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Solid phase extraction-liquid chromatography-mass spectrometric detection method of glyphosate in aquatic products

A liquid chromatography and glyphosate technology, which is applied in the field of solid-phase extraction-liquid chromatography-mass spectrometry detection of glyphosate in aquatic products, can solve the problems of soil microorganisms, the probability of soybean root diseases, and threats to human health. , to achieve the effect of good extraction effect, low consumption cost and short time consumption

Active Publication Date: 2016-11-23
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although glyphosate has always been considered a "safe" herbicide, its long-term and large-scale use will still affect soil microorganisms and the probability of soybean root diseases; some studies have also shown that glyphosate can accumulate in the environment and in organisms , and ultimately threaten human health

Method used

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  • Solid phase extraction-liquid chromatography-mass spectrometric detection method of glyphosate in aquatic products
  • Solid phase extraction-liquid chromatography-mass spectrometric detection method of glyphosate in aquatic products
  • Solid phase extraction-liquid chromatography-mass spectrometric detection method of glyphosate in aquatic products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Determination of Glyphosate in Carp by Liquid Chromatography-Mass Spectrometry

[0023] (1) Ultrasonic solvent extraction: Weigh 5.00 g of minced and homogenized carp muscle samples into a polyethylene plastic centrifuge tube, add 15 mL of ultrapure water and 5 mL of dichloromethane, cover and vortex for 2 min, and then store at room temperature Ultrasonic extraction for 20min, then centrifugation at 4000r / min for 10min, transfer the supernatant to another polyethylene plastic centrifuge tube, add 15mL ultrapure water and 5mL dichloromethane to the residue, vortex again, and sonicate and centrifuge, combine and mix the two supernatants, centrifuge at 4000r / min for 10min, take 8mL of supernatant, add 2mL of acetonitrile, vortex and mix to obtain extract A;

[0024] (2) Enrichment and purification by solid phase extraction: C 18 Solid-phase extraction cartridge, the specification is 500mg, 3mL, activate C with 2mL acetonitrile and 2mL ultrapure water in sequence 18 Soli...

Embodiment 2

[0033] Determination of glyphosate in shrimp by liquid chromatography-mass spectrometry

[0034] (1) Ultrasonic solvent extraction: Weigh 5.00 g of minced and homogenized prawn muscle samples into a polyethylene plastic centrifuge tube, add 20 mL of ultrapure water and 5 mL of dichloromethane, cover and vortex for 2 min, and place at room temperature Ultrasonic extraction for 25 minutes, centrifugation at 5000r / min for 8 minutes, transfer the supernatant to another polyethylene plastic centrifuge tube, add 20mL ultrapure water and 5mL dichloromethane to the residue, vortex again, and sonicate and centrifuge, combine and mix the two supernatants, centrifuge at 5000r / min for 8min, take 8mL of supernatant, add 2mL of acetonitrile, vortex and mix to obtain extract A;

[0035] (2) Enrichment and purification by solid phase extraction: C 18 Solid-phase extraction cartridge, the specification is 500mg, 3mL, activate C with 2mL acetonitrile and 2mL ultrapure water in sequence 18 Solid...

Embodiment 3

[0040] Determination of Glyphosate in Carp by Liquid Chromatography-Mass Spectrometry

[0041] (1) Ultrasonic solvent extraction: Weigh 10.0 g of minced and homogenized carp muscle sample into a polyethylene plastic centrifuge tube, add 20 mL of ultrapure water and 10 mL of dichloromethane, cover and vortex for 3 min, and place at room temperature Ultrasonic extraction for 30min, centrifugation at 4000r / min for 15min, transfer the supernatant to another polyethylene plastic centrifuge tube, add 20mL ultrapure water and 10mL dichloromethane to the residue, vortex again, and sonicate and centrifuge, combine and mix the two supernatants, centrifuge at 4000r / min for 15min, take 4mL supernatant, add 1mL acetonitrile, vortex and mix to obtain extract A;

[0042] (2) Enrichment and purification by solid phase extraction: C 18 Solid-phase extraction cartridge, the specification is 500mg, 3mL, activate C with 2mL acetonitrile and 2mL ultrapure water in sequence 18 Solid-phase extract...

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Abstract

The invention discloses a solid phase extraction-liquid chromatography-mass spectrometric detection method of glyphosate in aquatic products. The method has the advantages that ultrasonic-assisted ultrapure water is mixed with dichloromethane to extract the glyphosate in the aquatic products, time consumption is reduced, and good extraction effect and simpleness in operation are achieved; a C18 solid phase extraction column is used to perform enrichment and purification, a good purification effect is achieved, and interference of impurities in extract on final instrument measurement is lowered effectively; a liquid chromatography-mass spectrometry method is used to perform multi-reaction monitoring, and high sensitivity and accuracy are achieved; compared with the existing testing technology, the method does need derivation during glyphosate detection, derivatization reagents and equipment such as high-temperature water bath and oil bath pots or an ultra-low-temperature refrigerator are not needed, the method can perform qualitative and quantitative measurement at the same time and is simple to operate, practicable, low in consumption cost and capable of fast analyzing the glyphosate in the aquatic products.

Description

technical field [0001] The invention relates to the technical field of aquatic product quality and safety detection, in particular to a solid-phase extraction-liquid chromatography-mass spectrometry detection method for glyphosate in aquatic products. Background technique [0002] Glyphosate is a broad-spectrum herbicide with stable properties and low toxicity. It is widely used in the control of various weeds in farmland, gardens, nurseries, railways, roads, forests, lakes, etc. At present, it is the most widely used and used pesticide variety in the world. In 2010, glyphosate accounted for 24% of the total herbicide market and 10.8% of the global pesticide market demand. In 2012, the global demand for glyphosate has reached 650,000 tons. Although glyphosate has always been considered a "safe" herbicide, its long-term and large-scale use will still affect soil microorganisms and the probability of soybean root diseases; some studies have also shown that glyphosate can acc...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/062
Inventor 郝青刘秀梅金衍健胡红美郭远明严忠雍陈思
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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