CN113419008B - Synthetic phase chromatography tandem mass spectrometry determination method for fluensulfone metabolite - Google Patents
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Abstract
The invention relates to a synthetic phase chromatography tandem mass spectrometry determination method of a fluensulfone metabolite, belonging to the technical field of pesticide residue detection. The method comprises the following steps: a QuEChERS pretreatment method is adopted, a sample is extracted by an organic solvent, after centrifugation, supernatant is subjected to dispersion solid phase extraction and purification, and the detection is carried out by a combined phase chromatography tandem mass spectrum. The invention establishes the synthetic phase chromatography tandem mass spectrometry analysis method of the fluensulfone metabolite for the first time, and is suitable for extracting and determining the fluensulfone metabolite residue in samples such as vegetables, melons, fruits, tobaccos and the like. When the method is used for measuring the residual quantity of the fluensulfone metabolite, a fluensulfone metabolite blank sample is adopted for matrix matching, so that the measurement result is more accurate. In addition, when the detection is carried out by the combined phase chromatography tandem mass spectrometry, the used main mobile phase is supercritical fluid CO 2 And the cosolvent uses a very small amount of methanol, so that the method has the advantage of environmental friendliness.
Description
Technical Field
The invention relates to a synthetic phase chromatography tandem mass spectrometry method for residual fluensulfone metabolites in tobacco, belonging to the technical field of pesticide residue detection.
Background
Fluensulfone, fluoroolefinsulfone and flosulin are fluoroolefin thioether compounds, are the only new chemical nematicide developed in more than 20 years, have contact activity, can enable growers to get rid of dependence on fumigation type nematicides for many years, and simultaneously avoid some adverse effects brought by applying fumigants. The fluensulfone metabolite can be used for comprehensive treatment of nematode diseases of various crops, such as solanaceous crops such as eggplant, hot pepper, tomato, tobacco and the like, melon crops such as cucumber, pumpkin, watermelon, hami melon and the like, leafy vegetables of Compositae and Cruciferae, and yams such as potato, sweet potato and the like.
Fluensulfone was developed by Israeli Mark Semm, inc. (Shi' ao wheat) in 1993-1994 and marketed in 2014, and in recent years, the market has been growing rapidly. In 2019, 30 days in 1 month, 95% of a fluoro-alkene-sulfone raw drug and 40% of a fluoro-alkene-sulfone emulsifiable concentrate are registered by Amacriximal Limited, andao; the product of the preparation has the tradename of nimide, soil spraying and cucumber root-knot nematode prevention and control, and the dosage of the preparation is 500-600 mL/667 m 2 . In the same year, nimide is marketed in China. Fluensulfone is metabolized primarily in plants and/or animals to thiazolesulfonic acid metabolites (TSA), methylsulfone metabolites (MeS), and butenesulfonic acid metabolites (BSA). Among them, studies have shown that: the main metabolite of fluensulfone in tobacco is BSA, and the structure is shown in figure 1. Toxicology data indicate that fluensulfone causes proliferation of mouse lung cells and further causes alveolar/bronchiolar hyperplasia, eventually leading to the appearance of tumors. And studies have shown that BSA metabolites have similar toxicity to fluensulfone.
At present, the residual limit of fluensulfone in vegetables and fruits released by the U.S. environmental protection agency is 0.5 mg/kg, and the temporary guiding residual quantity (GRL) in Tobacco recommended by CORESTA (Cooperation Centre for Scientific Research Relative to Tobacco) is 0.15 mg/kg, including the residual quantity of fluensulfone converted from the metabolite BSA.
The essence of the combined phase chromatography tandem mass spectrometry is a chromatography technique based on supercritical fluid chromatography. In recent years, with the great improvement of supercritical fluid chromatography, the supercritical fluid chromatography has wider application space, and has attracted the attention of more and more researchers. In view of the fact that the synthetic phase chromatography also adopts non-toxic, nonflammable and environment-friendly supercritical fluid CO2 as a main mobile phase, the method is a real green and environment-friendly technology, has a plurality of outstanding advantages compared with liquid chromatography and gas chromatography, has good separation degree and selectivity for structural analogs, isomers, enantiomers and diastereomers, and is combined with the use of a tandem mass spectrometry detector, so that the detection sensitivity is further improved.
