection methods are time-consuming and are limited in practical application to single-component detection in most cases. The development of the multi-residue rapid detection technology for pesticides can overcome the limitations of the traditional method at present, and realize rapid, sensitive and multi-component simultaneous detection of the pesticides.
QuEChERS (Quick, easy, cheap, effective, rugged, safe) is a rapid sample pretreatment technology for pesticide multi-residue detection, which is developed internationally in recent years, and the principle is that impurities in a matrix are adsorbed by utilizing interaction of adsorbent filler and the impurities in the matrix, so that the purposes of impurity removal and purification are achieved. The QuEChERS pretreatment technology has the advantages of simple operation, short analysis time, less solvent consumption, less pollution and low cost, and is suitable for rapid detection. But the selection and dosage proportion of the adsorbent are critical, and unsuitable purification not only causes larger matrix effectIt should be noted that the detection limit, selectivity and accurate quantification of the test results of the method also have an impact, while also increasing the maintenance costs of the instrument. The adsorbent packing currently used consists mainly of octadecyl bonded silica gel (C 18 ) N-Propylethylenediamine (PSA), graphitized Carbon Black (GCB) and anhydrous magnesium sulfate (MgSO) 4 ) Etc. C (C) 18 Has strong adsorption effect on nonpolar compounds and is often used for removing nonpolar compounds in polar solution. PSA adsorbs and eliminates sugars, pigments, and fatty acids in the sample matrix by weak ion exchange of amine groups and formation of hydrogen bonds with polar matrix components. GCB has strong adsorption effect on impurities, but also has certain adsorption effect on nonpolar pesticides and substances with plane structures. Anhydrous MgSO 4 Are often used as basic water scavengers for aqueous samples. At present, quEChERS technology is generally used by mixing different adsorbent fillers in different proportions as an adsorption purification composition, for example, national standards such as GB23200.113-2018, GB 23200.121-2021 and the like all adopt QuEChERS pretreatment technology, and the used adsorption purification composition comprises C 18 PSA, GCB and anhydrous MgSO 4 Different proportions are adopted for different matrixes.
The flower and grass tea substrate is complex, contains a large amount of impurities such as pigment, polyphenol, organic acid, aromatic oil and the like, is quite different from the content of the residual target compound, and is a difficulty in the whole pretreatment process, namely how to effectively remove the impurities and realize pesticide multi-residue analysis at the same time and ensure good recovery rate. The traditional QuEChERS method is not very sufficient for purifying herb tea and the like, has large interference, and particularly causes a large amount of non-polar pesticide with a planar structure to be lost when the GCB is used for a sample with more pigment content, so that the recovery rate is low. The invention develops porous graphite phase carbon nitride (g-C) 3 N 4 ) And porous cross-linked polyvinylpyrrolidone (PVPP) adsorption material, and provides a novel adsorption purification composite agent and an application scheme thereof in detecting multi-residue of herb tea pesticides. Porous g-C 3 N 4 Has excellent effect in adsorbing safflower red and other pigment, and the porous PVPP is favorable to eliminating polyphenol impurity and has no non-polar and planar pesticideAdsorption effect. The novel adsorption purification composite agent is suitable for rapid sample pretreatment for pesticide multi-residue detection in flower and grass tea, and can be applied to simultaneous detection of pesticide multi-residue including nonpolar pesticides with planar structures.
Disclosure of Invention
The invention aims to provide a method for detecting multi-residue of a flower and grass tea pesticide and an adsorption purification composition used by the method.
To achieve the above and other related objects, the present invention provides the following technical solutions: an adsorption purification composition comprising graphite phase carbon nitride, cross-linked polyvinylpyrrolidone, octadecyl bonded silica gel, N-propylethylenediamine and anhydrous magnesium sulfate.
The preferable technical scheme is as follows: the graphite phase carbon nitride is porous graphite phase carbon nitride, and the preparation method comprises the following steps: mixing urea and ammonium bicarbonate in mortar, grinding, mixing, and placing in alumina crucible with cover at 5-8deg.C for min -1 Heating to 75-85deg.C, maintaining at 75-85deg.C for 1-2 hr, and then heating at 5-8deg.C for 5-min -1 Heating to 550-600 deg.C, maintaining at the temperature for 2-3 hr, and naturally cooling to room temperature to obtain porous g-C 3 N 4 A material.
