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Precolumn derivatization-UPLC(ultra performance liquid chromatography)-ESI(electronic spray ion)+-MS/MS (mass spectrometry) detection method of glyphosate and glufosinate-ammonium pesticide residue in tea

A technology for pesticide residues and glyphosate, which is used in measuring devices, instruments, scientific instruments, etc., can solve the problem of not meeting the requirements of pesticide residue analysis and testing, no glyphosate and glufosinate, and no published tests. Standards and other issues to overcome the derived competition, fewer steps, and low detection limits

Active Publication Date: 2015-06-24
MENGHAI TEA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] ①Liquid chromatography: There is no conjugated double bond in the molecular structure of glyphosate and glufosinate-ammonium, only n-π conjugation exists, and there is basically no absorption in the ultraviolet region. The sensitivity of direct measurement is poor, and it cannot meet the analysis and testing of pesticide residues. Require
[0007] In addition, the above methods only involve the analysis of a single pesticide residue, so far there has not been a method that can simultaneously detect the content of glyphosate and glufosinate (especially glufosinate) in tea, and relevant institutions or national units have not released any Detection standard, no relevant research literature was retrieved

Method used

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  • Precolumn derivatization-UPLC(ultra performance liquid chromatography)-ESI(electronic spray ion)+-MS/MS (mass spectrometry) detection method of glyphosate and glufosinate-ammonium pesticide residue in tea
  • Precolumn derivatization-UPLC(ultra performance liquid chromatography)-ESI(electronic spray ion)+-MS/MS (mass spectrometry) detection method of glyphosate and glufosinate-ammonium pesticide residue in tea
  • Precolumn derivatization-UPLC(ultra performance liquid chromatography)-ESI(electronic spray ion)+-MS/MS (mass spectrometry) detection method of glyphosate and glufosinate-ammonium pesticide residue in tea

Examples

Experimental program
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Effect test

Embodiment 1

[0113] Example 1. Detection of glyphosate and glufosinate pesticide residues in fermented tea leaves

[0114] The detection of this embodiment is completed according to the aforementioned steps 1)-9), the same content will not be repeated, and the changes are as follows:

[0115] 1) Mobile phase B is pure acetonitrile.

[0116] 2) The optimal conditions for derivation are 50g / L sodium borate buffered saline solution and 20g / L FMOC-Cl acetone solution, and the derivation time is the shortest 2h. Mix for 1 min, centrifuge for 5 min, and pass through a 0.2 μm organic filter.

[0117] 4) The UPLC-ESI+-MS / MS spectrum of the glyphosate standard solution in MRM mode is as follows Figure 7 As shown, it can be seen that the chromatographic peaks of the glyphosate ion m / z88 (A panel), m / z214 (B panel) and the total ion diagram (C panel) are good, symmetrical, and sensitive, and fully meet the requirements of pesticide residues. Quantitative analysis test requirements; UPLC-ESI of gl...

Embodiment 2

[0124] Example 2, Determination of residual amounts of glyphosate and glufosinate-ammonium pesticides in sun-dried green hair tea

[0125] The detection of this embodiment is completed according to the aforementioned steps 1)-9). Steps 1)-4) are the same as in Example 1. The detection part operates as follows:

[0126] 5)-6) Tea sample preparation and extraction: Take the raw material sample of sun-dried green tea as an example, the tea sample is ground and sieved according to GB / T8303 to obtain the tea sample to be tested; accurately weigh 1g of the ground tea sample (accurate to 0.001g) in 80mL capped centrifuge tubes (two parallel sample numbers are i and ii respectively), considering that glyphosate and glufosinate-ammonium may not be detected in the tea leaves, first add equal concentration to the two capped centrifuge tubes Add 1mL of 5.5μg / mL mixed standard, add 20mL ultrapure water, vortex mix and let stand for 2min, then add 5mL dichloromethane, extract by ultrasoni...

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Abstract

The invention discloses a precolumn derivatization-UPLC(ultra performance liquid chromatography)-ESI(electronic spray ion)+-MS / MS (mass spectrometry) detection method of glyphosate and glufosinate-ammonium pesticide residue in tea, sodium borate is used as a buffer salt, a relatively pure target derived product can be obtained by derivatization of glyphosate and glufosinate-ammonium and FMOC-Cl and then ultra performance liquid chromatography (UPLC) washing out and separation, and response signals can be detected by tandem mass spectrometry (MS-MS). According to the method, competition between the two pesticide residue derivatization can be eliminated, the detection effect caused by matrix effect can be effectively weakened, and the derivatization time is shortened. By experimental verification, the detection method of glyphosate and glufosinate-ammonium pesticide (herbicide) residue in tea has the characteristics of being efficient, fast and accurate, good in sensitivity and the like, is applicable in detection of the glyphosate and glufosinate-ammonium pesticide residue in tea samples of sundried green crude tea, fermented tea and substitutional tea (green food substitutional tea of agricultural industry standards of NY / T2140-2012 of the people's Republic of China) and finished tea (brick tea, Tuo tea, melon-shaped tea, cake tea, scattered tea and bagged tea and the like).

Description

technical field [0001] The invention belongs to the field of food detection, in particular to pre-column derivatization-UPLC-ESI of glyphosate and glufosinate-ammonium pesticide (herbicide) residues in tea (tea base or similar tea base) + - MS / MS detection method. Background technique [0002] Glyphosate and glufosinate-ammonium are two broad-spectrum contact herbicides that are widely used in agriculture, forestry and horticulture. Due to the increasing and unreasonable use of glyphosate and glufosinate-ammonium herbicides, they are often found in environmental water samples, soil and plants. Such long-term accumulation will cause environmental pollution and cause serious harm to human health. threaten. With the release and implementation of GB2763-2012 (National Food Safety Standard for Maximum Residue Limits of Pesticides in Food), glyphosate and glufosinate-ammonium have been added as mandatory inspection items for pesticide residues in tea. [0003] Glyphosate and gl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 陈孝权吴晓刚
Owner MENGHAI TEA IND
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