Method for detecting pyraclostrobin, fluxapyroxad and fluxapyroxad metabolites in peanut kernels and peanut straws

A technology for pyraclostrobin and flufenapyroxol in kernels, which is applied in the field of detection of pyraclostrobin, flufenapyroxamide and flufenapyroxamide metabolites, and can solve the problem of simultaneous detection of flufenapyroxad and flufenapyramide metabolites, etc., to improve the accuracy and stability, and the detection method is accurate and effective

Pending Publication Date: 2021-12-28
INST OF ZOOLOGY CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Based on the consideration of food safety and residents’ health, it is very necessary to detect pyraclostrobin and flufenapyr

Method used

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  • Method for detecting pyraclostrobin, fluxapyroxad and fluxapyroxad metabolites in peanut kernels and peanut straws
  • Method for detecting pyraclostrobin, fluxapyroxad and fluxapyroxad metabolites in peanut kernels and peanut straws
  • Method for detecting pyraclostrobin, fluxapyroxad and fluxapyroxad metabolites in peanut kernels and peanut straws

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] Detection method of pyraclostrobin, flufenapyramide and flufenapyramide metabolites in peanut kernels:

[0088] (1) Preparation of the liquid to be tested:

[0089] Weigh 5g (±0.05g) of peanut kernel samples into a 50mL PTFE centrifuge tube, add 5mL of ultrapure water, 5mL of 1.2% acetic acid acidified acetonitrile (chromatographically pure, v / v) respectively, break the cells and extract for 5min, add 3g of sodium chloride , vortexed for 1 min, centrifuged at 1110×g for 5 min, and took 1.5 mL of the supernatant in a medium containing 20 mg of octadecyl-bonded zirconium colloid, 50 mg of C18 and 150 mg of anhydrous MgSO 4 In a centrifuge tube, vortex for 30s, centrifuge for 1min at 9.6×g relative centrifugal force, use a 1mL syringe to take the supernatant and pass it through a 0.22μm filter membrane into a vial for testing.

[0090] (2) Standard solution preparation:

[0091] Dilute the first mixed standard solution and the second mixed standard solution containing 10...

Embodiment 2

[0114] Determination method of pyraclostrobin, flufenapyramide and flufenapyramide metabolites in peanut straw:

[0115] (1) Preparation of the liquid to be tested:

[0116] Weigh 5g (±0.05g) peanut straw samples into a 50mL PTFE centrifuge tube, add 10mL ultrapure water, 10mL1.2% acetic acid acidified acetonitrile (chromatographically pure, v / v) respectively, crush and extract the cells for 5min, add 3g sodium chloride , vortexed for 1min, centrifuged at 1110×g for 5min, took 1.5mL supernatant in a centrifuge tube filled with 50mg C18 and 150mg anhydrous MgSO4, vortexed for 30s, centrifuged at 9.6×g for 1min, and used Take the supernatant with a 1mL syringe and pass it through a 0.22μm filter membrane into a sample injection vial for detection by LC-ESI-MS / MS.

[0117] (2) Standard solution preparation:

[0118] Dilute the first mixed standard solution and the second mixed standard solution containing 10mg / L of pyraclostrobin · flufenapyramide and its metabolites with the bla...

Embodiment 3

[0155] Investigate the accuracy and precision of embodiment 1~2 and comparative example 1 detection method:

[0156] According to the detection method of Example 1 and Comparative Example 1, while processing the sample, add the mixed standard solution according to the addition amount of 0.0030mg / kg, 0.010mg / kg, 0.050mg / kg, 0.50mg / kg respectively, each group is set 5 parallel samples, according to the measurement results, calculate the recovery rate and relative standard deviation RSD, the results are shown in Table 11-Table 18.

[0157] According to the detection method of Example 2, while processing the sample, add the mixed standard solution according to the addition amount of 0.010mg / kg, 0.050mg / kg, 0.50mg / kg, 30mg / kg respectively, set 5 parallel samples in each group, According to the measurement results, the recovery rate and relative standard deviation RSD were calculated, and the results are shown in Table 19-Table 22.

[0158] See Table 23 for the requirements of diff...

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Abstract

The invention discloses a method for detecting pyraclostrobin, fluxapyroxad and fluxapyroxad metabolites in peanut kernels and peanut straws, and belongs to the technical field of pesticide residue detection. Pyraclostrobin, fluxapyroxad and fluxapyroxad metabolites in peanut kernel and peanut straw samples are extracted/purified by adopting a dispersive solid-phase extraction mode, and then extracted substances are determined by utilizing a liquid chromatography-tandem triple quadrupole mass spectrometer (LC-ESI-MS/MS). The purpose of accurately, qualitatively and quantitatively detecting pyraclostrobin, fluxapyroxad and fluxapyroxad metabolites in peanut kernel and peanut straw samples is achieved. The detection method provided by the invention is accurate, rapid and effective, the limit of quantitation is lower than the maximum residual limit (MRLs) of pyraclostrobin and fluxapyroxad on peanuts in the national standard, and the method can be applied to supervision of pesticide residues in peanuts.

Description

technical field [0001] The invention relates to the technical field of pesticide residue detection, in particular to a detection method for pyraclostrobin, flufenapyr and flufenapyr metabolites in peanut kernels and peanut straws. Background technique [0002] Pyraclostrobin is a methoxyacrylate broad-spectrum fungicide, and its mechanism of action is a mitochondrial respiration inhibitor, that is, by preventing electron transfer in the synthesis of cytochrome bcl, it has the functions of protection, treatment, and leaf penetration. Pyraclostrobin has good control effects on peanut mildew, cucumber powdery mildew, downy mildew, banana scab and leaf spot. [0003] Flufenapyramide is a new type of methoxyacrylate fungicide, the mechanism of action is succinate dehydrogenase inhibitor, both prevention and control, not only can inhibit the respiration of fungi, but also inhibit the germination of spores, the elongation of germination tubes, and the growth of hyphae and spore fo...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/72G01N27/62
CPCG01N30/02G01N30/06G01N30/34G01N30/7266G01N27/62
Inventor 陈增龙张明浩刘子琪郭靖立李薇
Owner INST OF ZOOLOGY CHINESE ACAD OF SCI
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