The preferable technical scheme is as follows: the crosslinked polyvinylpyrrolidone is porous crosslinked polyvinylpyrrolidone, and the preparation method comprises the following steps: adding 50-70wt% of N-vinyl pyrrolidone, 8-35wt% of water into a nitrogen-protected container, then adding 0.5wt% -1wt% of sodium hydroxide and 1-2wt% of divinylbenzene, 8-30wt% of N-hexane, introducing nitrogen and stirring; heating to 80-120 ℃, and reacting at constant temperature for 3-5 hours to obtain crosslinked polyvinylpyrrolidone swelling particles; washing, filtering, soaking in methanol, filtering, vacuum drying to constant weight, and grinding to obtain porous cross-linked polyvinylpyrrolidone.
To achieve the above and other related objects, the present invention provides the following technical solutions: a method for detecting multi-residue of a herb tea pesticide comprises the following steps:
step 1: placing a herbal tea sample to be detected in a brown centrifuge tube with a plug, adding an ascorbic acid aqueous solution, mixing uniformly by vortex, adding an acetonitrile formate solution, and extracting by vortex oscillation; adding sodium chloride into the brown centrifuge tube, carrying out vortex oscillation, centrifuging at 0-6 ℃, and taking supernatant;
the adsorption purification composition adopts the adsorption purification composition according to any one of claims 1 to 3;
the dosage ratio of the supernatant to the adsorption purification composition agent is as follows: 1mL of supernatant corresponds to 50-200mg of porous graphite phase carbon nitride, 50-100mg of porous crosslinked polyvinylpyrrolidone, 50-100mg of octadecyl bonded silica gel, 50-100mg of N-propylethylenediamine and 150-200mg of anhydrous magnesium sulfate. When the pesticide residue contains prothioconazole and a metabolite of the prothioconazole, the dosage of N-propyl ethylenediamine is less than 50mg.
The preferable technical scheme is as follows: in the step 1, 1-2g of herbal tea sample to be measured is weighed and placed in a brown centrifuge tube with a plug, an ascorbic acid aqueous solution with the mass of 2 times that of the herbal tea sample to be measured and the concentration of 15 mug/mL is added and mixed uniformly by vortex, and then a formic acid acetonitrile solution with the volume concentration of 5-10mL and the concentration of 1% is added, and the mixture is subjected to vortex oscillation extraction for 2-3min; then adding 5g of sodium chloride into the brown centrifuge tube, carrying out vortex oscillation for 1min, centrifuging at a rotating speed of 4000r/min or more, and taking supernatant.
The preferable technical scheme is as follows: in step 3, the conditions for UHPLC-MS/MS analysis were set as follows:
(1) Liquid chromatography conditions: c (C) 18 A chromatographic column; mobile phase: phase A is 5-10mmol/L ammonium acetate-0.05-0.2% formic acid-water solution, and phase B is acetonitrile; flow rate: 0.2-0.5mL/min; column temperature: 30-40 ℃; gradient elution.
(2) Mass spectrometry conditions: the ion source is an electrospray ionization source, positive ion scanning, negative ion scanning or positive and negative switching ion scanning, and a dynamic multi-reaction monitoring mode.
Due to the application of the technical scheme, compared with the prior art, the invention has the advantages that:
the method solves the technical problem of serious interference of pesticide multi-residue pretreatment matrixes in complex matrixes of the herbal tea, can effectively remove impurities such as pigment, polyphenol, organic acid, aromatic oil and the like, is used for rapidly extracting, purifying and accurately qualitatively quantifying pesticide multi-residues in the herbal tea such as safflower, chrysanthemum and rose, has the advantages of less reagent consumption, good purifying effect, low matrix effect, high sensitivity, high accuracy and high analysis speed, and can meet the detection requirements of various pesticide residues in the herbal tea.
Drawings
FIG. 1 shows porous g-C in the present invention 3 N 4 A sample graph.
FIG. 2 shows porous g-C in the present invention 3 N 4 The adsorption effect of the pigment in the safflower is shown.
FIG. 3 is a graph of a porous PVPP sample according to the present invention.
Fig. 4 is a graph showing ion chromatograms extracted from 53 kinds of pesticide DMRM in safflower according to the present invention.
Fig. 5 is a graph of ion chromatograms extracted from 39 kinds of pesticide DMRM in flos Chrysanthemi in the present invention.
Detailed Description
Further advantages and effects of the present invention will be readily apparent to those skilled in the art from the following disclosure of the present invention by reference to the specific embodiments.
