Rapid detection method for glyphosate, glufosinate-ammonium and aminomethylphosphonic acid in beer

A technology of aminomethylphosphonic acid and glyphosate, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of complex derivatization process, long processing time, increased detection cycle and cost, and improve the derivatization efficiency. , the effect of simplifying operating conditions

Active Publication Date: 2022-06-24
欧陆分析技术服务(苏州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 1. In the prior art, glyphosate and glufosinate are detected separately, resulting in increased detection cycle and cost;
[0011] 2. In the prior art, both detections need to be purified by SPE column, and the pretreatment time is relatively long;
[0012] 3. The derivation process in the prior art is complicated, it needs to be frozen for 0.5h and then derivatized for 1h, and the derivatized solution can be dried and reconstituted before being tested on the machine;
[0013] 4. There is no specific detection method for beer samples in the prior art, and the quantification limit is high

Method used

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  • Rapid detection method for glyphosate, glufosinate-ammonium and aminomethylphosphonic acid in beer

Examples

Experimental program
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Effect test

Embodiment

[0066] The rapid detection method of glyphosate, glufosinate and aminomethylphosphonic acid in beer comprises the following steps in sequence:

[0067] Step S1, pre-processing steps:

[0068] Step S11: weigh 2.0 g of the sample into a 50 mL polypropylene centrifuge tube, add 0.2 mL of 1 mg / L internal standard working solution, add 25 mL of 0.1 N hydrochloric acid solution, shake for 30 minutes, and centrifuge at 4000 rpm for 10 minutes;

[0069] Step S12: take 0.5 mL of the supernatant from step S11 into a 2 mL plastic centrifuge tube, add 0.5 mL of 0.1N potassium hydroxide solution, and vortex for 1 minute;

[0070] Step S13: after the vortexing in step S12, add 1 mL of deionized water, vortex for 1 minute, and centrifuge at 13,000 rpm for 10 minutes;

[0071] Step S14: Take 0.1 mL of the supernatant from step S13 into a 2 mL plastic centrifuge tube, add 0.1 mL of boric acid buffer solution, shake well, add 0.2 mL of 9-fluorenylmethyl chloroform solution, vortex for 1 minute...

no. 1 example

[0101] The invention aims to establish a rapid detection method for glyphosate, glufosinate and aminomethylphosphonic acid in beer. It was extracted with acidified water, the extract was neutralized with potassium hydroxide solution, and then derivatized with 9-fluorenylmethyltrichloromethane in a buffered saline solution, and then measured by liquid chromatography-mass spectrometry. The limit of quantitation was 0.002 mg / Kg.

[0102] Reagents:

[0103] Deionized water, concentrated hydrochloric acid, 9-fluorenylmethyltrichloromethane (FMOC-Cl), acetone, acetonitrile, n-hexane, boric acid, ammonium acetate, sodium hydroxide, potassium hydroxide, glyphosate, glufosinate, Glyphosate 1,2- 13 C 2 - 15 N.

[0104] equipment:

[0105] Balance, liquid chromatography-mass spectrometer / mass spectrometer (AB Sciex 5500), high-speed centrifuge, shaker, ultrasonic water bath, vortexer, oven.

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Abstract

The invention relates to a rapid detection method for glyphosate, glufosinate-ammonium and aminomethylphosphonic acid in beer, which comprises the following steps in sequence: step S1, a pretreatment step and step S2, and an on-machine test step. The present invention does not use SPE column purification, which greatly reduces the pretreatment time; the present invention enables simultaneous detection of glyphosate, glufosinate-ammonium and aminomethylphosphonic acid; the present invention simplifies the derivation operating conditions and improves the derivation efficiency; The present invention uses LC-MS / MS detection, and the limit of quantification can reach 0.010 mg / Kg, which is better than the detection method in the prior art.

Description

technical field [0001] The invention relates to the technical field of detection, in particular to a rapid detection method for glyphosate, glufosinate-ammonium and aminomethylphosphonic acid in beer. Background technique [0002] Glyphosate (PMG) is a potent active chemical in many widely used herbicides, and its use in the European Union is heavily regulated. In recent years, the media has repeatedly reported that glyphosate has been detected in beer, making people pay more and more attention to glyphosate residues in beer. Glufosinate-ammonium has become a non-selective herbicide coexisting with glyphosate and paraquat due to its rapid activity. In the existing GB method, the detection of glyphosate and glufosinate-ammonium is carried out separately, the detection time is relatively long, and the detection limit is relatively high. [0003] At present, the detection methods of glyphosate and its degradation product aminomethylphosphonic acid in plant-derived foods are d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/34G01N30/72
CPCG01N30/02G01N30/06G01N30/30G01N30/34G01N30/72
Inventor 王芳陈奎耿方娜
Owner 欧陆分析技术服务(苏州)有限公司
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