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

A technology of aminomethylphosphonic acid and middle glyphosate, which is used in the rapid detection of glufosinate and aminomethylphosphonic acid, and the field of glyphosate in beer, can solve the problem of increased detection cycle and cost, complicated derivation process, Dealing with problems such as long processing time, to achieve the effect of reducing time, improving derivation efficiency, and lowering the limit of quantification

Active Publication Date: 2020-06-05
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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Embodiment

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

[0067] Step S1, pre-processing steps:

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

[0069] Step S12: Take 0.5 mL of the supernatant in 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 vortexing in step S12, add 1 mL of deionized water, vortex for 1 minute, and centrifuge at 13000 rpm for 10 minutes;

[0071] Step S14: Take 0.1 mL of the supernatant in 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 trichloromethane solution, vortex for 1 minute, and let stand Af...

no. 1 example

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

[0102] Reagent:

[0103] Deionized water, concentrated hydrochloric acid, 9-fluorenylmethyltrichloromethane (FMOC-Cl), acetone, acetonitrile, n-hexane, boric acid, ammonium acetate, sodium hydroxide, potassium hydroxide, glyphosate, glufosinate-ammonium, 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, vortex apparatus, oven.

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Abstract

The invention relates to a rapid detection method for glyphosate, glufosinate-ammonium and aminomethylphosphonic acid in beer. The rapid detection method sequentially comprises the following steps: S1, a pretreatment step and S2, a computer test step. According to the method, an SPE column is not used for purification, so that the pretreatment time is greatly shortened; according to the invention,glyphosate, glufosinate-ammonium and aminomethylphosphonic acid are simultaneously detected; according to the method, the derivation operation conditions are simplified, and the derivation efficiencyis improved; according to the method, LC-MS / MS detection is adopted, the limit of quantitation can reach 0.010 mg / Kg, and the method is superior to a 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), the potent active chemical ingredient in many widely used herbicides, is strictly regulated in the European Union. In recent years, the media has repeatedly reported that glyphosate was detected in beer, making people pay more and more attention to glyphosate residues in beer. Glufosinate-ammonium is a non-selective herbicide co-existing with glyphosate and paraquat due to its fast action. In the existing GB method, the detection of glyphosate and glufosinate-ammonium is carried out separately, the detection time is longer and the detection limit is higher. [0003] At present, the detection methods for glyphosate and its degradation product aminomethylphosphonic acid residues in food of plant origin are divided into two categor...

Claims

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Application Information

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Patent Type & Authority Applications(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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