Please refer to fig. 1-5. It should be understood that the structures, proportions, sizes, etc. shown in the drawings are shown only in the drawings and should not be taken as limiting the invention to those having ordinary skill in the art, since modifications, changes in proportions, or adjustments of sizes, etc. could be made without departing from the spirit or essential characteristics of the invention. The following examples are provided for a better understanding of the present invention, but are not intended to limit the present invention. The experimental methods in the following examples are conventional methods unless otherwise specified. The experimental materials used in the examples described below were purchased from conventional biochemical reagent stores unless otherwise specified.
The reagents and materials described in the examples below are commercially available unless otherwise indicated.
Example 1: method for detecting multiple residues of herb tea pesticides and adsorption purification composition used by method
Simultaneous determination of 53 pesticide residues in safflower
Porous g-C 3 N 4 Is prepared from the following steps: weighing 10g of urea and 5g of ammonium bicarbonate, putting into an agate mortar, fully grinding the two, putting into an alumina crucible with a sealing cover, and standing at 5 ℃ for min -1 Is heated to 80℃for 1h at 80℃and then is heated at 5℃for a period of minutes -1 Is heated to 550 c and held at that temperature for 3 hours. After the crucible is naturally cooled to room temperature, porous g-C is obtained 3 N 4 A material.
Preparation of porous PVPP: 50% by weight of N-vinylpyrrolidone (NVP), 25% by weight of water and then 0.5% by weight of sodium hydroxide and 1.5% by weight of Divinylbenzene (DVB), 23% by weight of N-hexane are placed in a nitrogen-protected vessel and stirred with nitrogen. Heating to 80 ℃, and reacting for 5 hours at constant temperature to obtain the crosslinked polyvinylpyrrolidone swelling particles. Filtering, washing, soaking in methanol, filtering, vacuum drying to constant weight, and grinding to obtain porous PVPP.
Sample detection:
Weighing 1g of a sample, placing the sample into a brown centrifuge tube with a plug, adding 2mL of an ascorbic acid aqueous solution with the volume of 15 mug/mL, mixing uniformly by vortex, adding 10mL of a formic acid acetonitrile solution with the volume concentration of 1%, and extracting by vortex oscillation for 2min; and adding 5g of sodium chloride into the centrifuge tube, carrying out vortex oscillation for 1min, centrifuging at a low temperature of 2 ℃ at a rotating speed of not less than 4000r/min, and taking supernatant to be purified.
1.0mL of the supernatant obtained in step 2 was charged with 100mg of porous graphite phase carbon nitride, 50mg of porous crosslinked polyvinylpyrrolidone, 50mg of C 18 Vortex 1min,10 in a centrifuge tube of 50mg PSA and 150mg anhydrous magnesium sulfateCentrifuging at 4deg.C for 5min at 000r/min, and collecting supernatant.
And (3) taking 0.5mL of the supernatant obtained in the step (3), diluting 1 time with pure water, passing the obtained diluted solution through a 0.22 mu m organic system filter membrane to a brown sample bottle, and analyzing by UHPLC-MS/MS so as to determine the pesticide residue in the sample to be detected. The specific conditions are as follows:
(1) Liquid chromatography conditions: agilent ZORBAX SB-C 18 Columns (2.1 mm. Times.100 mm,3.5 μm); mobile phase: phase A is 5mmol/L ammonium acetate-0.1% formic acid-water solution, and phase B is acetonitrile; flow rate: 0.4mL/min; column temperature: 40 ℃; the sample injection amount is 10 mu L;
(2) Gradient elution procedure, in volume fraction: 0min,1% B;3min,30% B;6min,40% B;9min,40% B;15min,60% B;19min,90% B;23min,90% B;23.01min,1% B, hold for 4min.
(3) Mass spectrometry conditions: ion source: electrospray ionization source (ESI), positive ion scan mode, sheath gas temperature 320 ℃, sheath gas flow 12L/min, atomizing gas pressure 40psi, drying gas temperature 320 ℃, drying gas flow 6L/min, capillary voltage positive mode 3000V, DMRM monitoring mode, qualitative ion pair, quantitative ion pair, residence time, fragmentation voltage (FP) and collision gas voltage (CE) are shown in Table 1.
