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A method for the determination of glyphosate and its metabolite aminomethylphosphonic acid residues in food

A technology of aminomethylphosphonic acid and glyphosate, applied in the field of detection, can solve the problems of simultaneous analysis, cumbersome steps, low recovery rate, etc., and achieve good response and peak shape, good reproducibility, accurate and reliable quantification. Effect

Inactive Publication Date: 2017-09-05
INSPECTION & QUARANTINE TECH CENT OF XIAMEN ENTRY EXIT INSPECTION & QUARANTINE BUREAU +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] Since glyphosate and its metabolite aminomethylphosphonic acid are strong polar compounds, insoluble in most organic solvents, have no ultraviolet absorption, and are not volatile, detection by gas chromatography or high performance liquid chromatography often requires the aid of Derivatization before or after the column has cumbersome steps, poor repeatability, and difficult quality control; or ion chromatography is used, but due to its strong retention when separating GLY, the separation must use sodium carbonate as a strong eluent, while other The weak retention of common anions prevents the simultaneous analysis of GLY and other anions, and is limited to the test of relatively simple matrices such as water
[0005] Invention patent CN 101646348B discloses a method for the presence or content of glyphosate, N-acetylglyphosate, N-acetyl AMPA or aminomethylphosphonic acid (AMPA) and its various metabolites in a test matrix. Ion-exchange solid-phase extraction column is used for purification. Many samples such as bananas, lemons, tea powder, etc. will block the solid-phase extraction column and make it impossible to operate. Moreover, the recovery rate is very low, less than 5%, and expensive internal standards need to be used to calibrate the recovery.
Invention patent CN 103529148B discloses a detection method for herbicide glyphosate and its metabolite aminomethylphosphonic acid residues in food, which mainly consists of five steps: extraction, adsorption, rinsing, elution, and qualitative and quantitative analysis. It uses magnesium-aluminum binary hydrotalcite to absorb the residual glyphosate and aminomethylphosphonic acid in the extract, and then washes the magnesium-aluminum binary hydrotalcite with water and methanol respectively. Glyphosate and aminomethylphosphonic acid in the desorption, troublesome operation

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  • A method for the determination of glyphosate and its metabolite aminomethylphosphonic acid residues in food
  • A method for the determination of glyphosate and its metabolite aminomethylphosphonic acid residues in food
  • A method for the determination of glyphosate and its metabolite aminomethylphosphonic acid residues in food

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] Embodiment 1: Preparation of standard working solution

[0079] The standard working solution is a standard working solution of three concentrations prepared from glyphosate and its metabolite aminomethylphosphonic acid. The specific preparation method is: (1) Accurately weigh glyphosate and its metabolite aminomethylphosphonic acid Each 10mg of phosphonic acid standard substance was adjusted to 10mL with water to prepare a standard stock solution with a concentration of 1mg / mL; (2) absorb the standard stock solution, dilute it with water, and prepare a standard intermediate solution with a concentration of 10μg / mL respectively, Store below 4°C in the dark and refrigerate; (3) Take a certain amount of standard intermediate solution and dilute it with aqueous solution to form a series of standard working solutions of 0.01, 0.02, 0.05, 0.1, 0.2, and 0.5 μg / mL, and keep it below 4°C. Keep light and refrigerated.

Embodiment 2

[0080] Example 2: Analysis of Standard Working Solution Using High Performance Liquid Chromatography-Tandem Triple Quadrupole Mass Spectrometer

[0081] The parameters set by the high-performance liquid chromatography-tandem triple quadrupole mass spectrometer should ensure that the measured component and other components can be effectively separated during chromatographic determination, such as the following parameters:

[0082] (1) Liquid phase conditions:

[0083] 1) Chromatographic column: NH2P-502D column, length 150mm, inner diameter 2.0mm, particle size 5μm or equivalent;

[0084] 2) Mobile phase: A: 5mmol / L ammonium acetate aqueous solution (adjust pH=10-11 with ammonia water), B: acetonitrile solution; flow rate: 0.25mL / min, see Table 1 for the gradient elution procedure;

[0085] 3) Column temperature: 35°C; 4) Injection volume: 10 μL.

[0086] Table 1 Mobile phase gradient elution program

[0087] time (min) Mobile phase A(%) Mobile phase B(%) 0...

Embodiment 3

[0094] Embodiment 3: drawing standard working solution regression curve

[0095] Using high performance liquid chromatography-tandem triple quadrupole mass spectrometry, a series of standard working solutions in embodiment 1 are respectively carried out liquid chromatography-tandem mass spectrometry, and the instrument parameters are set according to those listed in embodiment 2 Carry out, then take the concentration x of glyphosate and its metabolite aminomethylphosphonic acid in the standard working solution as the abscissa, and take the corresponding measured quantitative ion peak area y as the ordinate, draw the regression curve of the standard working solution, see image 3 . From image 3 It can be seen that the concentration of glyphosate and its metabolite aminomethylphosphonic acid in the solution is linearly related to the corresponding measured quantitative ion peak area.

[0096] According to the straight line drawn, the slope and intercept of the straight line a...

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Abstract

The invention relates to a method for detecting the residual quantities of glyphosate and phosphonic acid being a metabolite of glyphosate in food. The method comprises the following steps: preparation of a standard working solution, preparation of a food sample test solution, drawing of a standard working solution regression curve and calculation of the residual quantities of glyphosate and phosphonic acid in a food sample. The method has the advatnages that the residual quantities of glyphosate and phosphonic acid in food can be detected accurately, wherein the detection results are accurate, reliable, and high in reproducibility; a dialysis bag and a divinyl benzene solid phase extraction cartridge are adopted for purification to avoid blockage, ensure 80 percent or high recovery rate, and avoid use of expensive internal standard substances for recovery correction; as an NH2P-502D cartridge is adopted, and 5 mmol / L liquid ammonium acetate and acetonitrile are adopted as mobile phases, the method is excellent in response and peak shape.

Description

technical field [0001] The invention relates to a detection method, in particular to a method for determining the residual amount of glyphosate and its metabolite aminomethylphosphonic acid in food. Background technique [0002] Glyphosate (Glyphosate, GLY), chemical name N-(phosphonomethyl) glycine, is the broad-spectrum non-selective herbicide that is most widely used and produced in the world, but its unreasonable use will still lead to its excessive residue in plants. Glyphosate and its main metabolite, aminomethylphosphonic acid (AMPA), have similar toxicities to organophosphorus compounds, mainly causing nervous system dysfunction by inhibiting the activity of cholinesterase. Cases of water pollution, vegetation destruction, and livestock poisoning have also increased year by year. [0003] my country's "National Food Safety Standard Maximum Residue Limits of Pesticides in Food" (GB 2763-2014) came into effect on August 1, 2014. The strong inspection (required inspec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 吴敏杜凤君严丽娟余宇成林立毅周爽徐敦明黄志强
Owner INSPECTION & QUARANTINE TECH CENT OF XIAMEN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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