Pretreatment method for measuring pesticides of glyphosate and phosphinothricin in tea leaves

A technology for glyphosate and glufosinate, which is used in the pretreatment of pesticide residue determination and the pretreatment field of glyphosate and glufosinate in tea, which can solve the problem of affecting the quality of glyphosate and glufosinate. It can achieve high sensitivity, reduce the interference of impurities, and meet the needs of residual detection.

Active Publication Date: 2014-06-18
TEA RES INST CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection of glufosinate-ammonium and glyphosate residues in agricultural products usually adopts the detection method of pre-column derivatization-liquid chromatography tandem triple quadrupole mass spectrometry, but tea is a special and complex sample, which contains a large amount of tea Polyphenols, pigments and sugars, during the derivatization reaction of the sample, these substances will interfere with the formation of reaction products, thus affecting the qualitative and quantitative determination of glyphosate and glufosinate-ammonium

Method used

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  • Pretreatment method for measuring pesticides of glyphosate and phosphinothricin in tea leaves
  • Pretreatment method for measuring pesticides of glyphosate and phosphinothricin in tea leaves
  • Pretreatment method for measuring pesticides of glyphosate and phosphinothricin in tea leaves

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A pretreatment method for measuring glyphosate and glufosinate pesticides in tea leaves is carried out through the following steps:

[0015] (1) Extraction: Weigh 2.0 g of tea samples into a 50 mL centrifuge tube, add 15 mL of 0.5 mol / L KOH solution, adjust the pH to above 13, shake well and let stand for 30 min. Centrifuge at 4000 rpm for 10 min, filter to obtain the filtrate, take 3 mL of the filtrate to a 10 mL centrifuge tube, add 5 mol / L hydrochloric acid solution and 0.5 mL strong acid solution to adjust the pH of the sample solution to below 7, shake evenly, and centrifuge at 4000 rpm for 10 min to obtain the extracted liquid.

[0016] (2) Purification: pipette 1 mL of the supernatant after extraction to a 60 mg oasis HLB solid-phase extraction column as 60 mg HLB filler (activation of the column: first add 2 mL of methanol to rinse, then add 2 mL of water to activate), Solid phase extraction is carried out to obtain a solid phase extract. The oasis HLB solid-p...

Embodiment 2

[0018] Example 2 Determination method for glufosinate-ammonium, glyphosate and aminomethylphosphonic acid residues-liquid chromatography-tandem mass spectrometry

[0019] 1. scope

[0020] It is suitable for qualitative identification and quantitative determination of glufosinate-ammonium, glyphosate and aminomethylphosphonic acid residues in green tea, black tea, Pu-erh tea and oolong tea. The detection limits of glufosinate-ammonium, glyphosate and aminomethylphosphonic acid are 0.075mg / kg, 0.050mg / kg and 0.050mg / kg respectively.

[0021] 2. method summary

[0022] The sample was extracted by potassium hydroxide solution, purified by HLB column, derivatized by FMOC-CL, detected by ultra-high pressure liquid chromatography-tandem mass spectrometer, and quantified by external standard method.

[0023] 3. Reagents and Materials

[0024] Water is secondary ultrapure water, unless otherwise specified, all reagents are analytically pure. Methanol (purified by liquid ...

Embodiment 3

[0068] Accurately weigh 2.0 g of organic tea samples into a 50 mL centrifuge tube, add the mixed standard at a concentration equivalent to 0.8 mg / kg, add 15 mL of water, shake well and let stand for 30 min. After centrifugation at 4000 rpm for 10 min, the filtrate was obtained by filtration.

[0069] Pipette 1 mL of the extract to a 60 mg HLB solid-phase extraction cartridge (column activation: first add 2 mL of methanol to rinse, then add 2 mL of water to activate), transfer the post-column filtrate to a 5 mL centrifuge tube, add 1 mol / Shake 0.25 mL of L KOM solution, then add 0.48 mL sodium borate buffer solution, shake well and add 0.18 mL FMOC-CL derivative solution, shake well and let stand overnight. The derivatized liquid sample was centrifuged at 10,000 rpm for 10 min, and passed through a 0.45 μm water filter membrane for analysis by liquid chromatography-tandem mass spectrometry.

[0070] Since this example only uses water as the extraction sol...

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Abstract

The invention provides a pretreatment method for measuring pesticides of glyphosate and phosphinothricin in tea leaves. In general, acidic precipitation, solid phase extraction, precolumn derivatization and a liquid chromatograph / mass spectrometer are used for measuring, and a method for measuring the residual amounts of glyphosate and phosphinothricin in the tea leaves by using the liquid chromatograph / mass spectrometer is established. In the method, a large quantity of tea polyphenols in the tea leaves are precipitated, so that the deviation efficiency of solid phase extraction liquid and 9-fluorenylmethyl chloroformate is increased, the interference of impurities is reduced, and the high sensitivity is realized. The method is accurate, efficiency and stable, can meet the requirement of residue detection, and can be applied to the qualitative and quantitative analysis of the glyphosate and the phosphinothricin in the various tea leaves.

Description

technical field [0001] The invention belongs to the field of determination of pesticide residues, and relates to a pretreatment method for determination of pesticide residues, in particular to a pretreatment method for determination of glyphosate and glufosinate pesticides in tea leaves. Background technique [0002] Pesticide residue refers to the phenomenon that a part of pesticide remains directly or indirectly in grains, vegetables, fruits, aquatic products, soil and water after the application of pesticide in agricultural production. Glyphosate is an excellent and efficient herbicide, and it is also the most widely used organophosphorus herbicide in the world. Glufosinate-ammonium is another herbicide with excellent performance after glyphosate. Aminomethyl phosphate is the main metabolite of glyphosate. Glyphosate and glufosinate-ammonium, as new organophosphorus herbicides, have long been considered as low-toxic and safe herbicides, and are widely used in agricult...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/14
Inventor 王川丕诸力刘新
Owner TEA RES INST CHINESE ACAD OF AGRI SCI
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