TABLE 1 Multi-reaction monitoring mode parameters for 53 pesticides
In order to verify the effect of the method for removing matrix interference such as pigment, polyphenol, organic acid, aromatic oil and the like, the matrix effect is examined, and as shown in table 2, the matrix inhibition effect of 53 pesticides is less than 10%. To verify the sensitivity and accuracy of the above method, more than 53 pesticides were added to the safflower samples at 3 levels of 10 μg/kg, 20 μg/kg, 100 μg/kg, and recovery measurement was performed, each level was repeated 5 times, extraction, purification and detection were performed by the method of this example, and the results are shown in table 2, the recovery rates of the 53 pesticides were higher than 60%, and the indoor precision was less than 10%, satisfying the detection methodology requirements.
Table 2 average recovery and precision of samples (n=5)
The method is adopted to detect 5 commercial safflower samples, and the result shows that the acetamiprid residue is detected in 2 samples, and the content is 15.3 mug/kg and 25.6 mug/kg respectively; thiamethoxam residue was detected in 1 sample at a level of 17.6 μg/kg.
Example 2: method for detecting multiple residues of herb tea pesticides and adsorption purification composition used by method
Simultaneous determination of 39 pesticide residues in chrysanthemum
Porous g-C 3 N 4 Is prepared from the following steps: weighing 15g of urea and 6g of ammonium bicarbonate, putting into an agate mortar, fully grinding the two, putting into an alumina crucible with a sealing cover, and standing at 6 ℃ for min -1 Is heated to 80℃for 1.5h at 80℃and then is heated at 6℃for a period of minutes -1 Is heated to 580 ℃ at a rate ofThis temperature was maintained for 2 hours. After the crucible is naturally cooled to room temperature, porous g-C is obtained 3 N 4 A material.
Preparation of porous PVPP: 60wt% of N-vinylpyrrolidone (NVP), 20wt% of water and then 0.8wt% of sodium hydroxide and 1.2wt% of Divinylbenzene (DVB), 18wt% of N-hexane were added to a nitrogen-protected vessel and stirred with nitrogen. Heating to 100 ℃, and reacting for 4 hours at constant temperature to obtain the crosslinked polyvinylpyrrolidone swelling particles. Filtering, washing, soaking in methanol, filtering, vacuum drying to constant weight, and grinding to obtain porous PVPP.
Sample detection:
Weighing 2g of sample, placing the sample into a brown centrifuge tube with a plug, adding 2mL of an ascorbic acid aqueous solution with the volume of 15 mug/mL, mixing uniformly by vortex, adding 10mL of a formic acid acetonitrile solution with the volume concentration of 1%, and extracting by vortex oscillation for 2min; and adding 5g of sodium chloride into the centrifuge tube, carrying out vortex oscillation for 1min, centrifuging at a low temperature of 6 ℃ at a rotating speed of not less than 4000r/min, and taking supernatant to be purified.
1.0mL of the supernatant obtained in step 2 was placed in a centrifuge tube containing 50mg of porous graphite phase carbon nitride, 50mg of porous crosslinked polyvinylpyrrolidone, 50mg of C18, 50mg of PSA and 150mg of anhydrous magnesium sulfate, vortexed and oscillated for 1min, centrifuged at 10000r/min at 4℃for 5min, and the supernatant was taken for detection.
And (3) taking 0.5mL of the supernatant obtained in the step (3), diluting 1 time with pure water, passing the obtained diluted solution through a 0.22 mu m organic system filter membrane to a brown sample bottle, and analyzing by UHPLC-MS/MS so as to determine the pesticide residue in the sample to be detected. The specific conditions are as follows:
(1) Liquid chromatography conditions: agilent ZORBAX SB-C18 column (2.1 mm. Times.100 mm,3.5 μm); mobile phase: phase A is 5mmol/L ammonium acetate-0.1% formic acid-water solution, and phase B is acetonitrile; flow rate: 0.4mL/min; column temperature: 40 ℃; the sample injection amount is 10 mu L;
(2) Gradient elution procedure, in volume fraction: 0min,1% B;3min,30% B;6min,40% B;9min,40% B;15min,60% B;19min,99% B;23min,99% B;23.01min,1% B, hold for 4min.
(3) Mass spectrometry conditions: ion source: electrospray ionization source (ESI), positive ion scan mode, dryer air temperature: 300 ℃, drying gas flow rate: 10L/min, atomizing air pressure 40psi, capillary voltage positive mode 4000V, DMRM monitoring mode, qualitative ion pair, quantitative ion pair, residence time, fragmentation voltage (FP), and collision air voltage (CE) are shown in Table 3.