Disclosure of Invention
The invention aims to analyze and detect the residues of the fluensulfone metabolites in a sample by adopting a QuEChERS pretreatment technology and combining a combined chromatography-tandem mass spectrometry detection method so as to provide technical support for monitoring the residues of the fluensulfone and the metabolites thereof.
The invention aims to provide a combined phase chromatography tandem mass spectrometry method for measuring residues of fluensulfone metabolites.
In order to achieve the purpose, the technical scheme of the invention comprises the following steps:
soaking a sample in water, adding acetonitrile to carry out vortex oscillation extraction, carrying out freezing preservation at the temperature of-18 ℃ to avoid decomposition or volatilization of residual fluensulfone metabolites caused by excessive local heat release in the subsequent dewatering and salting-out process, then respectively adding anhydrous magnesium sulfate, sodium chloride, sodium citrate and disodium citrate to carry out dewatering and salting-out, wherein the sodium citrate and the disodium citrate are used for providing an alkaline buffer environment to ensure the recovery rate of the fluensulfone metabolites, carrying out vortex oscillation and centrifugation, taking a supernatant into a centrifuge tube, adding anhydrous magnesium sulfate and an N-propyl ethylenediamine bonded solid-phase adsorbent, carrying out vortex oscillation and centrifugation, filtering the supernatant through an organic phase filter membrane, and finally carrying out ultra-high performance combined phase chromatography tandem mass spectrometry.
10mL of water and 10mL of acetonitrile are added for every 2g of sample.
The vortex was shaken at 2000rpm for 2min.
The centrifugation is carried out for 10min at the rotating speed of 4000 rpm.
The filtration is performed by adopting a 0.22 mu m organic phase filter membrane.
The conditions of the ultra-high performance synthesis chromatography-tandem mass spectrometry are as follows: a chromatographic column: viridis HSS C18 SB chromatography column (100 mm. Times.3.0 mm,1.8 μm); column temperature: 40 ℃; sample injection amount: 2 mu L of the solution; flow ofPhase (1): mobile phase A: supercritical fluid CO 2 And the mobile phase B: methanol, gradient elution is carried out; flow rate: 2.0 mL/min; compensation solution: 1% formic acid solution in methanol with flow rate of 0.1 mL/min; mass spectrum conditions: the scanning mode is as follows: scanning negative ions; an ion source: electrospray ionization source (ESI), temperature: 150 ℃; capillary voltage: 2.4 kV; temperature of the desolventizing gas: 350 ℃; desolventizing air flow rate: 650 L/h; reverse blowing airflow rate: 55 L/h; a monitoring mode: multiple Reaction Monitoring (MRM).
The elution conditions for the gradient elution are shown in table 1 below:
TABLE 1 gradient elution procedure
| Time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0.00 | 95 | 5 |
| 1.00 | 95 | 5 |
| 2.00 | 90 | 10 |
| 5.00 | 90 | 10 |
| 5.01 | 95 | 5 |
| 6.00 | 95 | 5 |
The MRM mass spectral parameters are shown in table 2 below:
TABLE 2 MRM Mass Spectrometry parameters for Fluthiamethoxam sulfone metabolites
* Quantitative ion
In the combined phase chromatography-tandem mass spectrometry, a blank matrix is adopted to prepare a series of standard working solutions.
The fluensulfone metabolite BSA has the advantages of small molecular weight, strong polarity, low ionization efficiency and technical difficulty in detecting the fluensulfone metabolite BSA. At present, no detection method for the substance is reported. The method for determining the fluensulfone metabolite residue performs system optimization on sample treatment, chromatographic conditions and the like, firstly uses a QuEChERS pretreatment technology to extract the fluensulfone metabolite residue in the sample, then performs ultra-high performance synthetic chromatography-tandem mass spectrometry and performs external standard quantification. The method for measuring the fluensulfone metabolite residue is green, simple, accurate and high in precision.
Drawings
FIG. 1 chemical Structure of Fluthiamethoxam sulfone metabolite BSA;
figure 2 blank matrix matched standard working solution chromatograms.
Detailed Description
The following examples are given only for the purpose of illustrating the present invention in further detail, and are not to be construed as limiting the present invention in any way.
Instruments and reagents
Ultra-high performance compatible chromatography tandem mass spectrometry (Waters corporation, usa);
Milli-Q ultra pure water system (Millipore, USA);
fluensulfone metabolites (Amachromachem, inc., andao);
methanol (chromatographically pure, U.S. j.t. Baker).
