Special solid-phase extraction cartridge for glyphosate and its metabolite aminomethylphosphonic acid and its application

A solid-phase extraction cartridge, aminomethylphosphonic acid technology, applied in the fields of food safety and analytical chemistry, can solve problems such as unreported, and achieve the effects of saving solvent, good stability and large adsorption capacity

Inactive Publication Date: 2016-01-20
INSPECTION & QUARANTINE TECH CENT OF FUJIAN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Magnesium-aluminum binary hydrotalcite (LayeredDoubleHydroxides, LDHs) is a typical anionic layered material. Due to its special layered structure, it can be calcined under certain conditions to obtain a composite oxide with a large specific surface area. It can be reabsorbed under certain conditions. The anions in the water are thus restored to a layered structure of hydrotalcite. This unique "memory effect" structure allows hydrotalcite to be used as an efficient anion absorbent. At present, hydrotalcite has been used as an adsorbent for inorganic and organic anion pollutants. There are few reports, such as the use of hydrotalcite to adsorb dyes in wastewater, and the use of hydrotalcite as a chemical slow-release agent for glyphosate, etc., but the use of hydrotalcite as an adsorption material for solid-phase extraction columns has not been reported

Method used

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  • Special solid-phase extraction cartridge for glyphosate and its metabolite aminomethylphosphonic acid and its application
  • Special solid-phase extraction cartridge for glyphosate and its metabolite aminomethylphosphonic acid and its application

Examples

Experimental program
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Effect test

Embodiment 1

[0021] A special solid phase extraction cartridge for glyphosate and its metabolite aminomethylphosphonic acid is applied to the separation, enrichment and purification of glyphosate and its metabolite aminomethylphosphonic acid in tea.

[0022] Sample extraction:

[0023] Weigh about 200g of the sample, put it into the pulverizer, homogenize, and mix well. Weigh 1.0g (accurate to 0.01g) of a homogeneous sample into a 50mL polyethylene centrifuge tube with a stopper, add 5.00mL 0.1% formic acid water, fully shake for 1min, ultrasonically extract for 30min, and centrifuge at 4500r / min 5min, take the supernatant; add 5.00mL 0.1% formic acid water to extract again, combine the supernatants to make the volume to 10.0mL, and wait for purification.

[0024] Purification of special solid phase extraction cartridges for glyphosate and its metabolite aminomethylphosphonic acid

[0025] Take 2.0 mL of the supernatant and add it to the GLY-AMPA special column activated with 3 mL of methanol a...

Embodiment 2

[0031] A special solid phase extraction cartridge for glyphosate and its metabolite aminomethylphosphonic acid is applied to the separation, enrichment and purification of glyphosate and its metabolite aminomethylphosphonic acid in rice.

[0032] Sample extraction:

[0033] Weigh about 200g of the sample, put it into the pulverizer, homogenize, and mix well. Weigh 1.0g (accurate to 0.01g) of a homogeneous sample into a 50mL polyethylene centrifuge tube with a stopper, add 5.00mL 0.1% formic acid water, fully shake for 1min, ultrasonically extract for 30min, and centrifuge at 4500r / min 5min, take the supernatant; add 5.00mL 0.1% formic acid water to extract again, combine the supernatants and dilute to 10.0mL, to be purified.

[0034] Purification of special solid phase extraction cartridges for glyphosate and its metabolite aminomethylphosphonic acid

[0035] Take 2.0 mL of the supernatant and add it to the GLY-AMPA special column activated with 3 mL of methanol and 3 mL of 0.1% fo...

Embodiment 3

[0041] A special solid phase extraction cartridge for glyphosate and its metabolite aminomethylphosphonic acid is applied to the separation, enrichment and purification of glyphosate and its metabolite aminomethylphosphonic acid in soybeans.

[0042] Sample extraction:

[0043] Weigh about 200g of the sample, put it into the pulverizer, homogenize, and mix well. Weigh 1.0g (accurate to 0.01g) of a homogeneous sample into a 50mL polyethylene centrifuge tube with a stopper, add 5.00mL 0.1% formic acid water, fully shake for 1min, ultrasonically extract for 30min, and centrifuge at 4500r / min 5min, take the supernatant; add 5.00mL 0.1% formic acid water to extract again, combine the supernatants to make the volume to 10.0mL, and wait for purification.

[0044] Purification of special solid phase extraction cartridges for glyphosate and its metabolite aminomethylphosphonic acid

[0045] Take 2.0 mL of the supernatant and add it to the GLY-AMPA special column activated with 3 mL of metha...

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Abstract

The invention provides a special solid-phase extraction column for glyphosate and its metabolites and its application. The filler is composed of anion adsorption filler, acid substance adsorption filler and filter aid; the anion adsorption filler is magnesium-aluminum binary water Talc, the molecular composition formula is MgAl3(OH)16CO3·4H2O; the acidic substance adsorption filler is ethylenediamine-N-propylsilane; the filter aid is diatomaceous earth celite? 545 filler; the weight ratio of the anion adsorption filler, acid substance adsorption filler and filter aid is 2:2:1. The special extraction filler for glyphosate and its metabolite aminomethylphosphonic acid provided by this application has strong adsorption capacity and high column capacity, and can effectively remove vegetable oil, fat, acidic substances and other impurities in food, and the recovery rate can reach 90% It is more than %, stable and reproducible, which overcomes the defects of unstable alumina activity and small capacity of anion exchange column in the traditional method.

Description

technical field [0001] The invention relates to the fields of analytical chemistry and food safety, and relates to the preparation method and application of a special solid-phase extraction column (GLY-AMPA column) for the simultaneous extraction of glyphosate and its metabolite aminomethylphosphonic acid, mainly used in food (including Highly selective separation, enrichment and purification of glyphosate and its metabolite aminomethylphosphonic acid in water, food of animal origin, food of plant origin, etc.). Background technique [0002] Glyphosate (Glyphosate, Gly), chemical name N-(phosphonomethyl) aminoacetic acid, is the broad-spectrum non-selective herbicide most widely used and produced in the world at present, aminomethylphosphonic acid (aminomethylphosphonic acid, AMPA) is the main metabolite of glyphosate, its chemical properties are similar to its parent, and its structural formula is shown in Table 1. Glyphosate and its main metabolite, aminomethyl phosphate,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30B01D15/22G01N1/34G01N1/40
Inventor 刘正才蔡春平林永辉刘素珍
Owner INSPECTION & QUARANTINE TECH CENT OF FUJIAN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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