TABLE 3 Multi-reaction monitoring mode parameters for 39 pesticides
To verify the effect of the above method for removing matrix interference such as pigment, polyphenol, organic acid, aromatic oil, etc., the matrix effect was examined, and as shown in table 4, the matrix inhibition effect of 39 pesticides was less than 10%. In order to verify the sensitivity and accuracy of the method, more than 39 pesticides with the levels of 10 mug/kg, 20 mug/kg and 100 mug/kg are respectively added to a chrysanthemum sample, recovery measurement is carried out, each level is repeated 5 times, extraction, purification and detection are carried out by using the method of the embodiment, the result is shown in table 4, the recovery rate of the 39 pesticides is higher than 60%, the indoor precision is less than 10%, and the detection method requirement is met.
Table 4 average recovery and precision of samples (n=5)
By adopting the method to detect 6 commercial chrysanthemum samples, the result shows that difenoconazole residues are detected in 3 samples, and the content is 12.3-21.6 mug/kg; azoxystrobin residue was detected in 1 sample at a level of 11.2 μg/kg.
Example 3: method for detecting multiple residues of herb tea pesticides and adsorption purification composition used by method
An adsorption purification composition comprising graphite phase carbon nitride, cross-linked polyvinylpyrrolidone, octadecyl bonded silica gel, N-propylethylenediamine and anhydrous magnesium sulfate.
The preferable technical scheme is as follows: the graphite phase carbon nitride is porous graphite phase carbon nitride, and the preparation method comprises the following steps: placing urea and ammonium bicarbonate into a mortar, grinding, mixing, placing into an alumina crucible with a cover, and standing at 5deg.C for min -1 Is heated to 75℃for 1h at 75℃and then is heated at 5℃for a period of minutes -1 Is heated to 550 ℃ and kept at the temperature for 2 hours, and after the crucible is naturally cooled to room temperature, the porous g-C is obtained 3 N 4 A material.
The preferable technical scheme is as follows: the crosslinked polyvinylpyrrolidone is porous crosslinked polyvinylpyrrolidone, and the preparation method comprises the following steps: 50wt% of N-vinyl pyrrolidone, 20wt% of water and then 0.5wt% of sodium hydroxide, 1wt% of divinylbenzene and 28.5wt% of N-hexane are added into a nitrogen-protected container, and nitrogen is introduced and stirred; heating to 80 ℃, and reacting at constant temperature for 3 hours to obtain crosslinked polyvinylpyrrolidone swelling particles; washing, filtering, soaking in methanol, filtering, vacuum drying to constant weight, and grinding to obtain porous cross-linked polyvinylpyrrolidone.
A method for detecting multi-residue of a herb tea pesticide comprises the following steps:
step 1: placing a herbal tea sample to be detected in a brown centrifuge tube with a plug, adding an ascorbic acid aqueous solution, mixing uniformly by vortex, adding an acetonitrile formate solution, and extracting by vortex oscillation; adding sodium chloride into the brown centrifuge tube, carrying out vortex oscillation, centrifuging at 0 ℃, and taking supernatant;
the dosage ratio of the supernatant to the adsorption purification composition agent is as follows: 1mL of supernatant corresponds to 50mg of porous graphite phase carbon nitride, 50mg of porous crosslinked polyvinylpyrrolidone, 50mg of octadecyl bonding silica gel, 50mg of N-propylethylenediamine and 150mg of anhydrous magnesium sulfate, and the dosage of N-propylethylenediamine is less than 50mg when the pesticide residue contains prothioconazole and the metabolite of the prothioconazole.
The preferred embodiments are: in the step 1, 1g of herbal tea sample to be measured is weighed and placed in a brown centrifuge tube with a plug, an ascorbic acid aqueous solution with the mass of 2 times that of the herbal tea sample to be measured and the concentration of 15 mug/mL is added and mixed uniformly by vortex, then 5mL of acetonitrile formate solution with the volume concentration of 1% is added, and vortex oscillation is carried out for 2min; then adding 5g of sodium chloride into the brown centrifuge tube, carrying out vortex oscillation for 1min, centrifuging at a rotating speed of 4000r/min or more, and taking supernatant.
