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Method for splitting fenpropimorph enantiomer and analyzing residues in agricultural products

A technology of enantiomer resolution and fenpropimorph, which is applied in the field of pesticide residue analysis in agricultural products, can solve the problems of inability to obtain monomer samples, unclear differences in bactericidal activity and differences in beneficial biological toxicity residues, etc., and achieve high purity and preparation The effect of large quantity and broad application prospects

Active Publication Date: 2021-07-27
TEA RES INST CHINESE ACAD OF AGRI SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, none of the analysis and detection methods involved the level of enantiomers, and it is not clear about the difference in bactericidal activity of the R-body or S-body, the toxicity to beneficial organisms, and the difference in the residues of enantiomers in agricultural products and the environment. The possible reason is that it is not possible to obtain Monomer samples and no enantiomer-specific residue analysis method

Method used

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  • Method for splitting fenpropimorph enantiomer and analyzing residues in agricultural products
  • Method for splitting fenpropimorph enantiomer and analyzing residues in agricultural products
  • Method for splitting fenpropimorph enantiomer and analyzing residues in agricultural products

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Experimental program
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Effect test

Embodiment 1

[0047] Embodiment 1: Separation of fenpropimorph racemate by liquid chromatography ultraviolet detector

[0048] On the liquid chromatograph, inject 1000mg L -1 Standard solution of fenpropimorph racemate, separated by SuperchiralS-OJ column (0.46cm I.D.×15cm L, 5μm), mobile phase is methanol / diethylamine (100 / 0.05), flow rate 0.80mL min -1 , injection volume 20μL, column temperature 30°C, UV detector wavelength 230nm, chromatogram see figure 1 , the separation data of fenpropimorph enantiomers are shown in Table 1. It shows that the standard solution of fenpropimorph racemate has peaks at 4.114min and 4.649min, which are two enantiomers in fenpropimorph racemate respectively.

[0049] Table 1 Liquid Chromatography UV Detector Separation Data of Fenpropimorph Racemate

[0050]

Embodiment 2

[0051] Example 2: Liquid Chromatography Laser Polarizer Detector Separation and Detection of Fenpropimorph Racemate

[0052] On the liquid chromatograph, inject 1000mg L -1 Standard solution of fenpropimorph racemate, separated by SuperchiralS-OJ column (0.46cm I.D.×15cm L, 5μm), mobile phase is methanol / diethylamine (100 / 0.05), flow rate 0.80mL min -1 , injection volume 20μL, column temperature 30°C, laser polarimeter detector wavelength 670nm, see spectrum figure 2 , it can be determined that the first effluent is (-)-fenpropimorph, and the latter is (+)-fenpropimorph.

Embodiment 3

[0053] Example 3: Liquid Chromatography UV Detector Detects (-)-Fenpropimorph Monomer Obtained After Resolution and Preparation

[0054] On the liquid chromatograph, the (-)-fenpropimorph single solution obtained by the resolution of sample injection example 1 was separated by Superchiral S-OJ chromatographic column (0.46cm I.D.×15cm L, 5 μm), and the mobile phase was Methanol / diethylamine (100 / 0.05), flow rate 0.80mL min -1 , injection volume 20μL, column temperature 30°C, UV detector wavelength 230nm, chromatogram see image 3 , see Table 2 for the separation data of fenpropimorph enantiomers. It shows that (-)-fenpropimorph monomer solution has a peak at 4.135min, and the purity reaches more than 99%.

[0055] Table 2 liquid chromatography ultraviolet detector detects the data of (-)-fenpropimorph monomer obtained after resolution and preparation

[0056]

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Abstract

The invention discloses a method for splitting a fenpropimorph enantiomer and analyzing residues in agricultural products. The method comprises the following steps: 1) preparing a fenpropimorph racemate solution; and 2) separating and confirming the fenpropimorph racemate. The resolution can effectively separate the chiral fenpropimorph of the butylphenylmorpholine, has the characteristics of high purity of the separated monomer and large preparation amount, and can be used for analyzing and researching the activity, toxicity and residual metabolism of the monomer. The chiral pesticide residue analysis method comprises the following steps: 1) extracting and purifying a sample; (2) carrying out gradient elution separation by adopting a C-3 chromatographic column, and carrying out ultra-high performance liquid chromatography-tandem mass spectrometry to detect the bufenmorph enantiomer; 3) calculating standard curves and linear correlation coefficients of the tetramorph enantiomers in different matrix solutions, and 4) calculating the addition recovery rate, the relative standard deviation, the detection limit and the quantitation limit of the method. The residue analysis method meets the residue analysis requirement, and an analysis method can be provided for research and detection of tetramorph enantiomer residues in agricultural products such as tea.

Description

technical field [0001] The invention belongs to the technical field of enantiomer resolution of chiral compounds and pesticide residue analysis in agricultural products such as tea, and specifically relates to the separation and preparation of fenpropimorph enantiomers and its residue analysis method in agricultural products such as tea. Background technique [0002] Fenpropimorph, (±)-cis-4-[3-(4-tert-butylphenyl)-2-methylpropyl]-2,6-dimethylmorpholine,C 20 h 33 NO, CAS No. 67564-91-4) was first reported by K.Bohnen and A.Pfiffner in 1979, a kind of morpholine fungicide and An ergosterol reduction inhibitor, used to prevent and control important diseases in the seedling stage of crops such as grains, beans and sugar beets, such as rust, powdery mildew, cotton blight, cereal smut, etc. The chemical structure of fenpropimorph is unique. Although there are 3 chiral carbon centers in its structure, the two methyl groups on its morpholine ring have a cis configuration. Therefo...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/74G01N30/8679G01N2030/047G01N2030/065
Inventor 张新忠黎洪霞奚文伟顾建波罗逢健
Owner TEA RES INST CHINESE ACAD OF AGRI SCI