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A kind of determination method of glyphosate, aminomethylphosphonic acid and glufosinate-ammonium in food

A technology of aminomethylphosphonic acid and glyphosate, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of unstable recovery rate of glyphosate, small adsorption capacity, and large eluent volume.

Active Publication Date: 2020-10-23
烟台杰科检测服务有限公司
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  • Abstract
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Problems solved by technology

[0003] Glyphosate and its main degradation products Aminomethyl phosphonic acid (AMPA) and glufosinate-ammonium have similar chemical structures, both are easily soluble in water, insoluble in general organic solvents, difficult to volatilize, and lack color development. and fluorescent groups and other characteristics, so it is difficult to detect by conventional methods
Our national standard can only detect glyphosate and its metabolite aminomethylphosphonic acid. Currently, there is no national standard for the detection method of glufosinate in food, such as GB / T 23750-2009 "Glyphosate Residues in Plant Products Determination of Glyphosate Residues in Food by Gas Chromatography-Mass Spectrometry", NY / T 1096-2006 "Determination of Glyphosate Residues in Food", SN / T 1923-2007 "Determination of Glyphosate Residues in Imported and Exported Foods by Liquid Chromatography- Mass Spectrometry Mass Spectrometry", when using liquid chromatography-mass spectrometry to detect glyphosate residues in food according to the above three standards, the experimental process consumes a lot of reagents and a lot of operating steps, especially the use of cation exchange columns (CAX), Eluent elution, the price of the column is relatively expensive, the column volume is large, the adsorption capacity is small, and there are still a lot of impurities after purification, and the eluent volume in the method is large and the proportion of water is large, it is not easy to evaporate to dryness during concentration, pressurization The recovery rate of glyphosate is easy to be unstable during the rotary evaporation process, which requires a lot of time and energy in actual work
[0004] Domestic reports on the simultaneous detection of glyphosate, aminomethylphosphonic acid, and glufosinate-ammonium are limited to tea and drinking water, and there is a lack of research on methods for the simultaneous detection of the three pesticides in food

Method used

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  • A kind of determination method of glyphosate, aminomethylphosphonic acid and glufosinate-ammonium in food
  • A kind of determination method of glyphosate, aminomethylphosphonic acid and glufosinate-ammonium in food
  • A kind of determination method of glyphosate, aminomethylphosphonic acid and glufosinate-ammonium in food

Examples

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Embodiment 1

[0025] Example 1. A method for determining glyphosate, aminomethylphosphonic acid and glufosinate-ammonium in food. Take the above apple sample and detect its residual content of glyphosate, aminomethylphosphonic acid and glufosinate-ammonium. The steps are as follows :

[0026] (1) Extraction: Weigh 5.0g apple sample into a 50mL centrifuge tube, add 20mL ultrapure water, 2.0mL 2mol / L hydrochloric acid solution, vortex thoroughly, then add 10mL dichloromethane, vortex to mix well Then, ultrasonic extraction was performed for 20 minutes, and centrifuged at 4000r / min for 5 minutes;

[0027] (2) Purification: The 5.0 mL of the aqueous solution obtained after centrifugation in step (1) is purified through a solid phase extraction column containing lipophilic hydrophilic copolymers, and collected directly. The solid phase extraction column uses 6 mL methanol and 6 mL 0.1 % Formic acid water, 3 mL centrifugal extract solution pretreatment;

[0028] (3) Derivation: Pipette 1.0 mL of the p...

Embodiment 2

[0040] Example 2. A method for determining glyphosate, aminomethylphosphonic acid and glufosinate-ammonium in food. Take the spinach sample above and detect its residual content of glyphosate, aminomethylphosphonic acid and glufosinate-ammonium. The steps are as follows :

[0041] (1) Extraction: Weigh 5.0 g of spinach sample into a 50 mL centrifuge tube, add 20 mL of ultrapure water, 2.0 mL of 2 mol / L hydrochloric acid solution, vortex thoroughly, and then add 10 mL of dichloromethane, vortex to mix well Then, ultrasonic extraction was performed for 20 minutes, and centrifuged at 4000r / min for 5 minutes;

[0042] (2) Purification: The 5.0 mL of the aqueous solution obtained after centrifugation in step (1) is purified through a solid phase extraction column containing lipophilic hydrophilic copolymers, and collected directly. The solid phase extraction column uses 6 mL methanol and 6 mL 0.1 % Formic acid water, 3 mL centrifugal extract solution pretreatment;

[0043] (3) Derivatio...

Embodiment 3

[0055] Example 3, a method for determining glyphosate, aminomethylphosphonic acid and glufosinate-ammonium in foods, taking the above wheat flour sample and detecting its residual content of glyphosate, aminomethylphosphonic acid and glufosinate-ammonium, the steps are as follows :

[0056] (1) Extraction: Weigh 5.0g of wheat flour sample into a 50mL centrifuge tube, add 20mL ultrapure water, 2.0mL 2mol / L hydrochloric acid solution, vortex thoroughly, then add 10mL dichloromethane, vortex to mix well After that, ultrasonic extraction was performed for 20 minutes and centrifuged at 4000 r / min for 5 minutes;

[0057] (2) Purification: The 5.0 mL of the aqueous solution obtained after centrifugation in step (1) is purified through a solid phase extraction column containing lipophilic hydrophilic copolymers, and collected directly. The solid phase extraction column uses 6 mL methanol and 6 mL 0.1 % Formic acid water, 3 mL centrifugal extract solution pretreatment;

[0058] (3) Derivati...

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Abstract

The invention discloses a method for determining glyphosate, aminomethylphosphonic acid and glufosinate in food. The method comprises the following steps: extracting a sample with hydrochlorinated ultrapure water; then subjecting crude liquid extract obtained in the previous step to liquid-liquid distribution via dichloromethane; carrying out purification with a lipophilic hydrophilic copolymer solid-phase extraction column to remove impurities; then subjecting the liquid extract and 9-fluorenylmethyl chloroformate [FMOC-Cl] to a derivative reaction under the condition of a pH value of 9; andthen carrying out detection via ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC / MS / MS) and quantification via an external standard method, wherein the average recovery rateof glyphosate, aminomethylphosphonic acid and glufosinate residues is 72 to 116%, and relative standard deviation (RSD) is no more than 10%. The method provided by the invention is simple to operate,good in reproducibility, and capable of effectively removing impurities in the extract of the sample and simultaneously carrying out qualitative and quantitative analysis on the three pesticides consisting of glyphosate, aminomethylphosphonic acid and glufosinate in food; and the method can meet technical requirements of security detection and provides powerful technical support for food safety and export trade.

Description

Technical field [0001] The invention belongs to the technical field of food detection methods, and particularly relates to a method for determining glyphosate, aminomethylphosphonic acid and glyphosate in food. Background technique [0002] Glyphosate and glufosinate ammonium are both broad-spectrum herbicides. In recent years, as the problem of glyphosate-resistant weeds has become increasingly serious, glufosinate has become the most popular recently due to its effectiveness. One of the products. In order to improve the effect of weed control, there are research and development and registration of glyphosate and glufosinate-ammonium compound products at home and abroad to improve the effect of weed control. The use of glyphosate, glufosinate, or related compound products at home and abroad has been increasing year by year, and the problem of its residues has attracted more and more attention. [0003] Glyphosate and its main degradation product, Aminomethyl phosphonic acid (AMP...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 宫明杰池连学张禧庆郭海霞
Owner 烟台杰科检测服务有限公司
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