The preferred embodiments are: in step 3, the conditions for UHPLC-MS/MS analysis were set as follows:
(1) Liquid chromatography conditions: c (C) 18 A chromatographic column; mobile phase: phase A is 5mmol/L ammonium acetate-0.05-0.2% formic acid-water solution, and phase B is acetonitrile; flow rate: 0.2mL/min; column temperature: 30 ℃; gradient elution.
(2) Mass spectrometry conditions: the ion source is an electrospray ionization source, positive ion scanning, negative ion scanning or positive and negative switching ion scanning, and a dynamic multi-reaction monitoring mode.
Example 4: method for detecting multiple residues of herb tea pesticides and adsorption purification composition used by method
An adsorption purification composition comprising graphite phase carbon nitride, cross-linked polyvinylpyrrolidone, octadecyl bonded silica gel, N-propylethylenediamine and anhydrous magnesium sulfate.
The preferred embodiments are: the graphite phase carbon nitride is porous graphite phase carbon nitride, and the preparation method comprises the following steps: placing urea and ammonium bicarbonate into a mortar, grinding, mixing, placing into an alumina crucible with a cover, and standing at 8deg.C for min -1 Is heated to 85 ℃ at a rate of 75-85 ℃ for 2 hours and then at 8 ℃ for min -1 Is heated to 600 ℃ and kept at the temperature for 3 hours, and after the crucible is naturally cooled to room temperature, the porous g-C is obtained 3 N 4 A material.
The preferred embodiments are: the crosslinked polyvinylpyrrolidone is porous crosslinked polyvinylpyrrolidone, and the preparation method comprises the following steps: adding 70wt% of N-vinyl pyrrolidone 15wt% of water into a nitrogen-protected container, then adding 1wt% of sodium hydroxide and 2wt% of divinylbenzene, 12wt% of N-hexane, introducing nitrogen and stirring; heating to 80-120 ℃, and reacting at constant temperature for 5 hours to obtain crosslinked polyvinylpyrrolidone swelling particles; washing, filtering, soaking in methanol, filtering, vacuum drying to constant weight, and grinding to obtain porous cross-linked polyvinylpyrrolidone.
A method for detecting multi-residue of a herb tea pesticide comprises the following steps:
step 1: placing a herbal tea sample to be detected in a brown centrifuge tube with a plug, adding an ascorbic acid aqueous solution, mixing uniformly by vortex, adding an acetonitrile formate solution, and extracting by vortex oscillation; adding sodium chloride into the brown centrifuge tube, carrying out vortex oscillation, centrifuging at 6 ℃, and taking supernatant;
the dosage ratio of the supernatant to the adsorption purification composition agent is as follows: 1mL of the supernatant corresponded to 200mg of porous graphite phase carbon nitride, 100mg of porous crosslinked polyvinylpyrrolidone, 100mg of octadecyl bonded silica gel, 100mg of N-propylethylenediamine and 200mg of anhydrous magnesium sulfate.
The preferred embodiments are: in the step 1, 2g of herbal tea sample to be measured is weighed and placed in a brown centrifuge tube with a plug, an ascorbic acid aqueous solution with the mass of 2 times that of the herbal tea sample to be measured and the concentration of 15 mug/mL is added and mixed uniformly by vortex, and then 10mL of acetonitrile formate solution with the volume concentration of 1% is added, and the mixture is subjected to vortex oscillation extraction for 3min; then adding 5g of sodium chloride into the brown centrifuge tube, carrying out vortex oscillation for 1min, centrifuging at a rotating speed of 4000r/min or more, and taking supernatant.
The preferred embodiments are: in step 3, the conditions for UHPLC-MS/MS analysis were set as follows:
(1) Liquid chromatography conditions: c (C) 18 A chromatographic column; mobile phase: phase A is 10mmol/L ammonium acetate-0.05-0.2% formic acid-water solution, and phase B is acetonitrile; flow rate: 0.5mL/min; column temperature: 40 ℃; gradient elution.
(2) Mass spectrometry conditions: the ion source is an electrospray ionization source, positive ion scanning, negative ion scanning or positive and negative switching ion scanning, and a dynamic multi-reaction monitoring mode.
The foregoing description of the preferred embodiment of the invention is not intended to be limiting in any way, but rather, it is intended to cover all modifications or variations of the invention which fall within the spirit and scope of the invention.
Claims (6)
1. An adsorption purification composition, which is characterized in that: the adsorption purification composite agent comprises graphite phase carbon nitride, crosslinked polyvinylpyrrolidone, octadecyl bonded silica gel, N-propyl ethylenediamine and anhydrous magnesium sulfate.