Example 1
The QuEChERS extraction method of residual fluensulfone metabolites in tobacco comprises the following steps:
2.00g (to the nearest 0.01 g) of tobacco powder sample is weighed into a 50mL centrifuge tube with a cover, 10mL of water is added, the mixture is manually shaken until the sample is fully soaked by the water, and then the mixture is kept stand for 10min. Adding 10mL of acetonitrile, performing vortex oscillation for 2min at 2000r/min, performing freeze preservation for 10min at-18 ℃, then respectively adding 4g of anhydrous magnesium sulfate, 1g of sodium chloride, 1g of sodium citrate and 0.5g of disodium citrate, immediately performing vortex oscillation for 2min at 2000r/min to prevent the anhydrous magnesium sulfate from being locally overheated and caking due to reaction with water, then performing centrifugation for 10min at 4000r/min, taking 1mL of supernatant into a 1.5mL centrifuge tube, adding 150mg of anhydrous magnesium sulfate and 25mg of N-propyl ethylenediamine bonded solid phase adsorbent, performing vortex oscillation for 2min at 2000r/min, then performing centrifugation for 10min at 4000r/min, filtering the supernatant through a 0.22 mu m organic phase filter membrane, and performing combined phase chromatography tandem mass spectrometry.
The combined chromatography-tandem mass spectrometry determination method for the residual fluensulfone metabolites in the tobacco comprises the following steps:
1) Preparation of the test solution
2.00g (to the nearest 0.01 g) of tobacco powder sample is weighed into a 50mL centrifuge tube with a cover, 10mL of water is added, the mixture is manually shaken until the sample is fully soaked by the water, and then the mixture is kept stand for 10min. Adding 10mL of acetonitrile, performing vortex oscillation for 2min at 2000r/min, performing freeze preservation for 10min at-18 ℃, then respectively adding 4g of anhydrous magnesium sulfate, 1g of sodium chloride, 1g of sodium citrate and 0.5g of disodium citrate, immediately performing vortex oscillation for 2min at 2000r/min to prevent the anhydrous magnesium sulfate from being locally overheated and caking due to reaction in water, then performing centrifugation for 10min at 4000r/min, taking 1mL of supernatant into a 1.5mL centrifuge tube, adding 150mg of anhydrous magnesium sulfate and 25mg of N-propyl ethylenediamine bonded solid phase adsorbent, performing vortex oscillation for 2min at 2000r/min, then performing centrifugation for 10min at 4000r/min, and filtering the supernatant through a 0.22 mu m organic phase filter membrane to obtain the product. It should be noted that: the extraction solvent is methanol besides acetonitrile, and the result shows that the extraction efficiency of the acetonitrile is higher.
2) Preparation of the blank matrix
2.00g (to the nearest 0.01 g) of a fluorosulfonamide metabolite-free tobacco dust sample was weighed into a 50mL centrifuge tube with a lid, 10mL of water was added, and the tube was shaken manually until the sample was thoroughly soaked in water and allowed to stand for 10min. Adding 10mL of acetonitrile, performing vortex oscillation for 2min at 2000r/min, performing freeze preservation for 10min at-18 ℃, then respectively adding 4g of anhydrous magnesium sulfate, 1g of sodium chloride, 1g of sodium citrate and 0.5g of disodium citrate, immediately performing vortex oscillation for 2min at 2000r/min to prevent the anhydrous magnesium sulfate from being locally overheated and caking due to reaction in water, then performing centrifugation for 10min at 4000r/min, taking 1mL of supernatant into a 1.5mL centrifuge tube, adding 150mg of anhydrous magnesium sulfate and 25mg of N-propyl ethylenediamine bonded solid phase adsorbent, performing vortex oscillation for 2min at 2000r/min, then performing centrifugation for 10min at 4000r/min, and filtering the supernatant through a 0.22 mu m organic phase filter membrane to obtain the product.
3) Preparation of series standard working solution
Preparation of stock solution: weighing 10 mg of the standard substance of the fluorosulfonyl Linne metabolite into a 10mL volumetric flask, diluting with methanol and finally preparing into a standard working solution with a concentration gradient (the fluorosulfonyl Linne metabolite is insoluble or has low solubility in other organic solvents).
Preparing a series of standard working solutions: respectively transferring 0.2mL of the standard working solution and 0.2mL of the blank sample extracting solution, mixing, diluting to 1mL by using acetonitrile, and preparing a matrix mixed standard working solution; the concentrations of the fluensulfone metabolite in each prepared matrix mixed standard working solution are respectively 0.004 mu g/mL, 0.01 mu g/mL, 0.02 mu g/mL, 0.04 mu g/mL, 0.1 mu g/mL and 0.2 mu g/mL.
4) Production of standard working curve
Carrying out ultra-high performance combined chromatography-tandem mass spectrometry analysis on the series of standard working solutions with the 6 concentrations obtained in the step 3), carrying out regression analysis by taking the chromatographic peak area of a target object as a ordinate and the content of the fluensulfone metabolite as an abscissa to obtain a standard curve and a regression analysis thereofAnd (4) an equation. The chromatogram of the third-stage standard working solution is shown in FIG. 2. The standard working curve isY=2.6408*X-14.8187（R 2 =0.999507）。
The measuring conditions of the ultra-high performance combined phase chromatography-tandem mass spectrometry are as follows: chromatographic conditions are as follows: the chromatographic column is a Viridis HSC 18 phase column (50 mm. Times.2.1 mm,3 μm); column temperature: 40 ℃; sample injection amount: 2. mu.L; mobile phase: a mobile phase A: acetonitrile, mobile phase B:0.1% formic acid aqueous solution, isocratic elution (10% A: 90% B, volume ratio); flow rate: 0.3 mL/min. Compensation solution: 1% formic acid solution in methanol with flow rate of 0.1 mL/min; mass spectrum conditions: the scanning mode is as follows: scanning negative ions; an ion source: electrospray ionization source (ESI), temperature: 150 ℃; capillary voltage: 2.4 kV; temperature of the desolvation gas: 300 ℃; desolventizing air flow rate: 800 L/h; reverse blowing airflow rate: 150 L/h; and (3) monitoring mode: multiple reaction monitoring mode (MRM), detailed parameters are given in table 2 above. It should be noted that: in addition to the Viridis HSC 18 SB synthetic phase chromatography column in step 4), ACQUITY UPC was also examined separately 2 CSH Fluoro Phenyl chromatography column, ACQUITY UPC 2 Effect of BEH chromatography column on the determination of fluorosulfamide metabolite, viridis HSS C18 was the best.
5) Ultra-high performance combined chromatography-tandem mass spectrometry of liquid to be detected
Carrying out ultra-high performance phase combination chromatography-tandem mass spectrometry on the solution to be tested obtained in the step 1), wherein the testing conditions are the same as those of the ultra-high performance phase combination chromatography-tandem mass spectrometry in the step 4). Substituting the ratio of the chromatographic peak area of the target analyte to the chromatographic peak area of the internal standard substance into the standard curve obtained in the step 4), and calculating to obtain the content of the fluensulfone metabolite in the solution to be detected.
Experimental example 2
The recovery rate test is carried out on the air-white tobacco powder samples according to three addition levels of 10 mg/kg, 20 mg/kg and 50mg/kg, the recovery rate test is carried out for 3 times in parallel, and the obtained relative recovery rate is in the range of 95.6-102.9%. Gradually diluting the lowest concentration standard working solution matched with the blank matrix by using the blank matrix, and obtaining the detection limit of the method by using 3 times of signal to noise ratio as the detection limit and 10 times of signal to noise ratio as the quantification limit, wherein the detection limit is as follows: 0.02 mg/kg, limit of quantitation: 0.05 mg/kg.