2. The adsorption purification composition according to claim 1, wherein: the graphite phase carbon nitride is porous graphite phase carbon nitride, and the preparation method comprises the following steps: placing urea and ammonium bicarbonate into a mortarGrinding, mixing, placing into alumina crucible with cover, and standing at 5-8deg.C for min -1 Heating to 75-85deg.C, maintaining at 75-85deg.C for 1-2 hr, and then heating at 5-8deg.C for 5-min -1 Heating to 550-600deg.C, maintaining at the temperature of 2-3h, and naturally cooling to room temperature to obtain porous g-C 3 N 4 A material.
3. The adsorption purification composition according to claim 1, wherein: the crosslinked polyvinylpyrrolidone is porous crosslinked polyvinylpyrrolidone, and the preparation method comprises the following steps: adding 50-wt-70-wt% of N-vinyl pyrrolidone, 8-wt-35-wt% of water into a nitrogen-protected container, then adding 0.5-wt-1-wt% of sodium hydroxide and 1-wt-2-wt% of divinylbenzene, 8-30% of N-hexane by weight, introducing nitrogen and stirring; heating to 80-120 ℃, and reacting at constant temperature for 3-5h to obtain crosslinked polyvinylpyrrolidone swelling particles; washing, filtering, soaking in methanol, filtering, vacuum drying to constant weight, and grinding to obtain porous cross-linked polyvinylpyrrolidone.
4. A method for detecting multi-residue of a herb tea pesticide is characterized by comprising the following steps: comprises the following steps:
step 1: placing a herbal tea sample to be detected in a brown centrifuge tube with a plug, adding an ascorbic acid aqueous solution, mixing uniformly by vortex, adding an acetonitrile formate solution, and extracting by vortex oscillation; adding sodium chloride into the brown centrifuge tube, carrying out vortex oscillation, centrifuging at 0-6 ℃, and taking supernatant;
step 2; placing the supernatant obtained in the step 1 into a centrifuge tube filled with an adsorption and purification composition, carrying out vortex oscillation, centrifuging at 0-6 ℃, and taking the supernatant;
step 3, diluting the supernatant obtained in the step 2 by 1 time with pure water, and allowing the obtained diluted solution to pass through a 0.22 mu m organic system filter membrane to a brown sample bottle, and performing UHPLC-MS/MS analysis to determine the residual quantity of various pesticides in a sample to be detected;
the adsorption purification composition adopts the adsorption purification composition according to any one of claims 1 to 3;
the dosage ratio of the supernatant to the adsorption purification composition agent is as follows: 1mL supernatant fluid corresponding to 50-200mg porous graphite phase carbon nitride, 50-100mg porous crosslinked polyvinylpyrrolidone, 50-100mg octadecyl bonded silica gel, 50-100mg N-propylethylenediamine and 150-200mg anhydrous magnesium sulfate;
when the pesticide residue contains prothioconazole and a metabolite of the prothioconazole, the dosage of N-propyl ethylenediamine is less than 50 and mg.
5. The method for detecting the pesticide residues in the herb tea according to claim 4, which is characterized by comprising the following steps: in the step 1, 1-2g of herbal tea sample to be measured is weighed and placed in a brown centrifuge tube with a plug, an ascorbic acid aqueous solution with the mass of 2 times that of the herbal tea sample to be measured and the concentration of 15 mug/mL is added and mixed uniformly by vortex, then an acetonitrile formate solution with the volume concentration of 5-10 mL% is added, and vortex oscillation is carried out for 2-3min; then adding 5g sodium chloride into the brown centrifuge tube, shaking for 1min by vortex, centrifuging at a rotating speed of more than or equal to 4000r/min, and taking supernatant.
6. The method for detecting the pesticide residues in the herb tea according to claim 4, which is characterized by comprising the following steps: in step 3, the conditions for UHPLC-MS/MS analysis were set as follows:
(1) Liquid chromatography conditions: c (C) 18 A chromatographic column; mobile phase: phase A is 5-10mmol/L ammonium acetate-0.05-0.2% formic acid-water solution, and phase B is acetonitrile; flow rate: 0.2-0.5mL/min; column temperature: 30-40 ℃; gradient elution;
(2) Mass spectrometry conditions: the ion source is an electrospray ionization source, positive ion scanning, negative ion scanning or positive and negative switching ion scanning, and a dynamic multi-reaction monitoring mode.
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