Claims (9)
1. A combined chromatography tandem mass spectrometry determination method of fluensulfone metabolites is characterized in that: the method comprises the following steps: soaking a sample in water, adding acetonitrile for vortex oscillation extraction, freezing and storing at-18 ℃, respectively adding anhydrous magnesium sulfate, sodium chloride, sodium citrate and disodium citrate, carrying out vortex oscillation and centrifugation, taking supernate into a centrifugal tube, adding anhydrous magnesium sulfate and N-propyl ethylenediamine bonded solid-phase adsorbent, carrying out vortex oscillation and centrifugation, filtering the supernate through an organic phase filter membrane, and finally carrying out ultra-high performance phase combination chromatography-tandem mass spectrometry;
the fluensulfone metabolite is specifically 3, 4-trifluoro-3-butene-1-sulfonic acid, and the structural formula is as follows:
the conditions of the ultra-high performance compatible chromatography-tandem mass spectrometry are as follows: and (3) chromatographic column: viridis HSS C18 SB synthetic phase chromatographic column with specification of 100 mm multiplied by 3.0 mm,1.8 μm; column temperature: at 40 ℃; sample introduction amount: 2. mu.L; mobile phase: mobile phase A: supercritical fluid CO 2 And a mobile phase B: methanol, gradient elution is carried out; flow rate: 2.0 mL/min; compensation solution: 1% formic acid solution in methanol with flow rate of 0.1 mL/min; mass spectrum conditions: the scanning mode comprises the following steps: scanning negative ions; an ion source: electrospray ionization source (ESI), temperature: 150 ℃; capillary voltage: 2.4 kV; temperature of the desolvation gas: 350 ℃; desolvation airflow rate: 650 L/h; reverse blowing airflow rate: 55 L/h; and (3) monitoring mode: multiple Reaction Monitoring (MRM);
the elution conditions for the gradient elution are shown in table 1 below:
TABLE 1 gradient elution procedure
。
2. The method for determining fluensulfone metabolite combination chromatography tandem mass spectrometry of claim 1, wherein: 10mL of water and 10mL of acetonitrile are added for every 2g of sample.
3. The method for determining fluensulfone metabolite combination chromatography tandem mass spectrometry of claim 1, wherein: the vortex oscillation is 2min at the speed of 2000 rpm; the centrifugation is performed for 10min at the rotating speed of 4000 rpm.
4. The method for determining fluensulfone metabolite combination chromatography tandem mass spectrometry of claim 1, wherein: the filtration is performed by adopting a 0.22 mu m organic phase filter membrane.
5. The method for determining fluensulfone metabolite combination chromatography tandem mass spectrometry of claim 1, wherein: the sample is vegetable, melon or fruit or tobacco.
6. The method for measuring fluensulfone metabolite of claim 1, wherein the mass spectrum of the fluensulfone metabolite comprises the following steps: the MRM mass spectral parameters are shown in table 2 below:
7. the method for measuring fluensulfone metabolite of claim 1, wherein the mass spectrum of the fluensulfone metabolite comprises the following steps: in the combined phase chromatography-tandem mass spectrometry, a blank matrix is adopted to prepare a series of standard working solutions.
8. The method for determining fluensulfone metabolite combination chromatography tandem mass spectrometry of claim 7, wherein: the preparation process of the blank matrix is as follows:
weighing 2.00g of tobacco powder sample without containing fluorosulfona-thiacloprid metabolite into a 50mL centrifuge tube with a cover, adding 10mL of water, manually oscillating until the sample is fully soaked by the water, and standing for 10min; adding 10mL of acetonitrile, performing vortex oscillation for 2min at 2000r/min, performing freeze preservation for 10min at-18 ℃, then respectively adding 4g of anhydrous magnesium sulfate, 1g of sodium chloride, 1g of sodium citrate and 0.5g of disodium citrate, immediately performing vortex oscillation for 2min at 2000r/min to prevent the anhydrous magnesium sulfate from being locally overheated and caking due to reaction in water, then performing centrifugation for 10min at 4000r/min, taking 1mL of supernatant into a 1.5mL centrifuge tube, adding 150mg of anhydrous magnesium sulfate and 25mg of N-propyl ethylenediamine bonded solid phase adsorbent, performing vortex oscillation for 2min at 2000r/min, then performing centrifugation for 10min at 4000r/min, and filtering the supernatant through a 0.22 mu m organic phase filter membrane to obtain the product.
9. The method for measuring fluensulfone metabolite of claim 7, wherein the mass spectrum of the fluensulfone metabolite comprises the following steps: the preparation process of the series of standard working solutions is as follows:
1) Preparation of stock solution: weighing 10 mg of a standard substance of the fluorosulfonate-Ling metabolite into a 10mL volumetric flask, diluting with methanol, and finally preparing a standard working solution with a concentration gradient;
2) Preparing a series of standard working solutions: respectively transferring 0.2mL of the standard working solution and 0.2mL of the blank sample extracting solution, mixing, diluting to 1mL by using acetonitrile, and preparing a matrix mixed standard working solution; the concentrations of the fluensulfone metabolite in each prepared matrix mixed standard working solution are respectively 0.004 mu g/mL, 0.01 mu g/mL, 0.02 mu g/mL, 0.04 mu g/mL, 0.1 mu g/mL and 0.2 mu g/mL.
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